Ion chromatography for food & beverage analysis
Discover simple, streamlined methods to overcome analytical challenges in the modern laboratory
BROUGHT TO YOU BY INDEPENDENT SCIENCE PUBLISHER IN PARTNERSHIP WITH IC for food & beverage analysis
Introduction
How do you analyze carbohydrates, Contents additives, and ionic substances in foods and beverages? How do you • Why choose ion chromatography? check the quality of raw materials for adulterants and contaminants? Do you • Applications use single-analyte methods such as o Beverages titration and/or sophisticated enzymatic o Additives, preservatives or LC-MS/MS methods? Does your & nutrients laboratory staff struggle with o Dairy time-consuming and error-prone manual sample preparation steps such as Carrez o Further applications precipitation and manual dilution? • IC compliance • Automation & Metrohm Inline In recent years, awareness of food quality Sample Preparation and ingredients has grown substantially. • Detection techniques Consumers want to know what they are eating and expect thorough and detailed o Conductivity food labeling to track this. o UV/Vis detection Public authorities have responded by o Amperometry introducing more stringent quality standards and labeling requirements (e.g., EU regulation • Featured products 1169/2011 or the US regulation 21CFR101).
2 IC for food & beverage analysis
To meet these regulations, fast, robust, preparation procedures such as dialysis, and reliable food analysis is a must. filtration, and dilution help save time and Food and beverage analysis is challenging reduce the number of error-prone and – not just because of the large number time-consuming manual steps. You can of analytes that must be monitored in expect the latest convenience and security compliance with the national and international features from modern IC software that norms and standards but also due to the provides automated data evaluation, complex matrix of many foodstuffs themselves. monitoring of quality criteria and output, Ion chromatography (IC) can address as well as full traceability of results. many of these challenges better than more In this application eBook, we outline how traditional methods. IC is an easy-to-use, you can bring your food and beverage highly robust analytical technique with the analysis to the next level – enhancing ability to quantify multiple components in a productivity, reducing costs, and achieving single run. Moreover, automated inline sample accurate, reliable, and robust results.
The 940 Professional IC Vario and 889 IC Sample Center from Metrohm AG
3 IC for food & beverage analysis
IC is a robust and time-saving technique for Why choosing ion multicomponent analysis in foods and chromatography (IC) for beverages. It is superior to single- component analytical techniques and less IC isICa isrobusta robustandandtimetime-saving-savingtechniquetechniquefor for complex than hyphenated techniques, but WhyWhyfood choosing choosingand beverage ion ion multicomponentmulticomponentanalysisanalysisin infoodsfoodsandand highly specific, precise, robust, and easy to beveragesbeverages. It. Itis issuperiorsuperiorto tosinglesingle- - chromatographychromatographyanalysis? (IC) (IC) for for use. Why choosing ion componentcomponentanalyticalanalyticaltechniquestechniquesIC is aandrobustandlessandless time-saving technique for foodfood and and beverage beverage complexcomplexthanthanhyphenatedhyphenatedtechniquesmulticomponenttechniques, but, but analysis in foods and chromatography (IC)highlyhighly forspecific specific, precise, precise, robust,, robust,beveragesandandeasyeasy. toIt tois superior to single- analysis?analysis? use.use. component analytical techniques and less food and beverage complex than hyphenated techniques, but highly specific, precise, robust, and easy to analysis? use. This technique is straightforward and easy to use with low instrument and operating costs.
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Applications – selected Applications – selected examples from the food Applicationsexamples from – selected the food and beverage sector Applicationsandexamples beverage from – sectorselected the food examplesand beverage from sector the food and beverage sector BEVERAGE BEVERAGE BEVERAGE Carbohydrates in juice, coffee, beer BEVERAGE Carbohydrates in juice, coffee, beer BEVERAGE Sweeteners and sugar substitutes SweetenersCarbohydrates and in sugar juice, substitutes coffee, beer Cations and anions in beer and water SweetenersCarbohydrates and in sugar juice, substitutes coffee, beer CarbohydratesCations and anions in juice, in beer coffee, and beer water Herbicides in water CationsSweeteners and andanions sugar in beer substitutes and water SweetenersHerbicides in and water sugar substitutes Organic acids and anions in wine HerbicidesCations and in anions water in beer and water CationsOrganic andacids anions and anions in beer in and wine water Biogenic amines and cations in wine OrganicHerbicides acids in waterand anions in wine HerbicidesBiogenic amines in water and cations in wine BiogenicOrganic acids amines and and anions cations in wine in wine Organic acids and anions in wine Biogenic amines and cations in wine ADDITIVES, PRESERVATIVES, NUTRIENTS ADDITIVES, PRESERVATIVES, NUTRIENTS Biogenic amines and cations in wine ADDITIVES, PRESERVATIVES, NUTRIENTS Nitrate and nitrite in foodstuffs ADDITIVES, Nitrate PRESERVATIVES, and nitrite in foodstuffs NUTRIENTS ADDITIVES, Polyphosphates PRESERVATIVES, in seafood NUTRIENTS PolyphosphatesNitrate and nitrite in inseafood foodstuffs Sulfite in mustard and dry fruits PolyphosphatesNitrate and nitrite in inseafood foodstuffs NitrateSulfite in and mustard nitrite andin foodstuffs dry fruits Bromate and iodate in flour SulfitePolyphosphates in mustard in and seafood dry fruits PolyphosphatesBromate and iodate in seafood in flour Iodate and iodide in salt BromateSulfite in andmustard iodate and in dryflour fruits SulfiteIodate inand mustard iodide andin salt dry fruits Galacto-oligosaccharides (GOS) in GalactoIodateBromate and-oligosaccharides and iodide iodate in insalt flour (GOS) in Bromatesupplements and iodate in flour supplementsGalactoIodate and-oligosaccharides iodide in salt (GOS) in Iodate and iodide in salt supplementsGalacto-oligosaccharides (GOS) in DAIRY Galacto-oligosaccharides (GOS) in DAIRY supplements supplements DAIRY Lactose in low-lactose products DAIRY Lactose in low-lactose products DAIRY Carbohydrates in milk products CarbohydratesLactose in low- lactosein milk products Iodide in milk CarbohydratesLactose in low- lactosein milk products LactoseIodide in in milk low-lactose products Nitrate and nitrite in milk CarbohydratesIodide in milk in milk products CarbohydratesNitrate and nitrite in milk in milk products Choline in milk powder formula NitrateIodide in and milk nitrite in milk IodideCholine in in milk milk powder formula Fructans in infant formula 5 CholineNitrate and in milk nitrite powder in milk formula NitrateFructans andin infantnitrite formula in milk 5 5 Choline in milk powder formula 5 Fructans in infant formula 5 Choline in milk powder formula 5 Fructans in infant formula 5 Fructans in infant formula 5 RETURN TO TOP 5 5 5 IC for food & beverage analysis
Beverage Coffee quality assurance – Free and total carbohydrate analysis
SUMMARY SAMPLES AND SAMPLE configuration). The amperometric PREPARATION detection was performed after One of the most popular beverages post-column addition with and of huge economic importance is Instant coffee (≈ 300 mg) 300 mmol/L NaOH. coffee. Quality assurance and tracing Free CHOs: Dissolution in of adulterants is therefore a widely 100 mg ultrapure water (UPW) RESULTS established process. Carbohydrates and filtration (0.25 µm) For the different instant coffee (CHOs) in particular, which can make samples, the free CHO content up to 50% of raw coffee beans, Total CHOs: Hydrolyzation in ranged from 10 to 100 g/kg with contribute to flavor, viscosity, and HCl (0.1 mol/L) at 100 °C arabinose, galactose/glucose, aroma. Furthermore, they serve as (150 min), dilution to 100 mL and fructose as the major authenticity tracers. ISO 11292 and UPW and filtration with an + + components. The total CHO AOAC 996.04 define quality Ag –H –cartridge content after HCl hydrolysis was standards for instant coffee - the combination, final dilution between 300–400 g/kg with analysis of free and total (10–50–fold) with UPW galactose and mannose as main carbohydrates. Free carbohydrates in EXPERIMENTAL constituents. coffee are determined after simple 10 CHOs (mannitol, arabinose, dilution, while total carbohydrates BENEFITS are determined as sum parameter galactose, glucose, mannose, after acidic hydrolysis. fructose, and sucrose for Separation of multiple CHOs dissolved CHOs plus xylose for by a concentration- and flow- The present method descibes the total CHOs in addition to gradient combination within a precise separation and rhamnose and ribose) were single run quantification of all relevant analytes baseline separated on a Metrosep according to AOAC and ISO on a Selective and sensitive Carb 2 column with a binary detection with PAD Metrosep Carb 2 column followed by high–pressure gradient combined post-column addition (PCR) and with a flow gradient (940 Conforms with ISO 11292, pulsed amperometric detection Professional IC Vario ONE/HPG AOAC 996.04, DIN 10780:2003 (PAD).
Metrosep Carb 2 - 250/4.0 Eluent A: UPW B: 0.2 mol/L NaOH + 1 mmol/L NaOAc Flow Flow gradient (0.5 – 0.8 mL/min) Temp 27 °C Injection 20 µL
Detection PAD, 0.05 V 6 Free sugars in instant coffee with mannitol (24 mg/L), rhamnose (1.3 mg/L), arabinose (11 mg/L), galactose (10 mg/L), glucose (51 mg/L), mannose (14 mg/L), xylose (0.6 mg/L), fructose (82 mg/L), ribose (5.6 mg/L), sucrose (29 mg/L).
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Beverage Carbohydrates in orange juice
SUMMARY SAMPLES AND SAMPLE RESULTS EU Regulation No. 2012/12/EU sets PREPARATION In the orange juice samples the standards for production, Orange juice (GraniniTM) monosaccharides glucose and composition and labelling of fruit diluted in ultrapure water fructose (≈2 g/100 mL) and the juices. These regulations are (500– or 1000–fold) disaccharide sucrose intended to comply with the newest (≈ 4 g/100 mL) are dominant. The technical improvements described in MISP sum of 8.8 g/100 mL the Codex-Norm. The CODEX STAN Inline Dilution (optional) carbohydrates corresponded to 247-2005 regulates quality and the product label (9 g/100 mL). Inline Ultrafiltration labelling of fruit juices and is a Inositol was found in low widely accepted role model for EXPERIMENTAL concentrations (≈0.2 g/100 mL). standards at national levels [1]. The system showed excellent Samples were injected after stability over 48 h with RSDs for One requirement for accurate manual dilution and Inline the analyzed check standards of labelling is the indication of the Ultrafiltration. The major <1.5%. No electrode cleaning sugar content and addition of carbohydrates, inositol, glucose, was necessary within that sugars. fructose, and sucrose, were timeframe. This robust and straightforward IC separated isocratically on a method with amperometric Metrosep Carb 2 column. Pulsed BENEFITS amperometric detection enabled detection is suitable to analyze Inline Ultrafiltration protects a very sensitive detection and various carbohydrates directly in the the column and system juice matrix. Automated inline prolongs the lifetime of sample preparation with Inline electrodes. Manual sample preparation is not required Ultrafiltration or Inline Dialysis This analysis is performed on a replaces manual steps making small footprint IC and cost of Sensitive quantification of sample preparation much more ownership is low. To check multiple carbohydrates in a efficient. system stability a check standard single run was measured every sixth sample.
Metrosep Carb 2 - 150/4.0 Eluent 100 mmol/L NaOH + 10 mmol/L NaOAc Flow 0.5 mL/min Temp 30 °C Injection 20 µL Detection PAD, 0.05 V
Pulsed amperometric signal of an orange juice sample (1000–fold dilution) containing inositol (0.2 g/100 mL), glucose 7 (2.1 g/100 mL), fructose (2.3 g/100 mL), and sucrose (4.3 g/100 mL) as major carbohydrates.
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Beverage Tracing juice adulterants - cellobiose in apple juice
SUMMARY SAMPLES AND SAMPLE RESULTS PREPARATION Cellobiose, a disaccharide with two Cellobiose eluted after glucose molecules connected by a β- Apple juice, diluted 10–fold 22 minutes. The analyzed sample 1,4 - glycosidic bond, has gained contained about 5 mg/L importance as a novel food MISP cellobiose. Spiking tests with 5 ingredient serving as low-calorie Inline Ultrafiltration and 10 mg/L cellobiose showed bulking agent or lactose substitute. excellent recoveries of 102% However, it is also considered as a EXPERIMENTAL within the range of usual contaminant and adulterant from Separation of cellobiose from acceptance criteria. cellulose degradation and can be an other carbohydrates and sugar Beside cellobiose, other sugar indicator for authenticity alcohols was accomplished on a alcohols and carbohydrates (e.g., infringements. The International Metrosep Carb 2 column. Signal inositol, xylitol, arabitol, sorbitol, Fruit and Vegetable Juice detection was performed by PAD mannitol, rhamnose, glucose, Association (IFU) only recommends using a Wall-Jet cell (Au working xylose, fructose, sucrose) can be cellobiose analysis with capillary gas and Pd reference electrode). determined with this method. chromatography [1]. IC is an easy-to- Analysis time and column This shows the flexibility of IC: use and cost-efficient alternative. cleanup was accelerated with a without any further technical Analysis of cellobiose in apple juice is flow gradient: upgrades the complexity of the possible with manual or automated analyses can be increased dilution and filtration within less towards a multiple-analyte than 30 minutes using IC with pulsed method. amperometric detection (IC-PAD). The flow gradient elution from the BENEFITS robust Metrosep Carb 2 column Fast cellobiose elution reduces overall determination time. Multi-analyte determination possible
Metrosep Carb 2 - 150/4.0 Eluent 100 mmol/L NaOH + 10 mmol/L NaOAc Flow Flow gradient (0.3 – 0.8 mL/min) Temp 30 °C Injection 20 µL Detection PAD, 0.05 V Amperometric signal of the analysis of apple juice spiked with 5 mg/L cellobiose (recovery 102%). A step-flow 8 gradient improved the separation and shortened column clean-up time. Inline Ultrafiltration was used for automatic sample preparation, additionally set-up efficiency benefits from inline dilution replacing manual steps.
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Beverage Analysis of raffinose, stachyose, and verbascose
SUMMARY MISP sensitive detection of all carbohydrates. The raffinose family of Partial loop injection (MiPT) oligosaccharides are α-galactosyl Name RSD [%] R2 EXPERIMENTAL derivatives of sucrose. The most Sorbitol 0.785 0.999980 common derivatives are the Standards were analyzed on a Mannitol 1.099 0.999960 trisaccharide raffinose, the 940 Professional IC Vario ONE tetrasaccharide stachyose, and the equipped with pulsed Glucose 0.246 0.999998 pentasaccharide verbascose [2]. amperometric detection (PAD). Galactose 0.371 0.999995 Such raffinose derivates occur The cooled autosampler Fructose 0.832 0.999977 naturally in vegetables (e.g., green contained an injection valve with Sucrose 0.493 0.999992 partial loop mode for variable beans, soybeans, and other beans) Stachyose 0.442 0.999994 injection volumes (2–50 µL with 1 and in other plants. Stachyose is less Verbascose 2.050 0.999861 sweet than sucrose, at about 28% by µL increments). Carbohydrates were separated on a Metrosep weight. It is mainly used as a bulk BENEFITS sweetener or for its functional Carb 2 column applying a flow Quantification of raffinose, oligosaccharidic properties. gradient for optimal separation within 45 minutes. stachyose, and verbascose next These oligosaccharides are readily to common sugars and sugar separated from polyols, and mono- RESULTS alcohols in a single run and disaccharides on the Metrosep Eight carbohydrates were Flow gradient with just one Carb 2 column. A flow gradient analyzed in the µmol/L range. high-pressure pump for enables optimal separation with Raffinose was separated from optimal separation minimal technical requirements of stachyose, eluting after 36 min. only one high-pressure pump. Calibration was linear over a Baseline resolution of glucose Detection with pulsed amperometry concentration range of 1:100, and galactose (PAD) is the method of choice for e.g., stachyose 0.4–40 µmol/L Stable samples thanks to 889 selective and sensitive (table below). PAD enabled IC Sample Center – cooltable determination.
Metrosep Carb 2 - 250/4.0 Eluent 200 mmol/L NaOH + 1 mmol/L NaOAc Flow Flow gradient (0.4 – 0.7 mL/min) Temp 30 °C Injection 20 µL Detection PAD, 0.05 V Amperometric signal for the analysis of a mixed standard with sorbitol, mannitol, glucose, galactose, fructose (25 9 µmol/L each), sucrose (12.5 µmol/L), stachyose, and verbascose (10 µmol/L each). Raffinose eluted after 36 minutes (data not shown).
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Beverage Controlling beer quality - carbohydrate analysis in beer wort
SUMMARY SAMPLES AND SAMPLE added, to accelerate later eluting carbohydrates to achieve a total When producing beer, germinated PREPARATION analysis time of approx. 60 min. and dried cereal grains (typically Beer wort barley) are subjected to a Filtered and diluted RESULTS fermentation process. Enzymes Due to the excellent detector convert the grain’s starch into MISP carbohydrates, including the sensitivity, signals were well Inline Dilution monosaccharide glucose, the above the detection limits, even disaccharide maltose, the Inline Ultrafiltration with low injection volumes of trisaccharide maltotriose, and the diluted samples. As expected, EXPERIMENTAL polysaccharide maltodextrin. maltose was the predominant Proteins, free amino acids, vitamins, After Inline Dilution and carbohydrate, with and minerals are also present. Ultrafiltration, injection volumes concentrations around 50 g/L. Knowledge about the carbohydrate of only 1.5 µL were required as Analysis of maltoheptaose will profiles helps to control the process high concentrations of also be possible but it was not and improve the beer quality. carbohydrates are present in the present in this sample. samples. Due to this, matrix The presented IC method monitors BENEFITS effects are minimized, and the different carbohydrates of interest. system was unaffected by Determination of Samples were diluted and their contamination for an extended monosaccharides and sugar components were separated time period. For optimal oligosaccharides in one on a Metrosep Carb 2 column with a separation a Dose-in gradient analysis Dose-in gradient within 60 minutes. was applied to the diluted Carbohydrates from mono- Dose-in gradient accelerates samples (1:100). After 35 minutes saccharides up to hexaoses were the elution of oligosaccharides with eluent A (100 mmol/L determined in one run with pulsed Sensitive detection of low NaOH + 25 mmol/L NaOAc), amperometric detection (PAD). concentrations next to high 95% of eluent B (220 mmol/L concentrations of e.g., maltose NaOH + 200 mmol/L NaOAc) was
Metrosep Carb 2 - 250/4.0 Glucose Eluent Dose-in gradient Maltose
(NaOH + NaOAc) Maltotriose Sucrose Maltotetraose Flow 0.7 mL/min Fructose Temp 30 °C Maltopentaose Injection 1.5 µL Maltohexaose Detection PAD, 0.05 V
Amperometric signal of a beer wort sample at the effluent of a boiler (diluted 100–fold), containing per 100 mL: 10 glucose (0.85 g), fructose (0.15 g), sucrose (0.38 g), maltose (4.81 g), maltotriose (1.22 g), maltopentaose, and maltohexaose (0.07 g each).
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Beverage Aspartame, cyclamate, acesulfame-K, and saccharin in soft drinks
SUMMARY SAMPLES AND SAMPLE RESULTS Artificial sweeteners like aspartame PREPARATION Samples were analyzed in (E 951), acesulfame-K (E 950), Coca-ColaTM Zero, Red BullTM triplicate with RSDs <1%. cyclamate (E 952), and saccharin sugar free, PepsiTM Max Aspartame and acesulfame-K were present in all samples, (E 954) are added to foodstuffs to Samples were degassed and whereas cyclamate was only reduce calories and sugar content diluted (dilution factor 5–10) while keeping a consistently sweet found in Coca-ColaTM Zero. taste. They are used worldwide in MISP Saccharin was not detected. various products even though Inorganic anions (e.g., chloride, Inline Dilution adverse health effects are being nitrate, sulfate, and phosphate) discussed. Strict regulations and EXPERIMENTAL as well as organic acids (e.g., labelling are mandatory in many formate, acetate, benzoate, The Metrosep A Supp 10 column countries, e.g., the acceptable daily citrate) were separated from the is suitable to separate the intake (ADI) for aspartame is set to sweeteners to avoid potential sweeteners from many water- 40 mg/kg body weight [3]. ADI for interferences. soluble components found in saccharin is between 0–5 mg/kg [4]. typical beverage matrices. The Sodium cyclamate’s ADI is BENEFITS separation was optimized by suggested between 0–11 mg/kg in Two complementary detectors combining a concentration EU and China, while it is prohibited used for peak identification gradient using a Metrohm Dosino in the US [5]. and quantification without any (Dose-in gradient) and a flow doubt IC with suppressed conductivity and gradient to accelerate late- UV/VIS detection in series is a eluting matrix components. The No interference from common sensitive and highly specific method conductivity signal was evaluated anions and other matrix to determine the four most common after suppression. The UV signal components in soft drinks, e.g., sweeteners, aspartame, acesulfame- at 210 nm was recorded in series citric acid or phosphate K, cyclamate, and saccharin, in a to confirm peak identities and to variety of soft drinks. evaluate the conductivity signal.
Metrosep A Supp 10 - 75/4.0 Eluent Dose-in gradient (NaOH + NaOAc + methanol) Flow 1.0 – 1.2 mL/min Temp 35 °C Injection 20 µL Detection Conductivity + UV Conductivity signal of a standard containing aspartame, cyclamate, acesulfame-K and saccharin (20 mg/L each). 11 Automatic calibration by Metrohm Inline Dilution of the highest standard can be applied (optional).
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All four sweeteners showed signals Conductivity in the conductivity detector and good UV absorption (except for cyclamate*, see table below). Therefore, the UV signal was used for confirmation of the three sweeteners aspartame, acesulfame- K, and saccharin. Quantification with both detectors gave consistent results (see table below). The figure to the right displays typical chromatograms for a Red BullTM sample (5–fold dilution). UV/VIS Potential interferences from phenylalanine and taurine were also investigated. These components become protonated in the suppressor module and leave the system during suppressor regeneration. They do not interfere with the analysis.
Aspartame Acesulfame-K Comparison of the conductivity signal (upper panel) and UV signal (lower panel) of a Red BullTM sample (5–fold dilution). The signal for aspartame (orange) and acesulfame-K (blue) are highlighted.
Sample Sweetener Conductivity [mg/L] RSD [%] UV 210 nm [mg/L] RSD [%] aspartame 106.76 0.2 100.75 0.6 Red BullTM acesulfame-K 195.24 0.1 197.62 0.2 aspartame 746.43 0.3 740.99 0.3 PepsiTM Max acesulfame-K 51.07 0.6 54.92 1.2 aspartame 92.25 0.5 111.12 0.7 Coca-ColaTM cyclamate 229.61 0.1 not detected* –* Zero acesulfame-K 145.77 0.3 158.89 0.7 12 Data summary for the evaluation of three soft drink samples. Results for conductivity and UV detection were comparable.
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Beverage Sucralose in soft drinks
SUMMARY SAMPLES AND SAMPLE dilution factors to this solution. PREPARATION Sucralose (E955) is an artificial sugar RESULTS substitute produced from sucrose by Soft drink with 11 g sugar per replacing three hydroxyl groups with 100 mL The analyzed samples contained up to 100 mg/L sucrose. Linear chlorine atoms. It is noncaloric [6], Sugar-free energy drink 320 to 1000 times sweeter than calibration from 0.5 to 25 mg/L sucrose [7], and does not promote Degassed (10 minutes sucralose was achieved with a tooth decay [8]. Since it is considered sonication) correlation coefficient of >0.9999 safe by regulatory bodies such as and <1.7% RSD. Spiking tests MISP FDA, WHO, and the EU’s Scientific with 5 mg/L sucralose resulted in Committee on Food, it is added as an Inline Dilution (20–fold) recoveries of ≈99.5%. artificial sweetener to many foods EXPERIMENTAL BENEFITS and beverages. Degassed and diluted samples Robust and straightforward As detailed metabolic pathways of were automatically injected into method with IC and PAD artificial sweeteners and their effects a 930 Compact IC Flex. Their ionic detection on health are still not fully components were isocratically understood, it is good practice to Isocratic separation of sucrose separated on a Metrosep monitor their content in foodstuffs. from other carbohydrates A Supp 17 column and their High accuracies proven by This IC method is a robust and sucralose content quantified with good recoveries of spiking simpler alternative to commonly pulsed amperometric detection tests used mass spectrometric methods, (PAD). Inline Dilution enabled fast e.g., HPLC-MS. Isocratic separation and accurate automated sample requires just one high-pressure dilution. Additionally, Inline pump. By utilizing amperometric Dilution was used for automatic detection, high selectivity and calibration from a single standard sensitivity can be achieved. solution by applying different
Metrosep A Supp 17 - 100/4.0 Eluent 125 mmol/L NaOH + 5% acetone Flow 0.6 mL/min Temp 45 °C Injection 20 µL Detection PAD, 0.05 V
Amperometric signal from the analysis of an energy drink (20–fold dilution) containing sucralose (4.8 mg/L). 13 Automatic calibration by Inline Dilution of the highest standard can be applied (optional).
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Beverage Rebaudiosides and stevioside in stevia sweetener
SUMMARY SAMPLES AND SAMPLE RESULTS Steviol glycosides from the PREPARATION Rebaudioside A was quantified in plant Stevia rebaudiana have been Stevia powder (97% steviasol (415 g/kg) and in used as sweetener and sugar Rebaudioside A), Kräuterhaus Zucristevia (142 g/kg). Inulin, substitutes for more than 1000 Sanct Bernhard, Germany sodium bicarbonate, and sodium citrate eluted in a single peak at years. The main components Steviasol, powder, Steviasol AG the beginning of the stevioside and rebaudioside are 30 – Herisau, Switzerland 150 times sweeter than sugar and chromatogram. Common do not metabolize in the human Zucristevia, pastilles, Migros carbohydrates eluted with the body, i.e., they do not contribute AG Zurich, Switzerland injection peak. calories [9]. 100 mg dissolved in 10 mL The modes flexIPAD and standard Discussions about safety or toxicity eluent, further manual dilution PAD were compared, as well as of stevia is reflected in a long history 20– or 100–fold the recording of current or of regulations. Its legal status differs charge. The flexIPAD mode while EXPERIMENTAL from country to country. measuring the current showed Glycosides from Stevia were the best signal-to-noise ratio. High-purity Stevia glycosides are separated on a Luna® 5 µm allowed as ingredients in food C18(2) 100 Å, LC Column 250 x BENEFITS products sold in the United States. 4.6 mm, Ea from Phenomenex. However, Stevia leaves and crude Robust separation of After post-column addition of extracts are not considered safe rebaudiosides and stevioside 400 mmol/L NaOH, a 945 according to the US FDA. Upgrade of any HPLC-system Professional Detector Vario – with a Metrohm amperometric This IC method shows the Amperometry was used in detector for sensitive glycoside quantification of the active flexIPAD mode. A 2 mm gold analysis ingredients rebaudioside A, working electrode ensured signal rebaudioside C, and stevioside in stability. Stevia powder was used FlexIPAD mode guarantees Stevia sweeteners. as reference standard. highest sensitivity for the analysis of Stevia products
Luna® 5 µm C18(2) 100 Å Eluent 10 mmol/L NaH2PO4, pH 4.5 30% acetonitrile Flow 0.3 mL/min Temp 40 °C Injection 20 µL Detection flexIPAD Amperometric signal for steviasol analysis showing rebaudioside A (415 g/kg), stevioside, and rebaudioside C (not 14 quantified). The measuring mode flexIPAD was used and the current was recorded as measuring signal.
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Beverage Monitoring beer quality - cations and anions in beer
SUMMARY SAMPLES AND SAMPLE logical dilutions, saving lab work PREPARATION and time. High accuracy is The ionic composition has massive achieved with an optimized influence on the taste of beer. Thus, Beer from different brands, calibration fit over a broad potassium chloride salts lead to a e.g., WarsteinerTM concentration range (feature: bitter, astringent, and soapy taste Filtration and dilution high-low calibration). while magnesium sulfates lead to a automatically controlled sweet-sour taste. RESULTS MISP Therefore, analytical monitoring of As the main cation constituent the beer is essential to guarantee Logical Inline Dilution potassium (K+) was identified in quality and meet consumer Ultrafiltration all samples, while the expectations. concentration of other cations Major cations in beer are precisely EXPERIMENTAL was lower than 100 mg/L (see + determined with IC and non- An autosampler (including figure below). K in beer provides suppressed conductivity detection. filtration and dilution equipment) a bitter and astringent taste. Anions are quantified by suppressed prepares the sample for two Chloride, phosphate, nitrate, and conductivity. With a two-channel analysis channels in such a way sulfate were the main anions system, cations (separated on a that anions and cations are detected in beer. Samples can be Metrosep C 6 column) and anions determined in parallel from the injected with the most suitable (separated on a Metrosep A Supp 10 same sample (figure next page). injection volume. Together with column) can be determined Two 930 Compact IC Flex systems logical dilutions, sample simultaneously. Automatic were used to simultaneously concentrations in the range of calibration, logical dilution, and analyze cations (results below) 1:10,000 can be analyzed reliably. filtration of the samples save manual and anions (next page) under High accuracy of results is preparation steps and ensure fast isocratic elution conditions. achieved by an optimal fit for the analysis of samples in high- MagIC Net software allows calibration points (feature: high- throughput laboratories. calibration using a single low calibration). standard solution and performs
Metrosep C 6 - 150/4.0
Eluent 2.3 mmol HNO3 + 1.7 mmol/L DPA Flow 0.9 mL/min Temp 35 °C Injection 20 µL Detection Conductivity
Non-suppressed conductivity cation signal for the analysis of a Warsteiner lager beer sample (10–fold dilution) 15 containing sodium (13 mg/L), potassium (365 mg/L), calcium (53 mg/L), and magnesium (56 mg/L) as major cations.
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Beverage Cations and anions in beer
BENEFITS High-low calibration for precise results of samples over Simultaneous analysis of a wide concentration range multiple anions and cations in one run Robust and simple method Automatic logical Metrohm with isocratic elution to Inline Dilution saves time and determine main anions and manual work cations in beer Samples with results outside Sulfite, a common preservative the calibration range are can be determined next to automatically re-diluted to fit other anions (retention time into the calibration range ≈11 minutes)
Schematic flow path for simultaneous analysis of anions and cations with Metrohm Inline Sample Preparation (MISP).
Metrosep A Supp 10 - 100/4.0
Eluent 4 mmol Na2CO3 + 6.0 mmol/L NaHCO3 + 5.0 µmol/L NaClO4 Flow 0.7 mL/min Temp 30 °C Injection 20 µL Detection Conductivity Suppressed conductivity anion signal for the anaylsis of a Warsteiner lager beer sample (10–fold dilution) containing 16 chloride (229 mg/L), phosphate (352 mg/L), nitrate (5 mg/L), and sulfate (60 mg/L) as major anions.
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Beverage Anions and oxyhalides in drinking water
SUMMARY SAMPLES AND SAMPLE between 4 and 200 µL (MiPT) PREPARATION allowed the analysis of various Safe drinking water is vitally water types with different important. Bottled water and Drinking water, tap water mineral contents. mineral water are the most popular No manual sample preparation beverages worldwide. For quality required RESULTS control of water, IC is the method of All relevant anions in water were choice for the quantification of MISP determined within a time frame common anions and for the analysis Inline Ultrafiltration of 35 min. The method is suitable of regulated, health critical to quantify 0.0005 mg/L chlorite substances such as bromate, nitrite, Partial loop injection (MiPT) and bromate in drinking water chlorite, and chlorate. They enter the EXPERIMENTAL (limit of quantification). water supply through various An optimized separation of pathways, such as disinfection BENEFITS byproducts during water treatment, bromate, bromide, chlorite and additives, and artificial or natural chlorate from all major anionic Compliance with US EPA 300.1 contaminations. US EPA method water components was achieved A/B 300.1 specifies the determination of by combining a Metrosep A Supp Quantification of low these critical water components. 7 column with a Metrosep A concentrations of oxyhalides Major standardization bodies (US Supp 16 guard column. The two (µg/L range) next to high FDA, WHO) regulated their different resins lead to a phase- concentrations of other ions allowable limits, e.g., <10 µg/L optimized IC separation (POPIC). (mg/L range) bromate in drinking water [10]. A calibration range of 1:100 was Integrated Inline Ultrafiltration covered by applying high-low- The robust IC setup from Metrohm to minimize matrix effects calibration, a technique where guarantees efficient analysis two calibration curves are used to Flexible application that can be according to regulatory standards optimally correlate the respective upgraded with a mass with high sample throughput, signal to the concentration. spectrometer to further automation, and precise results. Flexible injection volumes increases sensitivity
Metrosep A Supp 7 - 250/4.0
Eluent 3.2 mmol/L Na2CO3 1.0 mmol/L NaHCO3 Flow 0.7 mL/min Temp 45 °C Injection 100 µL Detection Conductivity
Conductivity signal of a water sample containing fluoride (0.73 mg/L), chlorite (0.002 mg/L), bromate (0.001 mg/L), 17 chloride (2.12 mg/L), nitrite (0.135mg/L), bromide (0.024 mg/L), chlorate (0.024mg/L), nitrate (2.338 mg/L), phosphate (0.258 mg/L), and sulfate (8.314 mg/L). Retention time of dichloroacetate (DCA) (green arrow).
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Beverage Glyphosate and AMPA in drinking water
SUMMARY SAMPLES AND SAMPLE of each compound showed 3.3% PREPARATION RSD for both, AMPA and Herbicides are health critical glyphosate. Recoveries ranged contaminants in food. Glyphosate Tap water of different between 88–112%, with strong (N-(phosphonomethyl) glycine) is a hardness (high–low) dependence on the type of nonselective broad-spectrum water. Waters with lower herbicide, that inhibits the shikimic MISP hardness tend to show better acid pathway in plants. Globally, it is Inline sample degasser to recoveries. the most widely used herbicide in remove dissolved carbon agriculture, and often used for dioxide BENEFITS weed-killing in domestic gardens. It Amperometric detection reaches drinking water reservoirs EXPERIMENTAL proved to be selective and through ambient air, rivers, or Separation was on a Metrosep sensitive, offering a simple and groundwater. Health concerns are Carb 2 column with a flow rate of economical alternative to more contradictorily discussed, e.g., WHO 0.4 mL/min, which was increased complex MS/MS or ICP/MS classified glyphosate as “probably to 0.8 mL/min after 6 minutes to methods [13] carcinogenic to humans” [11], accelerate the elution of whereas USEPA affirms that glyphosate. Detection was Robust and easy analytical “glyphosate poses no risk to public performed with a dedicated method for AMPA and health” [12]. Soil bacteria potential profile with flexIPAD glyphosate determination in decompose glyphosate into its mode. Calibration was from the µg/L range primary metabolite AMPA 2–100 µg/L for both compounds. Fulfills USEPA LOQ (0.7 mg/L (aminomethylphosphonic acid), for glyphosate) [14] which must also be monitored. RESULTS Limits of quantification (LOQs) Fulfills current LOQs for A straightforward IC method is regulations of glyphosate in introduced to determine glyphosate were 0.4 µg/L (AMPA) and 3.9 µg/L (glyphosate). Inter-day Canada (280 µg/L), Australia and AMPA in the µg/L range with (10 µg/L), and Brazil amperometric detection. precision (5 days, 13 injections) for tap water spiked with 5 µg/L (500 µg/L) [15]
Metrosep Carb 2 - 100/4.0 Eluent 10 mmol/L NaOH + 290 mmol/L NaOAc Flow Flow gradient (0.4 – 0.8 mL/min) Temp 30 °C Injection 250 µL Detection flexIPAD Amperometric signal of a tap water sample spiked with AMPA and glyphosate (5 µg/L each). Recoveries were 85.0% 18 (AMPA) and 99.6% (glyphosate).
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Beverage Fast screening of organic acids and inorganic anions in wine
SUMMARY SAMPLES AND SAMPLE RESULTS Consistency of product quality is of PREPARATION All major organic acids and utmost importance to winemakers. Red wine, white wine inorganic anions were separated Monitoring yeast performance and isocratically within a run time of Gravimetrically diluted 1:10 or efficiency throughout the 20 minutes. Tartrate and acetate 1:50 with ultrapure water fermentation process is just as were identified as the major critical. This wine analysis can aid To prevent oxidation, vials organic acid species. Injections of winemakers with ensuring were closed with polyethylene triplicates showed an excellent predictable flavor and aroma lids repeatability with RSDs of less characteristics in finished wine by than 2%. Phosphate and sulfate MISP monitoring common indicators of were identified as the dominant acidity, mouthfeel, and balance. It Inline Ultrafiltration inorganic anions. also evaluates nutrients and other EXPERIMENTAL additives which could potentially BENEFITS have negative effects on efficiency Samples were directly analyzed Inline Ultrafiltration protects and production during the after dilution and Inline the column and system, fermentation process. This work Ultrafiltration. Separation of increasing lifetime and shows the use of Metrohm IC to organic acids (as their conjugated ensuring trouble-free analyze red and white wine for bases) and inorganic anions was operation, and reduces manual chloride, phosphate, sulfite, sulfate, performed with a Professional IC work malate, tartrate, and oxalate. system equipped with sequential Rapid analysis enables high suppression and a conductivity A Metrohm Professional IC with throughput laboratories to detector. Suppression reduces the sequential suppression and maximize production background signal and the conductivity detection was used in baseline noise and improves Robust setup with isocratic combination with Inline detection sensitivity. The method separation and suppressed Ultrafiltration. working range spans from conductivity detection for 1–100 mg/L. sensitive analysis
Metrosep A Supp 10 - 100/4.0
Eluent 5 mmol/L Na2CO3 + 5 mmol/L NaHCO3 + 5 µmol/L HClO4 Flow 1.0 mL/min Temp 35 °C Injection 20 µL Detection Conductivity Conductivity signal for analysis of major organic acids (acetate (not quantified), malate (105 mg/L), tartrate 19 (1534 mg/L), oxalate (<10 mg/L)) and major anions (chloride (22 mg/L), phosphate (818 mg/L), sulfite (29 mg/L), and sulfate (367 mg/L)) in a white wine sample.
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Beverage Complex monitoring of organic acids and inorganic anions in wine
SUMMARY RESULTS IC setup can be combined with a sensitive MS detector. Nature and concentration of organic The method enables complex acids are important parameters in monitoring analysis of 15 organic BENEFITS enology. They affect organoleptic acids in a working range of properties (color, flavor, and aroma), 0.1–5 mg/L. Sample preparation Conductivity detection wine stability, and help to track can be facilitated with Inline prevents interferences from alteration processes and the wine’s Ultrafiltration, protecting the UV-active components in wine authenticity [16]. A range of organic column and enhancing Optional extension with inline acids are formed as products during instrument performance (figure sample preparation to save alcoholic fermentation influencing below). If peak identity needs time flavor in many ways. Acetic acid for confirmation, or very low Optional addition of a mass example causes an undesirable detection limits are required, the detector for peak identification vinegar taste. Overall, monitoring of organic acids is crucial to improve flavor and quality, and to fulfill universal standardized criteria such as the International Code of Oenological Practices [17]. Analytical monitoring of multiple organic acids can be achieved with IC and suppressed conductivity detection. Optionally, a mass detector can be added for peak verification. Here, a binary gradient on a Metrosep A Supp 7 - 250/4.0 column was used to separate 15 Schematic flow path for IC with Inline Ultrafiltration and suppressed organic acids. conductivity detection. To achieve higher sensitivity and peak confirmation the system can be upgraded with a mass sprectrometer (MS). Metrosep A Supp 7 - 250/4.0 Eluent A: ultrapure water B: 6.4 mmol/L Na2CO3 + 2.0 mmol/L NaHCO3 Flow 0.7 mL/min Temp 45 °C Injection 20 µL
Detection Conductivity 20 Signal of 1 mg/L gluconate (1), lactate (2), acetate (3), propionate (4), iso-butyrate (5), butyrate (6), methacrylate (7), valerate (8), methylsulfate (9), dichloroacetate (10), malonate (11), malate (12), glutarate (13), adipate (14), and phthalate (15).
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Beverage Preventing food allergies - Biogenic amines and cations in wine
SUMMARY SAMPLES AND SAMPLE detected next to the standard cations in the lower mg/L range. During the wine manufacturing PREPARATION process, production conditions, Red wine (Primitivo dal Salente RESULTS storage times, as well as possible 2014 – Cesario) microbiological contamination play a The amines analyzed are shown role in the content of biogenic MISP in the chromatogram below. In the red wine sample, calcium and amines. Histamine is most harmful Inline Dilution to sensitive people and a known magnesium were identified as Inline Ultrafiltration reason for food intolerances; major inorganic cations. Lower amounts of monomethyl- and however, other amines also exhibit EXPERIMENTAL adverse effects. The histamine triethylamine were detected. The Samples were automatically content for wine is often not allergen histamine was not diluted and filtered inline before regulated by law but recommended detected in the investigated injection into the IC system. A to not exceed limits of 2–10 mg/L, samples. binary high-pressure gradient depending on the country [18]. (940 Professional IC with HPG BENEFITS Nine (biogenic) amines and six specification) was used to Minimized matrix effects and inorganic cations were separated on minimize co-elution, to separate fully automated sample a Metrosep C Supp 1 column, using a matrix and analytes, and to preparation due to Inline binary gradient. Suppressed achieve a reasonable overall Dilution and Inline Filtration conductivity guarantees sensitive recording time. Sequential Excellent separation with a detection. Hence this IC method suppression was used to reduce binary gradient in a reasonable offers a robust and reliable way to the background signal and analysis time determine these compounds in wine background noise which is for quality control. important to keep sensitivity Sensitive cation detection with especially for gradient systems. suppressed conductivity With this setup, nine amines were
Metrosep C Supp 1 - 150/4.0
Eluent A: 2.5 mmol/L HNO3 + 100 µg/L Rb+ B: 25 mmol/L HNO3 + 100 µg/L Rb+ Flow 1.0 mL/min Temp 40 °C Injection 100 µL Detection Conductivity 21 Red wine sample (12.5–fold dilution) containing ammonium (26 mg/L), monomethylamine (106 mg/L), triethylamine (47 mg/L), magnesium (153 mg/L), calcium (153 mg/L), putrescine (24 mg/L), and serotonin (5 mg/L) as major cations. Monoethylamine, potassium, diethylamine, 2-phenyl-ethylamine, cadaverine, and histamine (arrow) were not detected.
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Additives, preservatives, nutrients Nitrite and nitrate in meat
SUMMARY SAMPLES AND SAMPLE nitrate 0.05–5.00 mg/L. A wide variety of food and beverage Nitrite and nitrate salts are used as PREPARATION samples were evaluated, showing preservatives for meat and meat Meat, sausages, beverages, symmetric peaks, high products. They are labeled on foods vegetables (5 g homogenized) reproducibility of the as E249–E252. These so-called curing Carrez precipitation concentration values, and salts prevent bacterial growth, keep negligible interferences from the meat’s red color and enhance its Diluted 100-fold, filtered matrix compounds. Limits of flavor. Nitrate salts (E 251, E 252) MISP quantification were well below have low toxicity. However, long- 5 mg/kg for sodium nitrite and term exposure is of concern, as Inline Ultrafiltration sodium nitrate in all tested nitrate is reduced to nitrite in the EXPERIMENTAL samples. lower gut, and nitrite is a precursor Analytes were separated by of nitrosamines, which are classified BENEFITS as carcinogenic [19]. Nitrite is isocratic anion exchange on two classified as probably carcinogenic to columns in series, followed by Fast and time-saving routine humans [20]. MPL (maximum sequential suppression and analysis, without requiring permitted levels) after the UV/VIS detection. The two sample preparation cartridges manufacturing process vary for columns with different properties High accuracy and nitrite (E 249, E 250) between 50– were used in series to avoid co- reproducibility independent 180 mg/kg, and for nitrate between elution of nitrite with other from the food matrix 150–300 mg/kg, depending on the components. A temperature of Automation and robustness product. 52 ºC further improved the surpass analytical performance resolution of the nitrite peak. For quality control, IC offers a highly of classical HPLC-UV sensitive, robust, and fast method for RESULTS Approved method in quality- nitrate and nitrite analysis in various The calibrated range for nitrite control labs of the meat meat products. was 0.02–2.00 mg/L, and for industry
Metrosep A Supp 7 - 250/4.0 + Metrosep A Supp 5 - 50/4.0 Nitrate Eluent 3.6 mmol/L Na2CO3 + 15% methanol Flow 0.7 mL/min Temp 52 °C Nitrite Injection 50 µL Detection UV 205 nm Chromatogram of a sample from pork knuckle containing sodium nitrite (1.5 mg/kg) and sodium nitrate 22 (9.6 mg/kg).
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Additives, preservatives, nutrients Polyphosphates in shrimps
SUMMARY SAMPLES AND SAMPLE 1:50 ( concentration range for pyrophosphate and tripoly- Polyphosphates improve the water- PREPARATION phosphate 5–250 mg/L each; and binding capacity, appearance, and Shrimp, seafood trimetaphosphate 1–50 mg/L) . texture of food products. They are ≈10 g of sample homogenized, often used in the production of 100 mL UPW added RESULTS seafood, such as shrimps, and also added to convenience food, boiled Extracted in an ultrasonic bath Three polyphosphates were sausages, cheese products, soft (30 minutes, 25 °C), analyzed within a run time of drinks, bakery products, or cereals as centrifuged (4000 rpm, 25°C, 13 minutes. The sample injection stabilizers and flavor enhancers. 10 min) and decanted volume was 4 µL and recovery Labeling is required (e.g., E 450 – rate >75%. MISP E 452) and the ADI (acceptable daily BENEFITS intake) of total phosphates is set to Inline Ultrafiltration Determination of the specific 40 mg/kg body weight by the Metrohm intelligent Partial polyphosphate oligomers, in European Food Safety Authority loop Technique (MiPT) (EFSA) [21]. contrast to average chain EXPERIMENTAL length determined in end- The IC method presented here group titration methods shows a fast and straightforward Inline Ultrafiltration removed any way to quantify pyrophosphate, remaining particles. Analysis was Flexible injection volumes to tripolyphosphate, and accomplished on a 930 Compact ensure that measured analytes trimetaphosphate in shrimp. Inline IC Flex with automation and are within the calibrated range sample preparation helps to inline sample preparation. For Upgrade the method with a minimize manual sample calibration, 4–200 µL of a single Dose-in gradient to also preparation steps. Additionally, mix standard (pyrophosphate, quantify fluoride, chloride, samples with a wide concentration tripolyphosphate 5 mg/L each; bromide, nitrate, phosphate, variability are readily analyzed due and trimetaphosphate 1 mg/L) and sulfate to flexible injection volumes. were injected, covering a ratio of
Metrosep A Supp 17 - 100/4.0
Eluent 60 mmol/L Na2CO3 + 2.0 mmol/L NaHCO3 Flow 0.6 mL/min Temp 30 °C Injection 4–200 µL (MiPT) Detection Conductivity
Conductivity signal of a shrimp sample that did not contain polyphosphates in the calibrated concentration range. The 23 samples were spiked with pyrophosphate, tripolyphosphate (100 mg/L each), and trimetaphosphate (20 mg/L).
RETURN TO TOP 23 3.2 mg/kg sulfite. The recovery was 101.5 %. was recovery The sulfite. 3.2 mg/kg 24] foodstuffssolid [23, suitable for beverages, but also for detection Not (patent filed). only is it tailor a on presented, based method is accurate and fast, innovative, An IC cumbersomequite to perform. from repeatability issues, and can be sufferhowever,beverages; they measure sulfite in food and methodsSeveral analytical exist to [22]. mg/kg<450 is sulfite level maximumThe permitted mg/kg. 10 exceeding food labels on declared the that presence of sulfites must be require laws European(EU) Union AdministrationDrug (FDA) and and Food U.S. Therefore, the both reactions. of range allergic a experience may and additives sulfite to sensitive are Some individuals prevent browning or oxidation. ofrange foods vast beverages to and preservative is a Sulfite to a added SUMMARY Overlay Overlay Detection Injection Temp Flow Eluent M e t r made mode of electrochemicalof mode -made o s of IC for food &beverage analysis e p amperometric C a r DC, 0.3 V DC, 3 µL 35 °C 0.5 mL/min 300 mmol/L 300 mmol/L + NaOH 300 mmol/L b
2
- 1 5 0 signals / . 4 . 0 NaOAc for a mustard sample sample PREPARATION SAMPLE ANDSAMPLES high resolution was obtained with the peak injection. Optimal CenterSample prior to IC 889 an were cooled (6samples sample stability, guarantee To EXPERIMENTAL column. The Sulfitein mustard Additives,nutrients preservatives, solution ( with stabilization diluted homogenized sample g 1 peppers chili capers, canned garlic, mustard, cherries,Chickpeas, NaOH formaldehyde 25000 Homogenized tightly closed. and sample completely with filled must be oxidation, vials µm.filtered avoid To with 0.2 rpm, 4000 Centrifuged at homogenizer ® turrax -capacity RETURN TO TOP containing ) to a total of of g. total 30 a to ) rpm 1.0 MagIC Metrosep with mmol /L 3.2 mg/kg sulfite and the same3.2the and sample spiked withmg/kg sulfite + 0.20 for 1 min at at min for 1 an an Net software software Net ultra ° mmol Carb 2 2 Carb C) with C) with - /L /L BENEFITS 90%. recoveries above were spiking matrices. All various sample seriessample with long and remained signal The stable for RESULTS samples. loaded highly measuring witheven the signal increases long the working electrode. This step automatically clean the surface of to filed) (patent treatment» commandoffers «CV a 10 minutes analysis time minutes analysis 10 throughputHighonly with food matrices sulfitetotal many in different quantification of Sensitive weeks for 3 fouling orelectrode deactivation No electrodes cleaned automatically tothanks signal series sample Long stable with -termof stability
Sulfite Spiked sample 24 Sample 24 IC for food & beverage analysis
Additives, preservatives, nutrients Sulfur in dried fruits with Combustion IC
SUMMARY SAMPLES AND SAMPLE Metrohm IC where it is analyzed. PREPARATION The sulfate concentration relates Since ancient times, sulfurization is a to the total sulfur content of the method of preservation to extend Apricots: naturally dried sample, as all sulfur species are shelf life and avoid degradation by (exposed to sunlight) or sulfur oxidized to sulfate with CIC. microorganisms in fruits, meat, fish, dried (exposed to sulfur vegetables, wine, and beer. Treating dioxide gas) RESULTS dry fruits with sulfur dioxide gas ≈75 mg sample weighed Sulfur dried apricots shortens the drying process and directly in a Combustion IC (2937 mg/kg) contained over 25 preserves the color of the product. quartz boat times more sulfur than natural However, sulfite is formed in the dried apricots (112 mg/kg). products which can induce allergic MISP Analysis was reproducible with reactions in some people. Sulfite is Combustion IC (CIC) for solid <3% RSD for triplicate injections. banned in raw foods and must be samples labeled on processed foods BENEFITS according to EC No 1333/2008 EXPERIMENTAL (95/2/EC Appendix III) or CODEX High sample throughput, With CIC, samples are first STAN 192-1995, e.g., if it exceeds precision, and accuracy digested under an argon 500–2000 mg/kg in dry fruits. Fully automated sample atmosphere in the oven unit and preparation for solid and liquid Such high concentrations of sulfur then pyrolized with oxygen and samples with a single modular are directly determined in solid water (pyrohydrolysis). In the 920 sample changer foodstuffs with Combustion IC (CIC). Absorber Module, the formed Complete automation, including gaseous compounds are passed Possible to determine sulfur sample preparation, makes into an absorption solution with and halogens simultaneously Combustion IC superior to offline hydrogen peroxide, to oxidize Compliance with standards digestion methods with regard to them. This absorption solution is such as FDA and GLP sample throughput and precision of then transferred inline to a the results.
Metrosep A Supp 5 - 150/4.0
Eluent 3.2 mmol Na2CO3 + 1.0 mmol/L NaHCO3 Flow 0.8 mL/min Temp 45 °C Injection 10 µL Detection Conductivity
Conductivity signal of the analysis of a naturally dried apricot sample after combustion. The total sulfur content is 25 determined as sulfate as all sulfur species are oxidized to sulfate by pyrohdrolysis. Here, 112 mg/kg sulfur was measured.
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Additives, preservatives, nutrients Bromate in flour
SUMMARY SAMPLES AND SAMPLE RESULTS PREPARATION Potassium bromate is added to flour The setup is compliant with to accelerate the maturation process. Wheat flour ISO/DIN 11206. Bromate was calibrated in the concentration This treatment improves dough 25 g sample suspended in range of 50–2000 µg/kg. Flour properties, leading to stronger and 250 mL water, sonicated for samples did not contain bromate. more elastic bread. Bromate should 30 min at ambient They were spiked with different degrade during the baking process, temperature but residual amounts may remain amounts of bromate, resulting in when baking time is too short, 10 mL sample aliquot recoveries between 94–110%. baking temperatures are too low, or centrifuged (10 min, the amount of added bromate is too 6000 rpm), analysis of the BENEFITS high. As potassium bromate is supernatant Selective and sensitive classified as a category 2B quantification of bromate in MISP carcinogen (possibly carcinogenic to complex food matrices Inline Dialysis humans) by the International Agency Sample preparation cartridges for Research on Cancer (IARC), it is EXPERIMENTAL are not necessary prohibited in any food. However, quality control is still necessary. Inline Dialysis automatically Minimized sample preparation removed matrix interferences. time due to Inline Dialysis Low concentrations of bromate in Pretreatment with sample flour are selectively and sensitively Excellent sensitivity with the preparation cartridges was not quantified with UV/VIS detection 947 Professional UV/VIS required. After chromatographic after separation on a Metrosep A Detector Vario separation, a PCR reagent was Supp 7 and post-column reaction added which allows the UV/VIS Method is compliant with (PCR) on a 940 Professional IC Vario detection at 352 nm of bromate ISO/DIN 11206 with a 947 Professional UV/VIS in the low µg/L range. Detector Vario SW.
Metrosep A Supp 7 - 250/4.0
Eluent 3.6 mmol/L Na2CO3 Flow 0.65 mL/min Bromate Temp 45 °C Injection 100 µL Detection UV/VIS 352 nm
UV/VIS signal of bromate (204 µg/L) in flour, after separation on a Metrosep A Supp 7 column and post-column 26 reaction with 0.5 mol/L potassium iodide.
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Additives, preservatives, nutrients Iodate in wheat powder
SUMMARY SAMPLES AND SAMPLE RESULTS PREPARATION Potassium iodate influences the final IC-C18 sample preparation quality of wheat-spelt baked goods Two types of wheat powder cartridges were necessary to remove organic matrix in different ways. Addition of 2 g sample dissolved in compounds. Two cartridges can potassium iodate reduces dough 0.1 mol/L NaOH (total volume be used in series, if required. development time and prolongs 100 mL) dough stability. Results of baking Iodate was reproducibly tests and sensory analyses have Sonicated for 20 minutes, determined in wheat powder in shown that products containing filtered through 0.2 µm filter, the low mg/L range. Spiking some potassium iodate have higher passed through IC-C18 sample tests with 5 mg/L iodate yielded volume and cambering in preparation cartridge in a recovery of 102%. comparison to control samples. MISP Higher doses of this additive BENEFITS negatively affect sensory parameters Inline Dialysis (optional) IC combined with an UV/VIS of final products. Enrichment of detector covers typical HPLC EXPERIMENTAL baked goods with potassium iodate applications Samples were analyzed with an not only helps to increase the daily Sufficient separation from 858 Professional Sample intake of iodine and but also interfering components while Processor and a 930 Compact IC positively affects rheological and keeping a short overall Flex. After separation on a sensory properties of final products. recording time of less than 10 Metrosep A Supp 5 column, the Here, a straightforward IC method minutes UV signal of iodate was with the Metrosep A Supp 5 column quantified within the Alternative method to for separation and UV/VIS detector concentration range of traditional titration (AOAC is shown to measure iodate in wheat 1–10 mg/L. Accuracy of the Official Method 956.03) in the mg/kg range. analysis was checked by spiking tests.
Metrosep A Supp 5 - 250/4.0
Eluent 3.2 mmol Na2CO3 + 1.0 mmol/L NaHCO3 Flow 0.7 mL/min Temp ambient Injection 20 µL Detection UV 215 nm
Chromatogram of the UV signal of a wheat powder sample, containing 89 mg/kg iodate. 27
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Additives, preservatives, nutrients Iodate and iodide in table salt
SUMMARY SAMPLES AND SAMPLE RESULTS PREPARATION Table salt may contain various The calibration range spanned additives that are beneficial to Straw mushroom table salt 5–100 µg/L iodide. The reduction of iodate to iodite by ascorbic humans. Iodate or iodide is often 0.1 g sample dissolved in water acid treatment was tested and added to salt as iodine plays an (total volume 100 mL) important role in the production of approved with standards thyroid hormone. Using iodized salt EXPERIMENTAL (500 μg/L). The conversion yielded >95%, aproving a in cooking helps to overcome goiter Samples were analyzed with an sucessful overal method (from a deficiency in iodine). Straw 889 IC Sample Center and a 930 performance. mushroom table salt contains straw Compact IC Flex, using a mushrooms, which contribute not Metrosep A Supp 7 column. Samples contained about only various mineral substances like Iodide was sensitively detected 20 mg/kg iodide. Treatment with iodide but also vitamin C, amperometrically using the direct ascorbic acid led to the same carbohydrates, and more than 18 current mode (DC 0.15 V). When result. Thus, total iodine content kinds of amino acids. Table salts are reducing the sample with was similar, which means that all subjected to quality control and their ascorbic acid (5 g/100 mL; 0.2 mL iodine was present as iodide. ionic components can be quantified added to the sample solution), all with IC. The determination of iodate iodate converts to iodide. Hence, BENEFITS and iodide in table salt is described total iodine content is Method according to SN/T in the Chinese norm SN/T 3727 [25]. determined in these samples. The 3727-2013 from AQSIQ The presented IC method with iodate content is calculated from Determination of the species amperometric detection quantifies the difference of total iodine and iodide and iodate iodide in the µg/L range in salt the iodide (a user-defined result samples. Dedicated sample in the MagIC Net software). Robust method that copes preparation allows to differentiate with various kinds of salt between iodide and iodate. samples
Metrosep A Supp 7 - 250/4.0
Eluent 9.0 mmol Na2CO3 Flow 0.7 mL/min Temp 40 °C Injection 100 µL Detection DC 0.15 V
Amperometric signal (DC mode) of a straw mushroom table salt containing 21.2 mg/kg iodide. Iodate was not found 28 in this sample.
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Dairy Lactose in low-lactose butter
SUMMARY SAMPLES AND SAMPLE results differed less than 6%. The method LOD is determined via Lactose-intolerance is a common PREPARATION signal to noise with 0.4 mg digestive problem due to the Low-lactose or lactose-free lactose/100 g. The method was deficiency of lactase. Lactase is the milk products (drinks, yogurt, developed following a call from essential enzyme to split the cheese, butter, chocolate) AOAC (Association of Official disaccharide lactose into its 0.1–5 g sample extracted in Agricultural Chemists) for a monomers glucose and galactose, water (total 50 g), then standardized method to which can be further metabolized. vortexed for 20 s determine low lactose contents Unsplitted lactose causes serious (AOAC 2018.001). problems in the intestine. Thus, MISP lactose-intolerant people rely on Inline Dialysis BENEFITS lactose-free or low lactose food and Separation of lactose from beverage, which can be industrially EXPERIMENTAL produced from milk products by lactulose and allo-lactose, Lactose in aqueous sample enzymatic hydrolysis of lactose. epilactose, galactosyllactose, extracts was separated from avoids false positive results An increasing global demand for other lactose derivates on a Determination of specific these products has also raised the Metrosep Carb 2 column using an carbohydrates, in contrast to need for a thorough quality control alkaline eluent (400 mM NaOH) determining the total in this sector. The remaining lactose and pulsed amperometric carbohydrate content content in the final product must be detection (flexIPAD). Calibration declared, e.g., when concentration for lactose ranged from No interferences from exceeds 1000 mg/kg product [26]. 0.05 mg/L to 80 mg/L. photometrically active This analytical method presented components, as often RESULTS here is straightforward and observed with competing accurately quantifies even lowest Sample preparation with either photometric methods concentrations of lactose in milk and Carrez precipitation or Inline Time and material saving easy milk products. Dialysis were compared, and sample preparation
Metrosep Carb 2 - 250/4.0 Eluent 400 mmol/L NaOH Flow 0.5 mL/min Temp 35 °C Injection 10 µL Detection flexIPAD
Amperometric signal of a low-lactose butter sample contaning residual lactose (0.4 mg/100 g). Injection was performed 29 after Inline Dialysis. Lactose was baseline separated from allo-lactose, epi-lactose, lactulose, and galactosyllactose.
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Dairy Carbohydrates in milk and milk products
SUMMARY SAMPLES AND SAMPLE RESULTS Detailed and proper food labeling is PREPARATION Results were obtained from a an increasing concern of regulatory Milk powders, coffee creamer, successful participation in a authorities and requested by many condensed milk, cream cheese, multilaboratory test (MLT) for educated consumers. ISO processed cheese qualifying ISO 22184. The amperometric detector cell with 22184:2021 describes an analytical Extraction/Carrez precipitation thin-layer geometry proved most method for the quantification of six as per ISO 22184:2021 different mono- and disaccharides suitable for heavily loaded (galactose, glucose, fructose, Dilution 10– or 50–fold samples. sucrose, lactose and maltose) in milk MISP All analytes were precisely and milk products with high quantified in seven blind MLT Inline Dilution (optional) performance anion exchange duplicate samples. Further chromatography with pulsed EXPERIMENTAL carbohydrates that might be amperometric detection (HPAEC- present in any sample (fucose, Samples were separated on a PAD) [27]. In contrast to classical melibiose, trehalose, lactulose, Metrosep Carb 2 column with a standard methods describing the and isomaltulose) were well binary high-pressure gradient. determination of a single separated from the six After post-column addition of carbohydrate in a certain food carbohydrates of interest. matrix, this method covers the six NaOH (0.3 mol/L) carbohydrates most important carbohydrates were detected with an optimized BENEFITS (galactose, glucose, fructose, wave form in PAD mode. Compliance with ISO sucrose, lactose, maltose) in different Calibration was from 22184:2021 matrices with a single analysis. 0.52–260 mg/L for glucose, galactose, fructose, sucrose, One method is suitable for This method determines the lactose, and maltose. Arabinose different milk products carbohydrate composition in milk was added to each sample and and milk products in accordance Minimal maintenance required used as internal standard (end with ISO 22184:2021. to clean auxiliary and working concentration 35 µg/L). electrode
Metrosep Carb 2 - 250/4.0 Eluent A: ultra pure water B: 0.4 mol NaOH + 2.0 mmol/L NaOAc Flow 0.8 mL/min Temp 25 °C Injection 5 µL Detection PAD, 0.65 V Amperometric signal (current) of a cream cheese sample, containing the major carbohydrates galactose 30 (0.393 g/100g), glucose (0.384 g/100g), and lactose (2.316 g/100g). Fructose, sucrose and maltose were below the calibrated concentrations. Arabinose was used as internal standard.
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Dairy Iodide in milk
SUMMARY SAMPLES AND SAMPLE methanol with a Metrohm PREPARATION Dosino. Iodine is an essential mineral to humans. The most important Organic or standard whole RESULTS function of iodine in the human milks, containing 3.5% fat The concentrations of free iodide body is its role in the production of 20–fold dilution in water (2.5 g ranged from 23.4 µg/L to thyroid hormones. These hormones milk per 50 g) 140.8 µg/L. Spiking tests showed are especially important for brain recoveries of 92–110% for iodide and neural development in infancy. MISP within the calibrated range. Major natural sources of iodine are Inline Dialysis seafood, eggs, and dairy products. BENEFITS Iodine deficiency and excess both Inline Dilution (optional) cause adverse health effects. Thus, Straightforward sample EXPERIMENTAL WHO gives recommendations for preparation without Carrez the total daily intake per age (e.g., Dialyzed samples were separated precipitation 150 µg/day for adults) [28]. If iodine on a Metrosep A Supp 17 column Efficient clean up of samples is added during food manufacturing, within 10 minutes. The from fats, proteins, and other it must be listed on the Nutrition amperometric detection of iodide higher molecular weight Facts label (FDA) [29]. was executed with direct current compounds with Low Volume within a range of 2–50 µg/L. The presented IC method excels with Inline Dialysis Electrodes were automatically simple and time-saving sample Precise determination of cleaned after each injection («CV preparation. Low Volume Inline iodide in milk products in the treatment», patent filed) with Dialysis requires small sample µg/L range flexIPAD cleaning. The sample volumes and provides for an path was kept clean by rinsing it Less maintenance of electrodes automatic clean-up. Maintenance is with methanol (10% v/v). The due to automatic cleaning minimized as the sample flow path solution was automatically cycles with «CV treatment» as well as electrodes are cleaned prepared from water and (patent filed) automatically after each injection.
Metrosep A Supp 17 - 150/4.0 Eluent 60 mmol NaOH + 20 mmol/L NaOAC Flow 0.6 mL/min Temp 35 °C Spiked sample Injection 80 µL Sample Detection DC, 0.05 V
Overlay of a chromatogram from a milk sample (20–fold dilution), containing 148 µg/L iodide (lower chromatogram), 31 and from a milk sample spiked with 100 µg/L iodide (upper chromatogram). The recovery was 102%.
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Dairy Nitrite and nitrate in milk products
SUMMARY SAMPLES AND SAMPLE cheese samples were further diluted (2–100-fold). Spiking tests In higher concentrations, nitrite can PREPARATION with nitrate and nitrite (0.1 mg/L react to form carcinogenic Milk powder, whey, and each) showed recoveries of nitrosamines or influence the oxygen cheese 90–120%. Milk samples transport in blood, causing 1 g sample in ≈60 mL water is contained <0.5 mg nitrite and methemoglobinemia. Sources for heated at 45 °C for 20 min. between 0.5–5 mg nitrate per nitrate and nitrite in milk are milk Afterwards, the volume is 100 g. Optionally, a UV/VIS powder preservatives, contaminated adjusted to 100 mL Detector can be placed in series animal feed, or fertilizers. Currently, after the conductivity detector for legal limits are not defined for nitrite MISP more sensitive detection of and nitrate in milk. However, the Inline Dialysis nitrite, nitrate, and bromide. Expert Committee from WHO (World Especially, as chloride is not UV Health Organization) and FAO (Food EXPERIMENTAL active, this is preferable for and Agriculture Organization) After Inline Dialysis, analytes are samples with high chloride recommends an acceptable daily separated on a Metrosep contents in the matrix. intake per kg body weight of 0.07 A Supp 5 column using a Dose-in mg for nitrite and gradient (A: 2.0 mmol Na CO + BENEFITS 3.7 mg for nitrate [30]. 2 3 2.0 mmol/L NaHCO3 + 2.5% Straightforward sample IC with Metrohm Inline Dialysis and acetone; B: 20.0 mmol Na2CO3 + preparation, no need for suppressed conductivity detection 2.0 mmol/L NaHCO3 + 2.5% sample preparation cartridges offers a straightforward analytical acetone). Calibration ranged Less consumables and less time technique to analyze the content of from 0.05 to 25 mg/L for all due to Inline Dialysis nitrate and nitrite in various milk analytes. products. Other anions like chloride, Dose-in gradient to accelerate phosphate, sulfate, or citrate can be RESULTS late-eluting peaks quantified in the same run. Milk samples were directly Robust and easy-to-handle injected, whereas the whey and method for anions in milk
Metrosep A Supp 5 - 250/4.0 Eluent Dose-in gradient (Na2CO3 + NaHCO3 + acetone) Flow 0.7 mL/min Temp 40 °C Injection 20 µL Detection Conductivity Suppressed conductivity signal for the analysis of a milk powder sample, containing chloride (11.5 mg/100 g), phosphate 32 (104.0 mg/100 g), and citrate (63.3 mg/100 g) as major inorganic anions, as well as nitrate (0.2 mg/100 g) and sulfate (2.6 mg/100 g). Nitrite was less than 0.5 mg/100 g.
RETURN TO TOP 32 robust and easy. robust and sensitive, be showedcholine to conductivity, detectionthe of - non with Even detection. conductivityby isocratic elution aftercholine determination of method shows the IC the SMPR 2012.013,withAOAC In line choline. total detection of the enables sphingomyelin and and lecithin fromcholine e.g., hydrolysisacidic to release bound preparationSample involves 32]. methods for its quantification [31, proposed have GB chromatographic and formulas.various infant AOAC common in supplement a ischoline importance,nutritional its to Due performance. physical and for fitness mental i.e., brain, the to transmissionfor the nerve signals of membranescomponentscell the in phospholipids necessaryare other mammals.many Choline and micronutrient, essential for humans water a Choline is SUMMARY Non analysis Detection Injection Temp Flow Eluent M e - t suppressed r o s IC for food &beverage analysis was e p C performed
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5% acetone Conductivity 20 µL 30 mL/min 0.9 HNO mmol/L 6.0 - conductivity 1 5 ° -soluble C 0 / 4 according . 0 suppressed signal to 3 of + requirements 2012.013 for. AOAC a powder milk on the high-capacity the on cation as separated Choline was EXPERIMENTAL MISP quality checks and validation, validation, checks and quality with direct conductivity. For minutes was detected13 and after elutes conditions. It column6 C using isocratic PREPARATION SAMPLE ANDSAMPLES formula milkformula powder Cholinein infant Dairy Inline Ultrafiltration (optional) (optional) Inline Dilution dilution and NaOH), adjustment to 2 to adjustment filtration (0.22 µm), pH rpm),Centrifugation (10,000 70 with 30mL mol/L)(1HCl at Acidic Acidic powder formula milk women pregnant/lactating -, childrenInfant sample, sample, RETURN TO TOP ° C for 3 hrs. 3 for C hydolysis containing – - of 5 g sample sample g 5 of , and , and 7 (50% Metrosep 20 mg/L 20 mg/L . Sample choline. Sample BENEFITS between results). RSD comparable results(<10% laboratories achieved five independent 2012.013, SMPR AOAC verification of mg/100g.1.02 Within method a was LOQ RSD. showed <3% RSDs samples of 200 Repeatability 50 for complied with the requirements They powderanalyzed. were milk seven brands of samples of Nine RESULTS is recommended. 1849a SRM NIST material of standard analysis conductivity - non and isocratic elution with setup -to easy and Robust possible Inlinepreparation sample AOACSMPR 2012.013 with method Compliance – 400 mg choline400 mg g.per 100 preparation suppressed suppressed
and Choline - handle 33 33 IC for food & beverage analysis
Further applications in brief
Analytes Matrix Technique Advantages
Anions, e.g., chloride, Fruit juice IC with Metrohm Inline Dilution Optimized settings, e.g., adjustment of the sample nitrate, sulfate concentrates Technique (MIDT) and Inline needle depth in a zone without pulp to avoid filter Ultrafiltration (UF) clogging.
Cations, e.g., Mineral water IC with Metrohm intelligent Non-suppressed conductivity is a robust and easy ammonium, Preconcentration Technique technique, compared to suppressed cation analysis. manganese, sodium, (MiPCT) MiPCT guarantees low detection limits and. The potassium system is automatically calibrated with one standard solution.
Food preservatives, Flavored bottled IC with conductivity detection Solvent extractions or sample derivatization is not e.g., sorbate and water after inverse suppression necessary, in contrast to many GC methods. Counter benzoate cations can be determined with a second analysis channel.
Chloride, nitrite, Whey, cheese, IC with Inline Dialysis as Gradient for optimal separation of all components in a nitrate, phosphate, milk powder automatic sample preparation single analysis. sulfate, citrate
Melamine Milk powder IC with Inline Dialysis and UV/VIS The technique is specific for melamine, in contrast to detection the non-specific nitrogen determination according to Kjeldahl. Illegal melamine addition is recognized. Complex GC/MS or LC/MS methods are not necessary.
Fructans Infant formula IC with a flow gradient and The method works without any additional sample pulsed amperometric detection derivatization. Thanks to the flow-gradient, only one (PAD) eluent and one high-pressure pump are necessary. The method was validated by successful participation in the multilaboratory trial for acceptance of ISO 22579/AOAC 2014.14). Carbohydrates, e.g,. Soft drinks, e.g. IC with isocratic elution and PAD Simple and robust system setup. glucose, fructose, cola sucrose
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Further applications in brief (cont.)
Analytes Matrix Technique Advantages
Cations, e.g., lithium, Skimmed milk IC with Inline Dialysis and non- Fully automated Metrohm Inline Dialysis reduces sodium, ammonium, suppressed conductivity manual sample preparation steps to a minimum. potassium, detection magnesium, calcium
Lactate and cations, Lactoserum IC with non-suppressed Separation and quantification of (anionic) lactate and e.g., sodium, powder conductivity detection cations in a single run on the same analysis channel is potassium, less complex than AAS or ICP/MS analysis. magnesium, calcium
Thiocyanate Formulated milk IC with sequential suppressed The Metrohm Suppressor Module (MSM) shows powder and liquid and conductivity detection outstanding performance, even when organic solvents milk are present in the eluent (here: 5% acetone). The setup guarantees stable results and robust long-time performance.
Stabilizers and flavor Shrimp, seafood IC with Inline Ultrafiltration and This simple and robust method determines the enhancers, e.g., Metrohm intelligent partial loop distribution of polyphosphate chain lengths, which polyphosphates technique (MiPT) gives valuable information about sequestering and (pyrophosphate, dispersing properties, whereas end-group titration trimetaphosphate, methods only provide an average for polyphosphate tripolyphosphate) chain lengths.
Clogging of the analytical system is excluded due to Metrohm Inline Ultrafiltration. Acrylamide Potato chips IC with mass spectrometric Coupling an IC with a mass detector guarantees detection selective and sensitive detection of the analyte of interest. Automated calibration is possible.
Sulfite Foodstuffs, e.g,. IC with amperometic detection This fast and accurate method is selective for sulfite chickpeas, (DC mode) and automated and replaces labor-intensive solution extraction as mustard, cherries, electrode cleaning sample preparation. capers, canned garlic, chili pepper, red wine
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IC compliance with norms and standards
Standards are the basis of national laws which give detailed instructions on the analytical method requirements [33].
Analytes Matrix Norm or standard
Bromate Water ISO 15061: 2001 Water quality — Determination of dissolved bromate — Method by liquid chromatography of ions Bromate Water ISO 11206: 2011 Water quality — Determination of dissolved bromate — Method using ion chromatography (IC) and post column reaction (PCR) Bromide, bromate, chloride, Water EPA Method 300.1 Determination of inorganic anions in drinking water by ion chlorite, chlorate, fluoride, chromatography nitrate, nitrite, phosphate, sulfate, dichloroacetate Bromide, chloride, fluoride, Water ISO 10304-1: 2007 Water quality — Determination of dissolved anions by liquid nitrate, nitrite, phosphate chromatography of ions — Part 1 and sulfate Chlorate, chloride, chlorite Water ISO 10304-4: 1997 Water quality — Determination of dissolved anions by liquid chromatography of ions — Part 4 Choline Infant Formula, AOAC Official Method 2012.20 Choline in infant formula and adult nutritionals ion Adult Nutritionals chromatography and suppressed conductivity Chromate, iodide, sulfite, Water ISO 10304-3: 1997 Water quality — Determination of dissolved anions by liquid thiocyanate, thiosulfate chromatography of ions — Part 3
Chromium Water AOAC Official Method 993.23 Dissolved hexavalent chromium in water
Chromium Water DIN 38405-52 German standard methods for the examination of water, wastewater and sludge – Anions (group D) – Part 52: Photometric Determination of dissolved chromium(VI) in water (D 52) Fluoride, chloride, nitrite, Water AOAC 993.30 Inorganic anions in water nitrate, phosphate, sulfate Fructans Foodstuff, e.g., AOAC Official Method 997.08 Fructans in food products cheese spread, chocolate, wine gum, drink mix, biscuits Fructans, glucose, fructose Infant Formula, AOAC Official Method 2016.14 Fructans in infant formula and adult nutritionals [34] Adult Nutritionals Fructans, glucose, fructose Infant Formula, ISO 22579: Infant formula and adult nutritionals — Determination of fructans — High Adult Nutritionals performance anion exchange chromatography with pulsed amperometric detection (HPAEC-PAD) after enzymatic treatment [34] Galactose, glucose, fructose, Milk and milk ISO 22184: 2021 [IDF 244] Milk and milk products — Determination of the sugar sucrose, lactose, maltose products contents — High performance anion exchange chromatography with pulsed amperometric detection method (HPAEC-PAD) [27] Glucose, fructose Cane Sugar AOAC Official Method 2000.17 Determination of trace glucose and fructose in raw cane sugar Glucose, fructose Raw sugar or ICUMSA Method GS1/2/3-4 (1998) The Determination of glucose and fructose in raw processed sugar and white sugars using high performance anion-exchange chromatography (HPAEC) – official 36
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IC compliance with norms and standards (cont.)
Metrohm ion analysis also offers equipment for titration and voltammetry, and pH value measurement to fulfill standards for the analysis of beverages.
Analytes, Matrix Norm or standard
Glucose, fructose, sucrose Cane and beet AOAC Official Method 996.04 Sugars in cane and beet final molasses final molasses Glucose, fructose, sucrose Cane juices, cane ICUMSA Method GS7/8/4-24 (2011) The determination of glucose, fructose and syrups, cane and sucrose in cane juices, syrups and molasses and of sucrose in beet molasses by high beet molasses performance ion chromatography – official method Iodide Pasteurized liquid AOAC Official Method 992.22: Iodine (as iodide) in pasteurized liquid milk and skim milk, skim milk milk powder powder Lactose Lactose-free and AOAC SMPR 2018.009 Standard Method Performance Requirements (SMPR®) for low-lactose milk lactose in low-lactose or lactose-free milk, milk products and products containing products dairy ingredients Lithium, sodium, Water DIN EN ISO 14911 - 1999: Water quality - Determination of dissolved Li, Na, ammonium, potassium, ammonium, K, Mn(II), Ca, Mg, Sr and Ba using ion chromatography manganese, calcium, magnesium, strontium, barium Mannitol, arabinose, Instant coffee AOAC Official Method 995.13 Carbohydrates in soluble (instant) coffee - anion- galactose, glucose, exchange chromatographic method with pulsed amperometric detection mannose, fructose, ribose, xylose, sucrose, fucose Mannitol, arabinose, Instant coffee DIN 10780 (2003)/ISO 11292: 1995 Instant coffee - Determination of free and total glucose, galactose, sucrose, carbohydrate contents - method using high-performance anion-exchange xylose, mannose, fructose chromatography Mannitol, Glucose, Fructose, Beet juice and ICUMSA Method GS8-26 (2013) The determination of mannitol, glucose, fructose, Sucrose cane juice sucrose and raffinose in beet brei and beet juices by HPAEC-PAD Myo-Inositol Infant and AOAC Official Method 2011.18 Myo-inositol (free and bound as phosphatidylinositol) pediatric formula, in infant and pediatric formula and adult nutritionals adult nutritionals Myo-Inositol Infant formula, ISO 20637: 2015 Infant formula and adult nutritionals — Determination of adult nutritionals myoinositol by liquid chromatography and pulsed amperometry Perchlorate Water ISO 19340: 2017 Water quality — Determination of dissolved perchlorate — Method using ion chromatography (IC) Polydextrose Various foodstuff AOAC official Method 2000.11 Polydextrose in food Propionic acid Cheese ISO/TS 19046-2: 2017 Cheese — Determination of propionic acid level by chromatography — Part 2: Method by ion exchange chromatography Raffinose Beet molasses and ICUMSA Method GS4/8-19 (2005) The Determination of raffinose by high beet sugar performance anion-exchange chromatography (HPAEC) – in impure beet sugar products – official Sulfite Brown Sugar ICUMSA Method GS 3-52 (2019) Sulfite as SO2 in brown sugars by the optimized Monier-Williams and HPIC single method Trans- Foodstuff, e.g., AOAC Official Method 2001.02: Determination of trans-galactooligosaccharides Galactooligosaccharides custard, cereal, (TGOS) in selected food products 37 (TGOS) yogurt drink, biscuits, syrup
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Time and money savers – Food analytics is a wide and comprehensive area. Samples are very complex, as are their automation and processing and analysis.
Metrohm Inline Sample Automation and MISP help to save valuable Preparation (MISP) laboratory time during processing, while increasing precision and robustness of results.
Real-world samples not only contain the target components, but also matrix components which can be aggressive and affect and degrade the system, leading to clogging or precipitation in the system. Therefore, proper sample preparation is essential for reliable and accurate analysis and for protection of the column and system. Metrohm offers a variety of automated Inline Sample Preparation Techniques (MISP), are fully integrated into the system sparing the user from tedious manual work and saving a substantial amount of time.
INLINE ULTRAFILTRATION INLINE DIALYSIS … is a fast and cost-effective alternative to manual … is the answer to complex sample matrices. This filtration with cartridges and syringes. The frequent technique separates not only particles from their replacement of filters after each single injection or analytes, but also colloids, oil components, and large manual filtration make this process costly, time molecules. Samples containing proteins can be consuming and wasteful. injected directly after Inline Dialysis, which saves time- Metrohm Inline Ultrafiltration is a fully automated consuming manual steps such as the removal of solution, using membrane filters with a pore size of proteins with Carrez precipitation. 0.2 µm. They can be applied to multiple samples, standards, and blanks with a carryover of < 0.1%. Applications: Concentrated fruit and vegetable juices, dairy products and other protein-containing samples, Applications: Diluted fruit and vegetable juices, e.g., flour and honey, emulsions, dispersions, oil- drinking water, extracts, digestion solutions, and containing samples, fermentation samples, and samples slightly or moderately contaminated with samples heavily contaminated with particles, algae, or particles, algae, or bacteria. bacteria.
Acceptor solution
Sample side
Metrohm Ultrafiltration cell 2: The two parts of the Ultrafiltration cell are separated by a filter membrane. On one Stopped-Flow Dialysis: Sample is continuously pumped on the side, the sample is carried through the cell at a constant flow sample side. After rinsing, the acceptor stream is stopped. Due rate. On the other side, some of the sample is drawn off to a concentration gradient, the ions pass through the through the membrane and transported to the injection valve. membrane until an equilibrium between acceptor and original 38 The formation of filter cake is prevented by continuous flushing solution is reached. Afterwards, the acceptor solution is injected of particles out of the cell at a high flow rate. directly into the IC.
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Time and money savers – Automation and logical features support reliability and accuracy of the results by automation and omitting manual error-prone steps. Metrohm Inline Sample Preparation (MISP)
Dilution is a routine procedure in sample analysis. It is still often performed manually and therefore is error-prone and time-consuming. The Metrohm Inline Dilution Technique (MIDT) or Metrohm intelligent Partial Loop Technique (MiPT) offer a precise, accurate, and fully automated alternative to manual dilution as well as the solution for automated calibration of the system over several orders of magnitude regarding concentrations of target analytes. The software MagIC Net can handle logical decision, a way to further optimize sample processing. MIDT The system automatically calculates the optimum dilution factor and analyzes the sample. Thus, your … provides automatic dilution of the sample results are always reliable, because they are depending on either a predefined or an automatically always within the calibration range. calculated optimum dilution factor (Logical Inline Dilution). Standards can also be diluted. The system MiPT dilutes the standard with different dilution factors … automatically adjusts the injection volume to and thus carries out multi-point calibration. Sample the concentration of the sample. This technique concentrations in the range of 1:10,000 can be ensures that the results are always within the analyzed reliably with a single automated calibration. calibration range. Injection volumes of anything MIDT can be combined with Inline Ultrafiltration and between 2 and 200 µL are possible. The optimum Inline Dialysis. injection volume is automatically calculated, making it possible to cover a very wide range of sample concentrations. Furthermore, this LOGICAL INLINE DILUTION technique is almost free of any carryover A further advantage of Metrohm IC is Logical Inline (<0.001%), enabling sequential analysis in the Dilution. The sample just needs to be placed on the mg/L and µg/L range. autosampler and the analysis is started. MiPT is characterized by outstanding linearity over the entire volume range. For this reason, this technique can also be used for automatic calibrations using a single multi-component standard.
Learn more about Metrohm’s automation and sample preparation:
• Monograph: Sample Preparation Techniques for Ion Chromatography • Brochure: Metrohm Inline Sample Preparation – IC analyses as simple as possible Logical dilution: If the sample concentration is outside the • Automation in ion chromatography – Save calibration range, it is diluted with the optimum dilution factor time and money through fully automated 39 and analyzed again. Hence, your results are always within the calibration range. sample preparation and analysis
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Learn more about IC IC in brief
From routine IC analysis to research and development, and from stand-alone analyzers to fully automated systems: Metrohm offers solutions for automated IC including inline sample preparation and separation columns for anions, cations, and carbohydrates in almost any sample matrix. Data integrity is guaranteed. Monograph Ion Chromatography Monograph – Practical Ion Chromatography – An Introduction Monograph: Sample Preparation Techniques for Ion Chromatography
A 3-year instrument warranty and 10-year warranty on our anion suppressor say it all about the robust Swiss quality of our high-pressure ion chromatographs (HPIC). Brochure: Suppression in anion chromatography – More sensitive analysis of anions and organic acids STREAM – the green way of suppression
Ion analysis with Metrohm: High-performance IC systems Complete automation for high sample throughput Highest sensitivity for lowest detection limits Compant with GLP and the FDA regulations Wide range of detection options including conductivity, UV/VIS, amperometry, ...
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DetectionDetectiontechniquestechniques ConductivityConductivity
IC ConductivityIC ConductivityDetectorDetector
AlmostAlmostevery ioniceverycompoundionic compoundgives agivessignala signalwith conductivitywith conductivitydetectiondetection. A conductivity. A conductivitydetectordetectoris a universalis a universal detectordetectorfor multifor-ionmultianalysis-ion analysisin foodinandfoodbeverageand beveragesamplessamples. It is .theIt isdetectorthe detectorof choiceof choicewhen whenusing ICusingas IC as separationseparationtechniquetechnique. The. intelligentThe intelligenthigh-performancehigh-performanceconductivityconductivitydetectordetectorfrom fromMetrohmMetrohmexcels excels with robustnesswith robustnessand a veryandlowa verybaselinelow baselinenoise ofnoiseless ofthanless0.than2 nS/cm0.2 nSunder/cm standardunder standardoperationoperationconditionsconditions. .
LowmaintenanceLow maintenancecosts andcostslongandlifetimelong lifetime
Robust RobustSwiss qualitySwiss quality
Highest Highestsensitivitysensitivityfor lowestfor lowestdetectiondetectionlimits limits
For routine For routineanalysesanalysesand researchand researchapplicationsapplicationsin the ng/Lin the- tong/L%--rangeto %-range
DetectionDetectiontechniquestechniques UV/VISUV/VIS detection detection
947 Professional947 Professional UV/VIS Detector UV/VIS Detector
UV/VISUV/VISdetectiondetectionenablesenablesreliablereliableand accurateand accuratequantificationquantificationof substancesof substancesthat absorbthat absorblight inlightthe ultravioletin the ultravioletor or visible visiblerange.rangeIC applications. IC applicationswith UV/VISwith UV/VISdetectiondetectionfrom thefromfoodtheandfoodbeverageand beveragesector oftensectorinvolveoften involvesamplessampleswith with salty matricessalty matrices. Since.chlorideSince chloridefrom saltfromdoessaltnotdoescausenot majorcause interferencesmajor interferenceswith UV/VISwith UV/VISdetectiondetectionit is suitableit is suitablefor for e.g., determinatione.g., determinationof nitrateof nitrateand nitriteand innitritesausagesin sausages. . With additionalWith additionalpre-columnpre-columnor postor-columnpost-columnreactionreaction(PCR) many(PCR) additionalmany additionalsubstancessubstancescan becantransformedbe transformedinto into UV-activeUV-oractiveVIS-activeor VIS-molecules,active molecules,which makeswhich makesthese substancesthese substancesalso detectablealso detectable. . The intelligentThe intelligentmulti-wavelengthmulti-wavelengthdetectordetectorfrom Metrohmfrom Metrohmhas severalhas severalwavelengthswavelengthsthat canthatbecanfreelybe selectedfreely selected. A . A diode arraydiodeisarrayusedisforuseddetectionfor detection. .
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DetectionDetectiontechniquestechniques AmperometryAmperometry
Wall-JetWall Cell-Jetwith Cellelectrodeswith electrodesfor amperometricfor amperometricdetectiondetection
IC equippedIC equippedwith anwithamperometrican amperometricdetectordetectoropensopensthe doorthe todooranalyzeto analyzealmostalmostany ionsanythationscanthatbecanoxidizedbe oxidizedor or reduced,reduced,e.g., ecarbohydrates,.g., carbohydrates,glycosides,glycosides,fructansfructans, alcohols,, alcohols,amines,amines,aminoaminoacids,acids,phenols,phenols,organosulfurorganosulfur compounds,compounds,cyanide,cyanide,sulfide,sulfide,ascorbicascorbicacid, vitaminsacid, vitaminsand manyand manymore.more. The analysisThe analysisof carbohydratesof carbohydrates(sugars)(sugars)is of isparticularof particularinterestinterestbecausebecausenot onlynot isonlytheistotalthe totalsugarsugarcontentcontent determined,determined,but thebutdistributionthe distributionand amountand amountof distinctof distinctcarbohydratescarbohydratescan alsocanbealsoanalyzedbe analyzed. The .amperometricThe amperometric detectordetectorfrom fromMetrohmMetrohmhas ahasthreea -threeelectrode-electrodeconfigurationconfigurationthat thatensuresensuresexcellentexcellentsignalsignal-to-noise-to-noiselevels.levels. NumerousNumerouselectrodeselectrodesand accessoriesand accessoriesare availableare availableto fit forto fiteveryfor everyapplicationapplicationneed.need. AmperometricAmperometricdetectiondetectionis muchis muchmore moresensitivesensitivethan thanrefractiverefractiveindexindexdetection,detection,whichwhichallowsallowsthe injectionthe injectionof of highlyhighlydiluteddilutedsamplessamplesin orderin orderto keepto thekeepsystemthe systemclean cleanand safeguardand safeguarduninterrupteduninterruptedoperationoperationof theofsystemthe systemfor for a longaperiodlong periodof timeof. timeThe system. The systemhas selfhas-monitoringself-monitoringfunctionalitiesfunctionalitiesfor fullfortraceabilityfull traceabilityand toandminimizeto minimizethe risktheofrisk of operatingoperatingerrorserrors. .
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CardiovascularCardiovasculardiseases,diseases,obesity,obesity,and diabetesand diabetesare thearemajorthe majorcausescausesof deathof deathin ourinsocietyour society. They. areTheyconnectedare connectedto to our nutritionalour nutritionalpracticepractice. WHO. WHOrecommendsrecommendsrestrictingrestrictingthe intakethe intakeof freeof sugarsfree sugars(monosaccharides(monosaccharidesand and disaccharides)disaccharides)to lesstothanless 10than% of10%totalof energytotal energyintakeintakein orderin orderto reduceto reducethe risktheofrisknoncommunicableof noncommunicablediseasesdiseases (NCD),(NCD),with awithparticulara particularfocus focuson theonpreventionthe preventionand controland controlof unhealthyof unhealthyweightweightgain andgaintoothand toothdecaydecay[35]. Even[35]. Even in Switzerland,in Switzerland,daily dailyconsumptionconsumptionof freeof sugarsfree sugarsper personper personper dayper isdayaboutis aboutfive timesfive timeshigherhigherthan thanthe the recommendedrecommendedintakeintake[36]. [36]. ManufacturingManufacturingof healthyof healthyproductsproductsrelies relieson dedicatedon dedicatedanalysisanalysisof foodstuffsof foodstuffsfor qualityfor qualitycontrolcontrolduringduringthe the productionproductionprocessprocess. Detailed. Detailedfood labelingfood labelingcan helpcantohelpincreaseto increaseawarenessawarenessand enableand enableconsumersconsumersto maketo makehealthyhealthy decisionsdecisions. Metrohm. MetrohmIC offersIC offersanalyticalanalyticalsolutionssolutionsto tackleto tacklethesethesechallengeschallengesin theinfoodtheandfoodbeverageand beverageindustriesindustries. .
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ReferencesReferences
[1] FAO[1] (Food FAO and (Food Agriculture and AgricultureOrganizationOrganizationof the Unitedof the UnitedNations Nations) (2005),) (2005), Codex generalCodex generalstandardstandardfor for fruit juicesfruitandjuices nectarsand nectars(CODEX(CODEX STAN 247 STAN-2005), 247-www.fao.org/input/download/standards/CXS_247e2005), www.fao.org/input/download/standards/CXS_247e (accessed(accessed Apr 1, 2021).Apr 1, 2021). [2] Nakakuki[2] Nakakuki, T. (2002),, T. (2002), Present Present status and status future and offuture functional of functional oligosaccharide oligosaccharide development development in Japan, in Japan, Pure andPure Applied and Applied Chemistry. Chemistry. 74 (7): 124574 (7):–1251, 1245 –doi:10.1351/pac200274071245.1251, doi:10.1351/pac200274071245. S2CID 35500606 S2CID 35500606 (accessed(accessed Apr 1, 2021).Apr 1, 2021). [3] EFSA[3] (European EFSA (European Food Safety Food AuthoritySafety Authority ), Aspartame, ), Aspartame, www.efsa.europa.eu/en/topics/topic/aspartame www.efsa.europa.eu/en/topics/topic/aspartame (accessed(accessed Apr 1, 2021).Apr 1, 2021). [4] WHO[4] (World WHO (WorldHealth HealthOrganization) Organization) Technical Technical Report ReportSeries 837 Series (Geneva 837 (Geneva 1993), Evaluation1993), Evaluation of certain of certain food additivesfood additives and contaminants, and contaminants, WHO_TRS_837.pdf; WHO_TRS_837.pdf; (accessed (accessed Apr 1, 2021).Apr 1, 2021). [5] Morrison,[5] Morrison, O. (2020), O. (2020), Food standards Food standards agencies agencies rule out rule aspartame out aspartame bans as bans scientists as scientists warn of warn ‘adverse of ‘adverse effects’effects’ on consumers, on consumers, foodnavigator.com foodnavigator.com https://www.foodnavigator.com/Article/2020/11/13/Food https://www.foodnavigator.com/Article/2020/11/13/Food- - standardsstandards-agencies-agencies-rule-out-rule-aspartame-out-aspartame-bans-as-bans-scientists-as-scientists-warn-of-warn-adverse-of-adverse-effect--oneffect-consumers-on-consumers (accessed (accessed Apr 1, 2021).Apr 1, 2021). [6] Bernadene[6] Bernadene, A. et al., A. (2017), et al. (2017), Critical Criticalreview reviewof the current of the current literature literature on the onsafety the of safety sucralose, of sucralose, Food and Food and ChemicalChemical Toxicology Toxicology 106 (A), 106 324 (A),-355. 324-355. [7] Friedman,[7] Friedman, M. A. (1998), M. A. (1998), Lead Deputy Lead Deputy Commissioner Commissioner for the forFDA, the Food FDA, Additives Food Additives Permitted Permitted for Direct for Direct AdditionAddition to Food to for Food Human for Human Consumption; Consumption; Sucralose Sucralose Federal Federal Register: Register: 21 CFR 21Part CFR 172, Part Docket 172, Docket No. 87F No.- 87F- 0086. 0086. [8] US FDA[8] US (US FDA Food (US and Food Drug and Administration) Drug Administration) (2006), (2006), Food labeling: Food labeling: health claims;health claims;dietary dietarynoncariogenic noncariogenic carbohydratecarbohydrate sweeteners sweeteners and dental and caries,dental Federalcaries, Federal Register. Register. 71 (60): 71 15559 (60):– 1555964. PMID–64. 16572525. PMID 16572525. [9] US FDA[9] US (US FDA Food (US and Food Drug and Administration) Drug Administration) (2019), (2019), Detention Detention without without physical physical examination examination of Stevia of Stevia leaves, leaves,crude extracts crude extracts of Stevia of leavesStevia andleaves foods and containing foods containing Stevia leavesStevia and/orleaves and/orStevia extracts, Stevia extracts, Import Import Alert 45Alert-06. 45-06. [10] WHO[10] (World WHO (WorldHealth HealthOrganization) Organization) (2005), (2005), Bromate Bromate in Drinking in Drinking-water,- Backgroundwater, Background document document for for developmentdevelopment of WHO of Guidelines WHO Guidelines for Drinking for Drinking-water -Quality,water Quality, WHO/SDE/WSH/05.08/78 WHO/SDE/WSH/05.08/78 www.who.int/water_sanitation_health/dwq/chemicals/bromate260505.pdfwww.who.int/water_sanitation_health/dwq/chemicals/bromate260505.pdf (accessed (accessed Apr 1, 2021).Apr 1, 2021). [11] WHO[11] (World WHO (WorldHealth HealthOrganization) Organization) (2005), (2005), Glyphosate Glyphosate and AMPA and inAMPA Drinking in Drinking-water,- Backgroundwater, Background documentdocument for development for development of WHO of Guidelines WHO Guidelines for Drinking for Drinking-water -Quality,water Quality, WHO/SDE/WSH/03.04/97, WHO/SDE/WSH/03.04/97, IARC MonographsIARC Monographs Vol. 112: Vol. evaluation 112: evaluation of five organophosphateof five organophosphate insecticides insecticides and herbicides and herbicides https://www.iarc.who.int/wphttps://www.iarc.who.int/wp-content/uploads/2018/07/MonographVolume112-content/uploads/2018/07/MonographVolume112-1.pdf (accessed-1.pdf (accessed Apr 1, Apr 1, 2021). 2021). [12] US[12] EPA US (US EPA Environmental (US Environmental Protection ProtectionAgency)Agency) (2019), (2019), EPA Takes EPA Next Takes Step Next in StepReview in Review Process Process for for HerbicideHerbicide Glyphosate, Glyphosate, Reaffirms Reaffirms No Risk No to RiskPublic to Health,Public Health, News Releases News Releases from Headquarters from Headquarters on Chemical on Chemical Safety andSafety Pollution and Pollution Prevention Preventionhttps://www.epa.gov/newsreleases/epahttps://www.epa.gov/newsreleases/epa-takes-next-takes-step-next-review-step--reviewprocess-process- - herbicideherbicide-glyphosate-glyphosate-reaffirms-reaffirms-no-risk--nopublic-risk--healthpublic-(accessedhealth (accessed Apr 1, 2021).Apr 1, 2021). [13] US[13] EPA US (US EPA Environmental (US Environmental Protection ProtectionAgency)Agency) (2009), (2009),NationalNational Primary Primary Drinking Drinking Water Regulations,Water Regulations, EPA 816EPA-F-09 816-004-F-09 https://www.epa.gov/ground-004 https://www.epa.gov/ground-water--andwater-drinking-and-drinking-water/national-water/national-primary-primary-drinking-drinking- - water-regulationswater-regulations(accessed(accessed Apr 1, 2021).Apr 1, 2021).
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References (cont.) References (cont.)
[14] US EPA (US Environmental Protection Agency) (1995) National primary drinking water regulations, [14] US EPA (US Environmental Protection Agency) (1995) National primary drinking water regulations, glyphosate, EPA 811-F-95-003q-T. glyphosate, EPA 811-F-95-003q-T. [15] Anvisa (Brazilian Health Regulatory Agency) (2021), Glifosato, www.gov.br/anvisa/pt- [15] Anvisa (Brazilian Health Regulatory Agency) (2021), Glifosato, www.gov.br/anvisa/pt- br/setorregulado/regularizacao/agrotoxicos/monografias/monografias-autorizadas/g-h-i/4378json-file- br/setorregulado/regularizacao/agrotoxicos/monografias/monografias-autorizadas/g-h-i/4378json-file- 1/view (accessed Apr 1, 2021). 1/view (accessed Apr 1, 2021). [16] Waterhouse et al. (2016), Understanding Wine Chemistry, John Wiley & Sons, UK, ISBN 1118627806. [16] Waterhouse et al. (2016), Understanding Wine Chemistry, John Wiley & Sons, UK, ISBN 1118627806. [17] OIV (International Organization of Vine and Wine) (2021), OIV, France, ISBN 978-2-85038-030-3. [17] OIV (International Organization of Vine and Wine) (2021), OIV, France, ISBN 978-2-85038-030-3. [18] Konakovsky, V. et. al. (2010) Levels of histamine and other biogenic amines in high quality red wines, [18] Konakovsky, V. et. al. (2010) Levels of histamine and other biogenic amines in high quality red wines, Food Additives and Contaminants - Part A Chemistry, Analysis, Control, Exposure and Risk Assessment Food Additives and Contaminants - Part A Chemistry, Analysis, Control, Exposure and Risk Assessment 28(4):408-16 28(4):408-16 [19] Wang, P. et al.(2002), Nitric Oxide Donors: Chemical Activities and Biological Applications, Chemical [19] Wang, P. et al.(2002), Nitric Oxide Donors: Chemical Activities and Biological Applications, Chemical Reviews 102 (4): 1091–1134. Reviews 102 (4): 1091–1134. [20] EFSA (European Food Safety Authority) (2017), Re-evaluation of potassium nitrite (E 249) and sodium [20] EFSA (European Food Safety Authority) (2017), Re-evaluation of potassium nitrite (E 249) and sodium nitrite (E 250) as food additives, EFSA Journal 15(6):4786. nitrite (E 250) as food additives, EFSA Journal 15(6):4786. [21] EFSA (European Food Safety Authority) (2019), Re-evaluation of phosphoric acid–phosphates – di-, tri- [21] EFSA (European Food Safety Authority) (2019), Re-evaluation of phosphoric acid–phosphates – di-, tri- and polyphosphates (E 338–341, E 343, E 450–452) as food additives and the safety of proposed extension of and polyphosphates (E 338–341, E 343, E 450–452) as food additives and the safety of proposed extension of use, doi: 10.2903/j.efsa.2019.5674 (accessed Apr 1, 2021). use, doi: 10.2903/j.efsa.2019.5674 (accessed Apr 1, 2021). [22] D'Amore, T. et al. (2020) Sulfites in meat: Occurrence, activity, toxicity, regulation, and detection. A [22] D'Amore, T. et al. (2020) Sulfites in meat: Occurrence, activity, toxicity, regulation, and detection. A comprehensive review, Food science and food safety 19 (5), 2701-2720. comprehensive review, Food science and food safety 19 (5), 2701-2720. [23] Metrohm AG. Simplified sulfite determination in foods and beverages using ion chromatography, [23] Metrohm AG. Simplified sulfite determination in foods and beverages using ion chromatography, Metrohm AG: Herisau, Switzerland, 2021. WP-065EN. Metrohm AG: Herisau, Switzerland, 2021. WP-065EN. [24] Lanciki, A., Espinosa, M. (2020) A Simplified Method to Determine Total sulfite Content in Food and [24] Lanciki, A., Espinosa, M. (2020) A Simplified Method to Determine Total sulfite Content in Food and Beverages via Ion Chromatography, LC/GC The Column 16 (2), 12-16. Beverages via Ion Chromatography, LC/GC The Column 16 (2), 12-16. [25] AQSIQ (State general administration of the Peoples Republic of China for quality supervision and [25] AQSIQ (State general administration of the Peoples Republic of China for quality supervision and inspection and quarantine) Determination of iodide content in foods for export – Ion chromatography, GB inspection and quarantine) Determination of iodide content in foods for export – Ion chromatography, GB China National Standards SN/T 3727-2013. China National Standards SN/T 3727-2013. [26] Association of official analytical collaboration (AOAC) (2018): AOAC SMPR® 2018.009, Standard Method [26] Association of official analytical collaboration (AOAC) (2018): AOAC SMPR® 2018.009, Standard Method Performance Requirements (SMPRs) for Lactose in Low-Lactose or Lactose-Free Milk, Milk Products, and Performance Requirements (SMPRs) for Lactose in Low-Lactose or Lactose-Free Milk, Milk Products, and Products Containing Dairy Ingredients, AOAC International, Rockville, MD, USA. Products Containing Dairy Ingredients, AOAC International, Rockville, MD, USA. [27] Brunt, K. et al. (2020), Results Multi-Laboratory Trial ISO/CD 22184 – IDF/WD 244: Milk and milk products [27] Brunt, K. et al. (2020), Results Multi-Laboratory Trial ISO/CD 22184 – IDF/WD 244: Milk and milk products – Determination of the sugar contents – High performance anion exchange chromatography method with – Determination of the sugar contents – High performance anion exchange chromatography method with pulsed amperometric detection (HPAEC-PAD), Journal of AOAC International, qsaa092. pulsed amperometric detection (HPAEC-PAD), Journal of AOAC International, qsaa092. [28] WHO (World Health Organization) (1996), Recommended iodine levels in salt and guidelines for [28] WHO (World Health Organization) (1996), Recommended iodine levels in salt and guidelines for monitoring their adequacy and effectiveness, WHO/NUT/96.13. monitoring their adequacy and effectiveness, WHO/NUT/96.13. [29] Trumbo, P. (2016), FDA regulations regarding iodine addition to foods and labeling of foods containing [29] Trumbo, P. (2016), FDA regulations regarding iodine addition to foods and labeling of foods containing added iodine, American Journal of Clinical Nutrition104(Suppl 3), 864S–867S. added iodine, American Journal of Clinical Nutrition104(Suppl 3), 864S–867S. [30] WHO (World Health Organization) (2011), Nitrate and nitrite in drinking-water, Background document [30] WHO (World Health Organization) (2011), Nitrate and nitrite in drinking-water, Background document for development of WHO Guidelines for Drinking-water Quality, WHO/SDE/WSH/07.01/16/Rev/1 for development of WHO Guidelines for Drinking-water Quality, WHO/SDE/WSH/07.01/16/Rev/1 https://www.who.int/water_sanitation_health/dwq/chemicals/nitratenitrite2ndadd.pdf (accessed Apr 1, https://www.who.int/water_sanitation_health/dwq/chemicals/nitratenitrite2ndadd.pdf (accessed Apr 1, 2021). 2021).
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References (cont.) References (cont.) [31] Chinese standard (2019), National food safety standard for determination of choline in infant foods and [31] Chinese standard (2019), National food safety standard for determination of choline in infant foods and dairy products, GB China National Standards 5413.20-2013. dairy products, GB China National Standards 5413.20-2013. [32] AOAC Official Method 2012.20 (2012), Choline in Infant Formula and Adult Nutritionals Ion [32] AOAC Official Method 2012.20 (2012), Choline in Infant Formula and Adult Nutritionals Ion Chromatography and Suppressed Conductivity First Action. Chromatography and Suppressed Conductivity First Action. [33] Lebensmittel- und Futtermittelgesetzbuch – LFGB (2005), Bundesministeriums der Justiz und für [33] Lebensmittel- und Futtermittelgesetzbuch – LFGB (2005), Bundesministeriums der Justiz und für Verbraucherschutz, Bundesamts für Justiz, www.gesetze-im-internet.de/lfgb/LFGB.pdf (accessed Apr 1, Verbraucherschutz, Bundesamts für Justiz, www.gesetze-im-internet.de/lfgb/LFGB.pdf (accessed Apr 1, 2021). 2021). [34] Spichtig, V. et al. (2020) ; Determination of Fructans in Infant Formula and Adult/Pediatric Nutritional [34] Spichtig, V. et al. (2020) ; Determination of Fructans in Infant Formula and Adult/Pediatric Nutritional Formula by Anion-Exchange Chromatography with Pulsed Amperometric Detection after Enzymatic Formula by Anion-Exchange Chromatography with Pulsed Amperometric Detection after Enzymatic Treatment: Collaborative Study, Final Action 2016.14, Journal of AOAC International 103(5), 1301–1317. Treatment: Collaborative Study, Final Action 2016.14, Journal of AOAC International 103(5), 1301–1317. [35] WHO (World Health Organization) (2015), Guideline: sugars intake for adults and children, [35] WHO (World Health Organization) (2015), Guideline: sugars intake for adults and children, WHO/NMH/NHD/15.2, https://apps.who.int/iris/handle/10665/149782 (accessed Apr 1, 2021). WHO/NMH/NHD/15.2, https://apps.who.int/iris/handle/10665/149782 (accessed Apr 1, 2021). [36] Chatelan, A. et al. (2019) Total, Added, and Free Sugar Consumption and Adherence to Guidelines in [36] Chatelan, A. et al. (2019) Total, Added, and Free Sugar Consumption and Adherence to Guidelines in Switzerland: Results from the First National Nutrition Survey menuCH, Nutrients 11(5), 1117; Switzerland: Results from the First National Nutrition Survey menuCH, Nutrients 11(5), 1117; https://doi.org/10.3390/nu11051117 (accessed Apr 1, 2021). https://doi.org/10.3390/nu11051117 (accessed Apr 1, 2021).
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