Your reliable partner for food testing
The rapid industrialization, globalization and Our Clients represent a variety of industries development of the world trade require professional including: evaluation and analysis of products and processes • food manufacturers and retailers, aimed at confirmation of their quality but also more • cosmetic and household chemistry producers, frequently than ever at consumers safety and our • packaging manufacturers, environment. • pharmaceutical and chemical industries, J.S. Hamilton Poland Ltd. is an unique example • petrochemical industry and fuel distributors, of professional organization which combines • international and domestic traders, independent inspection services with a wide • investors and contractors of industrial plants, About us spectrum of chemical and physical analysis carried • public and governmental organizations. out by own laboratories. Our team of experienced analysts, experts, Being a private and independent, the company inspectors and surveyors ensure the highest standard provides services for both international and of our services. Our own testing laboratories offer domestic trade as well as for many industries such a wide scope of chemical, physical, biochemical, as food processing including food safety, chemical, microbiological and sensory analysis. pharmaceutical and oil industries, plant machinery and construction, fuel quality monitoring etc. At present we are the leader in laboratory services The name of J.S. Hamilton Poland Ltd. means not in Eastern Europe. only professional approach to quality matters but also full impartiality and independence confirmed Why not to make use by relevant accreditations. of our services?
3 Our offer
J.S. Hamilton Poland Ltd. is offering a wide range We provide: Our purpose built food laboratories in Gdynia, of accredited chemical and microbiological testing • Fast, efficient turnaround of results ; Poznań, Katowice and Maków Mazowiecki (near to food, pharmaceutical and other industries. • Certification in English, German, capital city of Warsaw) are fully equipped for Located in Gdynia at the Baltic coast with three Russian in addition to Polish; a wide range of food analysis. Steady expansion and other laboratories in major inland locations, and • Independent testing and advice; investment in new technologies, instrumentation sample collection centers around the country, our • Fast and flexible response to your needs; a n d l a b o r a t o r y p e r s o n n e l h a s l e d u s t o o u r s c o p e laboratories are ideally situated to service Poland • Complete client confidentiality. o f a c c r e d i t a t i o n w h i c h i s t h e m o s t e x t e n s i v e and neighborhood countries. Dependent upon in Poland. your location and the number of samples involved, Food testing has been conducted by J.S. Hamilton a collection service, utilizing our own transport, Poland Ltd. laboratories since their inception in 1993 Our food testing laboratories are operational 7 days equipped with temperature controlled storage, and earlier by their predecessors Polcargo. a week to ensure a competitive, efficient and quality can be provided. service. Our sample collection service is operated During this time Hamilton has gained a vast free of charge subject to a minimum quantity At J.S. Hamilton Poland Ltd. we offer a cost effective experience and technical expertise within the fields collection and dependent upon location. quality service, tailored to your individual and of food microbiology and food chemistry testing. specific needs.
4 Basic Ingredient Composition Training & Minerals / Metals Consultancy p.6
p.70 p.10
Migration From Vitamins Packaging
p.62 p.14
Amino Acids & Microbiology Biogenic Amines
p.60 p.18
Sensory Analysis & Our laboratories Consummer Fat Composition Preference / Adulteration Testing p.58 offer p.22
Miscellaneous Carbohydrates Contaminants / Fibre
p.50 p.26
Preservatives, Dyes, Sweeteners Allergens & GMO & Other Additives
p.44 p.30 Pesticides Mycotoxins
p.38 p.34
5 Basic Ingredient Composition / Nutrition Information J.S. Hamilton Poland Ltd. offers a wide range The information shall consist of either Group 1 of chemical analysis covering basic composition or Group 2 below: of food as well as all minor but important ingredients Group 1 (such as vitamins and minerals) necessary for nutritional information.
Below please find our summary of key points • energy value • protein on nutritional information. • carbohydrate • fat
The main EU act on nutrition labeling for foodstuffs has been established in 1990 (Council Directive 90/496/ EEC of 24 September 1990 on, with amendments). The Directive defined ‘nutrition labeling’ as any Group 2 information appearing on labeling and relating to: • energy value; • nutrients such as: protein, • energy value carbohydrate, fat, fibre, sodium, vitamins • protein • carbohydrate and minerals. • sugars • fat • saturated fat Where a nutrition claim is made for sugars, saturates, • fibre • sodium fibre or sodium, the information to be given shall consist of Group 2.
7 Nutrition labeling may also include amounts of one Vitamins and minerals which may be declared and their recommended daily allowances (RDAs) or more of the following ingredients:
Vitamin A μg 800 Vitamin B12 μg 1 • starch, Vitamin D μg 5 Biotin mg 0,15
• polyols, Vitamin E mg 10 Pantothenic acid mg 6 • monounsaturated fat, Vitamin C mg 60 Calcium mg 800 • polyunsaturated fat, Tiamin mg 1,4 Phosphorus mg 800 Riboflavin mg 1,6 Iron mg 14 • cholesterol, Niacin mg 18 Magnesium mg 300 • any of the minerals or vitamins listed in the Annex Vitamin B6 mg 2 Zinc mg 15 to the Directive (see Table on the right). Folacin μg 200 Iodine μg 150
US Food and Drug Administration established the Daily Values as reference helping consumers to use information on food labels and to plan a healthy diet. A 2 000-calorie level is about right for moderately active women, teenage girls, and sedentary men, and 2 500 calories is the target level for most of men, teenage boys, and active women. Older adults, children, and sedentary women need less than 2,000 calories a day but some active men, teenage boys or very active women may select target levels based on 2 800 calories. Canadian Food Inspection Agency (CFIA) established similar standards for nutritional quality of food sold in Canada.
8 Guideline Daily Amounts (GDA)
In 2006, Confederation of the Food and Drink Nutrition information Guideline daily amounts Children Typical values Per 100 g Per 350 g serving Woman Men Industries (CIAA) introduced in European Union (5-10 years) a set of Guideline Daily Amounts (GDAs) based on Energy - kj 480 kj 1680 kj Eurodiet recommendations. - kcal (Calories) 115 kcal 405 kcal 2000 2500 1800 Protein 9.5 g 33.3 g 45 g 55 g 24 g
Carbohydrate 8.6 g 30.1 g 230 g 300 g 220 g The Eurodiet project, funded by the European of which sugars 2.0 g 7.0 g 90 g 120 g 85 g Commission, provided a framework for national Fat 4.6 g 16.1 g 70 g 95 g 70 g food-based dietary targets and an action plan for of which saturates 3.0 g 10.0 g 20 g 30 g 20 g the development of European dietary guidelines. Fibre 1.5 g 5.3 g 24 g 24 g 15 g
Sodium* 0.3 g 1.1 g 2.4 g 2.4 g 1.4 g
J.S. Hamilton Poland Ltd. offers not only chemical *Equivalent as salt 0.8 g 2.8 g 6 g 6 g 4 g analysis necessary for nutrition information but also helps food producers to design labels complying with existing rules.
9 Minerals / Metals J.S. Hamilton Poland Ltd. offers a wide range Heavy metals of minerals / metals analysis in foodstuffs, water and packing materials for food. The allowed contents of heavy metals in foodstuffs a r e l i s t e d i n C o m m i s s i o n R e g u l a t i o n ( E C ) Some of them like heavy metals are carried out to No 1881/2006 setting the maximum levels for certain confirm the compliance with current legislation, contaminants. Whereby the others are necessary for nutrition information (sodium, potassium, calcium, iron, The longest list of foodstuffs which should be phosphorus). Yet the others relate to minerals monitored refers to the lead contents. The regulation (containing magnesium, zinc, iodine etc.) which set maximum levels of lead for milk, infant and contents has to be strictly determined due to their follow-on formulae, meat, fish and crustaceans, effect on human health. cereals, legumes and pulses, vegetables and fruits, fats and oils, wine and wine products. It should be mentioned that J.S. Hamilton Poland Ltd. Cadmium should be determined mainly in meat, fish also conducts some special analysis for confirmation and crustaceans, cereals, soybeans, vegetable and of identity of products or for determination of mineral fruit, herbs, fungi and potatoes. and/or metal residues in herbs and pharmaceutical products (including nickel, tin, palladium, boron and Mercury contents are given in the above cited others). The metals/minerals analysis are performed regulation for fish products, and tin (inorganic) by inductively coupled plasma optical emission is to be analyzed in canned foods and beverages. spectrometry (ICP- OES). Other heavy metals analysis like arsenic, iron or copper are sometimes required.
11 Analysis for nutrition information Conditions applying to sodium are defined for 3 claims: ”low sodium/salt”, “very low sodium/salt” Sodium is a mineral of important value for and “sodium-free or salt-free”. nutrition. It belongs to the group 2 defined in the Council Directive 90/496/EEC and is also required List of recommended minerals and their daily to be presented in Nutrition Facts (obligatory in US allowances (RDAs) which may be declared and Canada). according to the Directive 90/496/EEC have been presented in the chapter BASIC INGREDIENT Sodium contents are shown in GDAs (see previous COMPOSITION / NUTRITION INFORMATION. chapter). In this case it is also presented as salt (NaCl = 2,5 x Na). Minerals contents in drinking water
Sodium, potassium, calcium, magnesium and The list of minerals which are analyzed in drinking phosphorus are main mineral elements present water contains such elements as: chromium, in food in relative high amounts, and are often cadmium, nickel, boron, lead, antimony, selenium, expressed in g/100 g. aluminum, arsenic, sodium, copper, iron and manganese. Nutrition and health claims
Nutrition claims and conditions applying to them are presented in Annex to the Regulation (EC) No 1924/2006 of 20 December 2006.
12 List of accredited metals/minerals analysis in J.S. Hamilton Poland Ltd. laboratories
A. Food and agricultural samples B. Water and waste samples
Element Range Procedure Element Range Procedure Ag 0,0007 mg/l - 20 mg/l PN-EN ISO 11885:2009
Pb 0,01 mg/kg - 5,0 mg/kg PB-68/ICP ed. II; Hg 0,00001 mg/l - 1 mg/l PN-EN 1483:2007 Tl 0,006 mg/l - 20 mg/l 28.02.2009 Cr 0,01 mg/kg - 5,0 mg/kg Hg 0,0001 mg/l - 2 mg/l PB-30/CVAAS ed. IV; Ti 0,006 mg/l - 20 mg/l 28.02.2009 Cu 0,01 mg/kg - 10,0 mg/kg V 0,008 mg/l - 20 mg/l Sb 0,001 mg/l - 20 mg/l PN-EN ISO 11885:2009 Fe 0,01 mg/kg - 50,0 mg/kg Ca 0,019 mg/l - 250 mg/l As 0,0007 mg/l - 20 mg/l Cd 0,002 mg/kg - 1,00 mg/kg Fe 0,001 mg/l - 20 mg/l Ba 0,004 mg/l - 20 mg/l Zn 0,05 mg/kg - 50,0 mg/kg Be 0,001 mg/l - 20 mg/l As 0,09 mg/kg - 35,7 mg/kg PB-49/ICP ed. II; 28.02.2009 B 0,003 mg/l - 20 mg/l Se 0,29 mg/kg - 62,5 mg/kg C. Packing materials (paper, plastics) Cr 0,001 mg/l - 20 mg/l Sn 0,16 mg/kg - 200 mg/kg Sn 0,006 mg/l - 20 mg/l Fe 0,20 mg/kg - 1000 mg/kg PB-36/ICP ed. III; 28.02.2009 Zn 0,0003 mg/l - 20 mg/l Element Range Procedure Mg 1,00 mg/kg - 5000 mg/kg P 0,010 mg/l - 50 mg/l Cd 0,5 mg/kg - 100 mg/kg Ca 2,00 mg/kg - 20000 mg/kg PB-118/ICP/AAS ed I;. 26.0 4.2 011 Al 0,014 mg/l - 20 mg/l Cr 2,5 mg/kg - 100 mg/kg Cu 6,00 mg/kg -200 mg/kg Cd 0,0001 mg/l - 20 mg/l Pb 2,5 mg/kg - 100 mg/kg Na 38,0 mg/kg - 20000 mg/kg Co 0,002 mg/l - 20 mg/l Hg 0,1 mg/kg - 50 mg/kg K 110 mg/kg - 20000 mg/kg PB-118/ICP/AAS ed I;. Si 0,020 mg/l - 20 mg/l 26.0 4.2 011 Zn 0,20 mg/kg - 1000 mg/kg Mg 0,011 mg/l - 250 mg/l P 6,00 mg/kg - 20000 mg/kg Mn 0,0001 mg/l - 20 mg/l Mn 0,10 mg/kg - 1000 mg/kg Cu 0,010 mg/l - 20 mg/l Hg 0,0006 mg/kg -10 mg/kg PB-30/CVAAS ed. IV; 28.02.2009 Mo 0,001 mg/l - 20 mg/l
P 0,1 g/kg - 10 g/kg PN-A-82060:1999 Ni 0,001 mg/l - 20 mg/l (in meat and meat Pb 0,0006 mg/l - 20 mg/l products) K 0,54 mg/l - 50 mg/l
P 1,00 mg/kg - 221 mg/kg PB-69/ICP ed. II; Se 0,0006 mg/l - 20 mg/l ( in fats 28.02.2009 and oils) S 0,02 mg/l - 20 mg/l
Na 0,10 mg/l - 200 mg/l
13 Vitamins Vitamins are very important components of J.S. Hamilton Poland Ltd. performs analysis a diet, necessary for growth and to maintenance of vitamins in its central laboratory in Gdynia and of body’s vital functions. They have diverse chemical in cooperation with the leading approved European structures. laboratories in this field.
Some of them are very sensitive to external factors Vitamins can be classified by their solubility: vitamins such as light, oxygen or temperature which makes soluble in fat and water. In the following table there difficult to determine their contents in food. are shown principal vitamins, their names, synonyms and vitamers (different forms of vitamins) as well as their main sources.
Vitamin Other names Main sources
Vitamins soluble in fat
Retinol, (β -carotene being present in vegetables is called “provitamin A” A Cod liver oil as it can be converted in animal organism to vitamin A)
D Main forms: D3 or cholecalciferol and D2 or ergocalciferol Cod liver oil
Tocopherols (4 vitamers: α- , β- ,γ- and δ-tocopherol; E Wheat germ oil the most biologically active form is α-tocopherol); tocotrienols
K Main forms: K1 or phylloquinone, K2 or menaquinones Leafy green vegetables
Vitamins soluble in water
B1 Thiamine Rice bran
B2 Riboflavin Meat, eggs
B3 PP, niacine, niacinamide Meat, eggs, grains
B5 Pantothenic acid Meat, whole grains
B6 Pyridoxine, pyridoxamine, pyridoxal Meat, dairy products
B7 Biotin, vitamin H Meat, dairy products, eggs
B9 Folic acid, folinic acid, folacin Leafy green vegetables
B12 Cobolamins Leaver, eggs, animal products C Ascorbic acid Citrus, most fresh foods
15 Vitamins, which may be declared and their recommended daily allowances (RDAs) according to the Council Directive 90/496/EEC of 24 September 1990 amended by the Commission Directive 2008/100/EC, are presented in the chapter BASIC INGREDIENT COMPOSITION/NUTRITION INFORMATION.
Some general information on most frequently methods used for determination of vitamins are given in the following table.
Methods of vitamins analysis
Limit of quantification Vitamin Principle of method (often depends on matrix) A saponification and liquid-liquid extraction; RP-HPLC with fluorimetric detection 0,01 mg/100g
β -carotene saponification and/or liquid-liquid extraction; RP-HPLC with UV detection 0,01 mg/100g
saponification, liquid-liquid extraction and GPC purification; D3 0,5 µg/100g RP-HPLC with UV detection
E (α-tocopherol or sum of saponification and liquid-liquid extraction; RP-HPLC with fluorimetric detection 0,1 mg/100g α-, β-, γ- and δ-tocopherols)
saponification and extraction; RP-HPLC with post-column reduction K1 0,8 µg/100g and fluorimetric detection
acid and enzymatic hydrolysis; RP-HPLC with post-column derivatization B1 0,1 mg/100g and fluorimetric detection
B2 acid and enzymatic hydrolysis; RP-HPLC with fluorimetric detection 0,01 mg/100g
B3 microbiological 0,06 mg/100g
B5 microbiological 7,0 µg/100g
B6 acid and enzymatic hydrolysis; RP-HPLC with fluorimetric detection 0,05 mg/100g
B7 microbiological 1,0 µg/100g
B9 microbiological 5,0 µg/100g
B12 microbiological 0,01 µg/100g
C titrimetry 10 mg/100g
extraction by acid solution; and reduction (depends on matrix); C 1,0 mg/100 g RP-HPLC with UV detection
16 Chromatograms of some vitamins (for standards and for samples)
400 000
l µV wit B6_0,106-1.DA TA 70 000 µV wit B1_w z76,67-2.DATA 350 000 HC 60 000 l a. 300 000 HC 50 000 in
250 000 a am
40 000 ti 200 000 30 000 ksyn
150 000 do
20 000 ry 100 000 pi 10 000 50 000 0 RT [mi n] RT [mi n] 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 l
µV wit B1_16298-1.DATA 400 000 µV pirydoks al HCl HC wit B6_16983-1.DA TA
70 000 a 350 000 60 000 l
300 000 ksyn 50 000 HC a. 250 000 do in 40 000 ry pi
am 200 000
30 000 ti 150 000 20 000 100 000 10 000 50 000 0 RT [mi n] RT [mi n] 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20
Vitamin B1 in a sample of baby food (480 μg/100 g). Vitamin B6 in a sample of isotonic beverage (0,30 mg/100 ml). Chromatographic conditions Chromatographic conditions HPLC with fluorescence detector (excitation 325 nm, emission 480 nm); RP-18 column; Mobile phase: gradient; HPLC with fluorescence detector (excitation 465 nm, emission 520 nm); RP-18 column; derivatization on-column with K3[Fe(CN)6] + 500 ml NaOH; Flow rate: 1,0 ml/min; Ambient temperature. Mobile phase: sodium hexasulphonate + water + methanol + acetic acid; Flow rate: 0,7 ml/min; Ambient temperature. l l a ro 6 000 µV wit B2_w z40-1.DA TA 300 000 µV ro witE-w z_0,8-1.DATA in fe fe ko ko
5 000 aw 250 000 to to fl a- a-
4 000 lt bo 200 000 ol ry de 3 000 mm ga
150 000 ofer 2 000 ok 100 000 -t 1 000 fa al 0 50 000 -1 000 RT [mi n] RT [mi n] 0 0 0,5 1 1,5 2 2,5 3 3,5 4 4,5 5 5,5 6 6,5 7 7,5 8 8,5 9 9,5 10 10,5 11 11,5 12 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20
12 000 µV wit B2_27575-1.DATA 300 000 µV witE-14469_1do100-1.DA TA ol
10 000 er 250 000 a of in
8 000 ok
200 000 -t aw fa fl
6 000 al 150 000 bo
4 000 ry 100 000 2 000 50 000 0 RT [min] RT [mi n] 0 -2 000 0 0,5 1 1,5 2 2,5 3 3,5 4 4,5 5 5,5 6 6,5 7 7,5 8 8,5 9 9,5 10 10,5 11 11,5 12 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20
Vitamin B2 in a sample of black berries in chocolate (84 μg/100 g). Vitamin E in a sample of liquid diet supplement (58,5 mg/100 ml as a-tocopherol). Chromatographic conditions Chromatographic conditions
HPLC with fluorescence detector (excitation 290 nm, emission 395 nm); RP Select B column; Mobile phase: KH2PO4 + HPLC with fluorescence detector (excitation 295 nm, emission 330 nm); RP-18 column; sodium heptasulphonate + water + methanol + ACN (pH = 2,5); Flow rate: 1,0 ml/min; Temperature: 35°C. Mobile phase water: methanol (50 ml : 950 ml); Flow rate: 1,5 ml/min; Temperature: 35°C.
17 Amino acids & Biogenic amines P r o t e i n c o n t e n t i n f o o d , d e t e r m i n e d o n t h e b a s i s These facts clearly demonstrated limitations of the of total nitrogen by Kjeldahl or similar methods, was old Kjeldahl method and a lack of appropriate for a long time generally considered as sufficient. method of analysis for real protein. It became Chinese protein export contamination was first obvious that alternative analytical methods identified in 2007 (pet food recalls). Then later, with improved selectivity and specificity able several Chinese companies sold products claimed to detect protein adulteration were of an immediate to be wheat gluten, rice protein or corn gluten, but need. Such method proved to be amino acid which proved to be wheat flour adulterated with analysis recommended by Food and Agriculture melamine, cyanuric acid and other contaminants. Organization of the United Nations (FAO).
On the other hand, growth of interest in diet supplements with free amino acids as main active compounds, has caused a need for analysis of amino acids composition.
19 Free amino acids are widely used as additives The allowed levels of histamine content in fish and fish In that latest case the analysis is possible thanks to animal feed. Their addition is necessary, since products are established in Commission Regulation to the high sensitivity method used by our laboratory s o m e i m p o r t a n t c o m p o n e n t s o f f e e d s , s u c h (EC) No 1441/2007. (limit of quantification amounts to 0,005%). as soybeans, have low levels or even a complete lack of the essential amino acids (such as lysine, Some countries established the maximum tolerable Histamine analysis is performed by J.S. Hamilton methionine, threonine and tryptophan). limits or recommended upper limits for histamine Poland Ltd. laboratories mainly in fish and fish also in other food: in meat products (Netherlands, products. Testing method is accredited and based In food industry, amino acids are used either Czech Republic) and in beer (Slovak Republic), on high performance liquid chromatography with as flavour enhancer in a form of sodium salt and in cheese (for tyramine in Slovak Republic). UV detection. of glutamic acid or as artificial sweetener in form of derivative of phenylalanine (aspartame). Following are amino acids most frequently analysed by J.S. Hamilton Poland Ltd. laboratories : List of amino acids and their abbreviations Biogenic amines are defined as basic nitrogenous • amino acids composition in: compounds exerting physiological action that can ◦◦ feedstuffs; affect human health. They are formed mainly by ◦◦ diet supplements; Essential Nonessential Isoleucine Ile Alanine Ala decarboxylation of amino acids or by amination ◦◦ special products as dried kiwi fruits, Leucine Leu Asparagine Asn and transamination of aldehydes and ketones. whey protein concentrates; Lysine Lys Aspartic acid Asp
◦◦ low protein food. Methionine Met Cysteine Cys One of the prominent members of the group • monosodium glutamate in food, Phenylalanine Phe Glutamic acid Glu is histamine – a compound derived from the amino • taurine (non protein amino acid) in feed Threonine Thr Glutamine Gln Tryptophan Trp Glycine Gly acid histidine. and in energy drinks, Valine Val Proline Pro • phenylalanine (traces) in phenyl free special Selenocysteine Sec
protein preparations. Serine Ser
Tyrosine Tyr
Arginine Arg
Histidine His
Pyrrolysine Pyl
20 Chromatograms of amino acids
240 000 µV aa-7715-nu-1.DATA A
230 000 u 220 000 Gl 210 000 200 000 190 000 180 000 170 000 160 000
150 000 p As 140 000 y s Gl l u Le 130 000 Ly Va
120 000 e 11 0 000 Nl g o 100 000 Ar Pr r e a
90 000 Il Se 80 000 Al 70 000 e Ph r r 60 000 Ty Th
50 000 t s 40 000 Me s Hi
30 000 Cy 20 000 10 000 RT [min] 0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 HPLC with UV detection of amino acids in sample of feedstuff (A) and in standard mixture (B).
180 000 175 000 µV aa-nu-1.DATA 170 000 B s
165 000 Ly 160 000 155 000 150 000 145 000 e 140 000 l t r Nl
135 000 Va e Ty 130 000 Me Il 125 000 120 000 u Le 115 000 e s 11 0 000 Ph p 105 000 Cy u 100 000 As Gl o
95 000 Pr y
90 000 g r a Gl Ar Al 85 000 Se r
80 000 s Th
75 000 Hi 70 000 65 000 60 000 55 000 50 000 45 000 40 000 35 000 30 000 25 000 20 000 15 000 10 000 5 000 RT [min] 0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 Chromatographic conditions Column: RP-18e; 250 mm x 4 mm x 5 µm; Detection at: 254 nm; Mobile phase: A - acetate buffer pH 6.2; B - acetonitrile: water (6:4); Column temperature: 40 ºC; Time: 38 min.
21 Fat composition / Adulteration Fat composition in food became of a great interest Composition of fats in foods is also important from for two reasons: economical point of view. Adulteration by use • different nutritional value of its main of cheaper fat instead of expensive one has been components (triacylglycerols), a common problem in trade for a long time. • the possibility of adulteration A classic example is “extra virgin” olive oil, diluted (economic reasons). with cheaper olive oils or with other vegetable oils. It has been estimated that adulterated olive oil has Triacylglycerols (TAGs) composed of saturated fatty become the largest source of agricultural fraud acids are less recommended for human body than problem in EU. mono - and polyunsaturated fatty acids. Recent progress in fat technology has made Moreover, the fats undergo some transformations it possible to increase the use of adulterants during processing resulting in change of unsaturated in dairy products, now more difficult to detect fatty acids configuration from natural cis to harmful and to quantify. The practice of adulteration is not trans isomers. It has been proved that trans isomers limited to butter itself but also to other dairy products increase the risk of coronary heart disease by raising containing significant percentage of fat, such „bad” LDL cholesterol and lowering „good” HDL as condensed milk, whole dried milk, ice cream and cholesterol levels. Health authorities recommend cheese. that consumption of trans fat should be reduced to trace amounts. In the result of big production and consumption of chocolate products a common fraudulent The “saturates” are those food components which practice is to replace cacao butter by other fats should be shown on nutritional labels in EU and without appropriate labeling. North America.
23 In the framework of the European Commission Fatty acids composition is often required for the scientific panels have been set up to develop nutritional information. Results of analysis may be Main fatty acids of milk fat methods allowing detection and quantitative presented either in a form of a profile of about 20
determination of foreign fats in food products such individual fatty acids or as a sum of saturated, Common or scientific Carbon atoms: % name double bonds as olive oil, dairy products (butter, cheese and milk monounsaturated, polyunsaturated and trans fatty Butyric 4:0 3,5
powder) and in chocolate. acids. The content of essential unsaturated fatty Caproic 6:0 2,0 acids (omega-3) is also available. Caprylic 8:0 1,1 The developed methods are based mainly on analysis Capri 10:0 2,5 Lauric 12:0 3,0 of TAGs composition with use of chromatographic Main fatty acids of cacao butter Myristic 14:0 11,0 techniques. Tetradecenoic 14:1 1,0
Pentadecanoic 15:0 2,0 Common or scientific Carbon atoms: J.S. Hamilton Poland Ltd. laboratory follows the % Palmitic 16:0 27,0 name double bonds Palmitoleic 16,1 2,0 Customers’ need to use the most up-to-date testing Myristic 14:0 0,1 Margaric 17:0 0,5 methods. Our own gas chromatographic analysis of Palmitic 16:0 26,0 Stearic Acid 18:0 12,0 triacylglycerols as well as the methods for detection Palmitoleic 16,1 0,4 Oleic Acid 18:1 28,5 Margaric 17:0 0,2 and quantitative determination of cacao butter Linoleic Acid 18:2 3,0 Stearic 18:0 35,0 equivalents in chocolate and milk fat purity were Linolenic 18:3 0,5 Oleic 18:1 34,0 Gadoleic 20:1 0,5 validated and accredited very soon after the Linoleic 18:2 3,0 methods of TAGs analysis had been developed Linolenic 20:0 1,0 in the world. Gadoleic 20:1 0,1 Behenic 22:0 0,2
24 DIRECTIVE 2000/36/EC OF THE EUROPEAN PARLIAMENT AND OF THE COUNCIL of 23 June 2000 relating to cocoa and chocolate products intended for human consumption
”The addition of certain vegetable fats other than cocoa butter to chocolate products, up to a maximum of 5 %, should be permitted in all Member States; those vegetable fats should be cocoa butter equivalents and therefore be defined according to technical and scientific criteria.” “In the case of chocolate products to which vegetable fats other than cocoa butter have been added, consumers should be guaranteed correct, neutral and objective information in addition to the list of ingredients.”
1 000 000 pop µV tag_crm-04-04-1.DATA 52 000 µV
950 000 50 000 s CBE_201 1 -06-09 11_54_27_ irmm-2.DATA 900 000 48 000 po Chromatograms 850 000 46 000 800 000 44 000 750 000 42 000 40 000 700 000 p 38 000 po 650 000 36 000 600 000 34 000 550 000 32 000
500 000 30 000 s 6 8 28 000 so C3
450 000 C3 400 000 26 000 0 6 24 000 C4 8 C4 350 000 4 0 22 000 2 C4 4 C3 300 000 C5 C4 L
C4 20 000 2
250 000 RO 18 000 C5 200 000 16 000 2 OLESTE 4
150 000 C3 14 000 0 C5 CH o
8 12 000
100 000 C3 o 6 4 po C2
10 000 so C2 50 000 C2 8 000 0 RT [min] RT [min] 6 000 -50 000 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 18 19 20 21 22 23 24 25 26 27 28 29 30 Pure milk fat (BCR 519) Pure cacao butter (IRMM 801)
1 000 000 pop µV tag_9783-1.DATA µV CBE_201 1 -04-22 19_19_27_ 12082-2.DATA 950 000 75 000 900 000 70 000 p s 850 000 0 po po 800 000 C5 65 000 750 000 60 000 700 000
2 55 000 650 000 C5 600 000 50 000 550 000 45 000 500 000 8 40 000 s so
450 000 C4 400 000 35 000 350 000 30 000 300 000 L 6 25 000 4
250 000 RO C3 200 000 C5
8 20 000 o OLESTE C3 4 150 000 po 4 o 6 CH 15 000 C4 so C4 100 000 C3 0 8 2 4 0 2 6 C3 C2 C3 C2 C4 50 000 C4 10 000 C2 0 RT [min] 5 000 -50 000 RT [min]
0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 19 19,5 20 20,5 21 21,5 22 22,5 23 23,5 24 24,5 25 25,5 26 26,5 27 27,5 28 28,5 29 29,5 Fat extracted from adulterated cheese; the analysis showed the presence Fat extracted from chocolate containing 5 % CBE of approximately 95% of the foreign fats Chromatographic conditions: Chromatographic conditions: GC Column: dedicated for triacylglycerol analysis, 30m x 0,25mm x 0,1µm; column GC Column: WCOT FUSED SILICA 10m x 0,32mm x 0,1µm; column temperature: programmed; temperature: programmed; detector: FID, 350 0C; carrier gas: helium. detector FID, 350 0C; carrier gas: helium.
25 Carbohydrates / Fibres Carbohydrates (other name - saccharides) are one For sugars contents analysis is performed by: The most difficult analysis is that of dietary fiber. of three main nutrients in food, the others being • classic titrimetric methods such as Lane-Eynon, This due to diversity of compounds belonging fats and protein. There are three common types Fehling, Luff-Schoorl, for total amount of to this group. An increasing interest on in dietary fiber of carbohydrates in foods: reducing sugars without or after inversion, or in food is recently observed. This may be caused by • sugars (mainly monosaccharides and • enzymatic treatment followed its positive action to humans body – the dietary fiber disaccharides), by spectrofotometric measurement, or contributes to prevention of heart diseases, diabetes • starch and other digestible polysaccharides, • gas chromatographic method after formation and some forms of cancer. Dietary fiber daily intake • dietary fibre (not digested in the human small of volatile sugar derivatives. recommended by WHO is min. 25 g. Average intake intestine). in Europe is 15 g to 20 g. The fiber content in food Determination of starch may be carried out can be a subject of nutrition claims in compliance Their contents in food are necessary for by polarometric or - by titrimetric method (after with Regulation (EC) No 1924/2006 of the European nutritional labeling (Council Directive 90/496/EEC reducing sugars by inversion). Parliament and of the Council of 20 December 2006 of 24 September 1990, with the later amendments, on nutrition and health claims made on food (see see chapter BASIC INGREDIENT COMPOSITION below). / NUTRITION INFORMATION) as well as for a diet formulation. Main carbohydrates data, their digestibility as well as the legal definition of dietary fiber are given on the next page.
For mandatory nutritional information, the content of digestible carbohydrates is established by calculation using the formula:
Carbohydrates, g/100 g = (100 - Water - Protein - Fat - Ash - Dietary Fibre)
27 Main types of carbohydrates and their digestibility J.S. Hamilton Poland Ltd. laboratories perform analysis • lactose in dry milk by spectrofotometric method (adapted from Statement of the Scientific Panel on Dietetic Products, Nutrition of carbohydrates by all above mentioned methods. ISO 5765-1:2002/IDF-FIL 79-1 :2002, and Allergies on a request from the Commission related to dietary fibre, by EFSA) The choice of an appropriate method depends ISO 5765-2:2002/IDF-FIL 79-2:2002, on the matrix and a purpose of the testing. range 30 % to 60 %; The choice is consulted with the customers, • starch in feed by polarimetric method Class Sub-group Components Digestibility
Glucose + if necessary. GAFTA 28:1 ed.2003; PN-R-64785:1994, Monosaccharides Galactose + Fructose + range 1,0 % to 80 %; Sugars Sucrose + In particular, following methods for carbohydrates / • starch in honey (qualitative test) Lactose + (-) Disaccharides Trehalose + fiber are validated and accredited at J.S. Hamilton by PN-A-77626:1988 p. 5.3.17.4; Maltose +
Malto- Poland Ltd.: • crude fibre in feed by GAFTA 10:0 ed. 2005, Maltodextrins + oligosaccharides • total carbohydrates in food by calculation; PN-EN ISO 6865:2002, PN-ISO 5498:1996; Oligosaccharides α-Galactosides (GOS) - Other Fructo-oligosaccharides (FOS) - • total sugars after inversion in pastry products range 0,2 % to 25 %; oligosaccharides Polydextrose (PDX) - Resistant dextrins - by titrimetric method (Luff-Schoorl) • dietary fibre in food by AOAC 991.43:1994 Maltitol, sorbitol, Polyols + - xylitol, lactitol PN-A 74252:1998 p.3.5.2; range 0,2 % to 30 %; range: 0,1 % to 75 %.
Amylose +(-) • sugars content in honey by liquid Amylopectin +(-) Starch Modified starch +/- chromatography with RI detection: Resistant starch +/- Polysaccharides Inulin - ◦◦ glucose: 2 g/100g to 50 g/100 g; Cellulose Hemicelluloses - ◦◦ fructose: 2 g/100g to 50 g/100 g; Pectins Hydrocolloids, - Non-starch e.g. gums, mucilages, - polysaccharides ◦◦ maltose: 2 g/100g to 30 g/100 g; β-glucans -
Related substance Lignin - ◦◦ sucrose: 2 g/100g to 30 g/100 g; • lactose in casein and caseinates by spectrofotometric method ISO 5548:2004/IDF-FIL 106:2004; range 0,01 % to 2 %;
28 COMMISSION DIRECTIVE 2008/100/EC of 28 October 2008 Definition of the material constituting fibre and methods of analysis as referred to in Article 1(4)(j)
Definition of the material constituting fibre. For the purposes of this Directive “fibre” means carbohydrate polymers with three or more monomeric units, which are neither digested nor absorbed in the human small intestine and belong to the following categories: • edible carbohydrate polymers naturally occurring in the food as consumed, • edible carbohydrate polymers which have been obtained from food raw material by physical, • enzymatic or chemical means and which have a beneficial physiological effect demonstrated by generally accepted scientific evidence, • edible synthetic carbohydrate polymers which have a beneficial physiological effect demonstrated by generally accepted scientific evidence.
REGULATION (EC) No 1924/2006 OF THE EUROPEAN PARLIAMENT AND OF THE COUNCIL of 20 December 2006 on nutrition and health claims made on foods
SOURCE OF FIBRE A claim that a food is a source of fibre, and any claim likely to have the same meaning for the consumer, may only be made where the product contains at least 3 g of fibre per 100 g or at least 1,5 g of fibre per 100 kcal.
HIGH FIBRE A claim that a food is high in fibre, and any claim likely to have the same meaning for the consumer, may only be made where the product contains at least 6 g of fibre per 100 g or at least 3 g of fibre per 100 kcal.
29 Preservatives, dyes, sweeteners & other additives Council Directive 89/107/EEC is the main European Following technical directives: legal act concerning additives authorized for use • Directive 94/35/EC on sweeteners, in food. • Directive 94/36/EC on colours and • Directive 95/2/EC on additives other Directive defines additives are defined as „any than sweeteners and colours substance not normally consumed as a food in establish the list of (1) additives which could be used itself and not normally used as a characteristic (with exclusion of others), (2) foods in which they ingredient of food whether or not it has nutritive could be used and (3) maximum levels. value, the intentional addition of which to food for a technological purpose „results” in it or its Some additives are used to maintain freshness by-products becoming directly or indirectly and to prevent deterioration of food, other help a component of such foods.” to enhance or promote sensory quality. The first group includes such additives as preservatives and Only those additives that are explicitly authorized antioxidants. by EU legislation may be used. Most food additives may only be used in limited quantities and only In the list of additives useful for improvement in certain foodstuffs. If no quantitative limits are of sensory characteristics or helping in food prescribed for use of a food additive, its applicable processing are colours, taste and texture modifiers. quantity has to be in accordance with a good manufacturing practice, i.e. it must be minimum to The full list of categories of food additives achieve desired technological effect. is appended to the Directive 89/107/EEC (next page).
31 J.S. Hamilton Poland Ltd. laboratories perform Categories of food additives following analyses of additives: (Appendix I of Directive 89/07/EC • preservatives - benzoic acid/benzoates, sorbic Colour Modified Starch acid/sorbates, sulphur dioxide, nitrites and Preservative Sweetener
nitrates; Anti-oxidant Raising agent
• anti-oxidants - butylated hydroxyanisole (BHA), Emulsifier Anti-foaming agent butylated hydroxytoluene (BHT); Emulsifying salt Glazing agent Thickener Flour treatment agent • sweeteners - acesulfam K, aspartame, Gelling agent Firming agent saccharin, sodium cyclamate; Stabilizer Humectant
• flavour enhancers - monosodium glutamate; Flavour enhancer Sequestrant
• dyes - Sudan I, II, III and IV and other; Acid Enzyme • water binding agent - phosphates (in meat Acidity regulator Bulking agent Anti-caking agent Propellent gas products). and packaging gas
32 Chromatograms of benzoic acid and sorbic acids used as preservatives in foodstuffs
µV BiS-wz 2,5-2.DATA µV BiS-2116 4_1 do 10-1.DATA 17 0 000 n 55 000 ia n
16 0 000 rbin n
So 50 000 150 000 oesa oesa
140 000 Benz Benz 45 000 n 130 000 ia rbin
120 000 40 000 So 11 0 000 100 000 35 000 90 000 30 000 80 000
70 000 25 000 60 000 50 000 20 000 40 000 15 000 30 000
20 000 10 000 10 000 RT [min] 0 5 000 RT [min] 0 0,5 1 1,5 2 2,5 3 3,5 4 4,5 5 5,5 6 6,5 7 7, 5 8 8,5 9 9, 5 10 10,5 11 11 ,5 12 0 0,5 1 1,5 2 2,5 3 3,5 4 4,5 5 5,5 6 6,5 7 7, 5 8 8,5 9 9, 5 10 10,5 11 11 ,5 12 Chromatogram of standards: benzoic acid (2,5 mg/100ml) + sorbic acid (2,5 mg/100ml). Chromatogram of sample of fish product; benzoic acid - 330 mg/kg, sorbic acid - 200 mg/kg.
120 000 µV BiS-21993_1 do 10-1.DATA Chromatographic conditions: 11 5 000 11 0 000 HPLC with UV-VIS detection; RP 18 column; 105 000 n
100 000 oesa Detection UV-VIS: at 227 nm;
95 000 Benz 90 000 Mobile phase: A = 950ml phosphate buffer + 50 ml MeOH; B = MeOH; 85 000 Flow rate: 1 ml/min; 80 000 75 000 Isocratic: 95 % A and 5 % B. 70 000 65 000 60 000 55 000 50 000 45 000 40 000 35 000 30 000 25 000 20 000 15 000 10 000 5 000
0 0,5 1 1,5 2 2,5 3 3,5 4 4,5 5 5,5 6 6,5 7 7, 5 8 8,5 9 9, 5 10 10,5 11 11 ,5 12 Chromatogram of sample of a nonalcoholic beverage; benzoic acid - 120 mg/l.
33 Mycotoxins Mycotoxins are toxic secondary metabolites produced Commission Regulation (EC) No 1881/2006 by molds. They occur in almost all agricultural of 19 December 2006 set the maximum levels for commodities, both raw and processed. In addition certain mycotoxins considered as a potential risk for to high risk factor to human health, they lead to very human beings. serious economic losses in food and feed supply chain. According to the FAO, mycotoxins contaminate The maximum levels are established for: up to 25% of the world’s food supply. • Aflatoxin 1B and sum of aflatoxins 1B , B2,
G1 and G2;
More than 300 mycotoxins are known, of which about • Aflatoxin 1M ; 20 seriously contaminate crops used for human foods • Ochratoxin A; and animal feed. • Patulin; • Deoxynivalenol; They can be classified in the following main groups: • Zearalenone; • aflatoxins, • Fumonisins; • trichothecenes, • T-2 and HT-2 toxins (not yet established). • fumonisins, • zearalenone, • ochratoxin, • ergot alkaloids, • patulin.
35 Testing of mycotoxins in food and feed at J.S. Hamilton It should also be mentioned that J.S. Hamilton Poland Poland Ltd. has a long years history coming back Ltd. laboratories have accredited an analytical to sixties when we started aflatoxins testing shortly method for determination of ergosterol content, after the famous incident of “turkey X disease” which can be used as preliminary testing for in England happened. Those first experiments have mycotoxins potential presence in cereals and cereal been continued and expanded to all mycotoxins products. being now tested. The accredited methods are The range of analysis: from 1 mg/kg to 30 mg/kg. presented below. The method is based on gas chromatography with mass spectrometric detection (PB-47/GC ed. III; 28.02.2009).
Mycotoxin Range Principle of method Procedure Products
Aflatoxin B , G 0,020 μg/kg - 300 μg/kg PN-ISO 14718:2001 1 1 HPLC with AOAC 999.07:2000 fluorescence Food and feed PN-EN 12955:2001 Aflatoxin B , G 0,005 μg/kg - 500 μg/kg detection 2 2 PN-EN 14123:2008
Aflatoxin B , G 0,20 μg/kg - 40 μg/kg HPLC with 1 1 PB-37/HPLC Cocoa and cocoa fluorescence ed. II; 19.12.2008 products Aflatoxin B2, G2 0,05 μg/kg - 10 μg/kg detection
0,01 μg/dm3 - 0,5 μg/dm3, HPLC with PN-EN ISO 14501:2009 Milk and milk Aflatoxin M in liquid milk; fluorescence IDF-FIL 171:2007 1 products 0,1 μg/kg - 5 μg/kg; in dry milk detection PB-113 ed. I; 15.01.2011
HPLC with PN-EN ISO 15141-1:2000 Ochratoxin A 0,25 μg/kg - 300 μg/kg fluorescence Food and feed PN-EN 14132:2010 detection
HPLC with Wine, beer, fruit and Ochratoxin A 0,1 μg/l do 20 μg/l fluorescence PN-EN 14133:2010 vegetable juices detection
Fumonisin B1 100 μg/kg - 100 000 μg/kg HPLC with fluorescence PB-43/HPLC ed. III; 28.02.2009 Food and feed
Fumonisin B2 40 μg/kg - 100 000 μg/kg detection
HPLC with Zearalenon 10 μg/kg - 4000 μg/kg fluorescence PB-44/HPLC ed. III; 28.02.2009 Food and feed detection
Deoxynivalenol, AOAC 986.18:1990 100 μg/kg - 20 000 μg/kg GC-ECD Food and feed DON, vomitoxin IWł-02/II/PO/2006 ed. II; 30.11.2006
Toxin T-2 300 μg/kg - 2000 μg/kg Cereals and cereal GC-ECD PB-70/GC ed. II; 28.02.2009 Toxin T-2 200 μg/kg - 2000 μg/kg products 36 Chromatograms of mycotoxins (upper chromatograms refer to reference standard samples, the lower ones – to tested samples)
4 500 µV AFLA-wz_0,808-3.DATA 4 000 a G1 a B1 a B2 yn yn 3 500 yn ks ks ks to to 3 000 to a G2 afla afla 2 500 afla yn Chromatographic conditions: 2 000 ks to HPLC with KOBRA cell for derivatization
1 500 afla 1 000 and with fluorescence detector; 500 0 RT [min] Column: RP-18; 250 mm x 4 mm x 5 µm; -500 Detection: excitation at 365 nm, emission at 435 nm; 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 Mobile phase: water, methanol, acetonitrile, HNO3, KBr; 2 500 µV AFLA-15641-1.DATA Flow rate: 1 ml/min; a B1 a G1 yn 2 000 yn ks ks Temperature: ambient. to to 1 500 afla afla a G2 a B2
1 000 yn yn ks ks to to 500 afla afla
0 RT [min]
0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 Determination of aflatoxins in a sample of sweets. Found values (in μg/kg): B1 = 0,40, B2,= <0,05, G1 = 0,48 and G2 = 0,07.
Chromatographic conditions: 8 000 µV M1_wz_0,5-2.DATA HPLC with fluorescence detector; 6 000 Column: RP-18; 250 mm x 4 mm x 5 µm; 4 000 M1
a Detection: excitation at 365 nm, emission at 430 nm;
2 000 yn ks Mobile phase: water, acetonitrile; to la
0 Af Flow rate: 1 ml/min;
-2 000 RT [min] Temperature: ambient.
0 0,5 1 1,5 2 2,5 3 3,5 4 4,5 5 5,5 6 6,5 7 7, 5 8 8,5 9 9, 5 10 10,5 11 11 ,5 12 12,5
8 000 µV M1_29529-idf-1.DATA
6 000 1 M
4 000 na ksy to
2 000 la Af 0
-2 000 RT [min]
0 0,5 1 1,5 2 2,5 3 3,5 4 4,5 5 5,5 6 6,5 7 7, 5 8 8,5 9 9, 5 10 10,5 11 11 ,5 12 12,5 Determination of aflatoxin M1 in a sample of cheese. Found value: M1 = 0,04 μg/kg.
37 Pesticides Pesticides are substances intended for preventing, and other plants that growth where they are not destroying or controlling any pest, including wanted, insecticides – to kill insects, etc.); vectors of human or animal disease, unwanted • toxicity (according to World Health Organization species of plants or animals, causing harm during lines there are four toxicity classes: from or otherwise interfering with the production, “extremely and highly hazardous” - class la processing and storage. The term includes and Ib to „product unlikely to present acute substances intended for use as a plant growth hazard in normal use – class IV); regulator, defoliant, desiccant or agent for thinning • persistence in the environment; fruit or preventing the premature fall of fruit. • formulation (e.g. granules, pellets, soluble Pesticides residues also are potentially toxic to other powder, wettable powder, aerosol, gel, living organisms, including animals and people. microencapsulated materials, solution, etc.) or • pathways to the pest organism. Pesticides are classified according to their: • chemical structure (e.g. organochlorines, organophosphates, pyrethroids, carbamates, thiocarbamates, chlorophenoxy compounds, etc.); • mode of action (e.g. algicides used to restrict alga growth in lakes and swimming pools, attractants lures pest to a treated location, chemosterilant used to control pest populations by sterilizing males, growth regulator – speeds up or retards growth processes, fungicides – used to kill fungi, herbicides – used to kill weeds
39 Possible consequence of pesticides use may be Monitoring and analysis Pesticide residues analyses presence of their residues in processed products. by J.S. Hamilton Poland Ltd. laboratories Therefore it is necessary to ensure that residues Due to the large number of pesticides and to the in 2005 – 2010 in foodstuffs of pesticides are not present in food or feed existing rules on MRLs it is necessary to use many at unacceptable levels, thus causing risk to humans analytical methodologies, of different sensitivity, Products Percentage Cereals and cereal 29,0% beings. precision and selectivity. At present, mainly preparations chromatographic techniques (both liquid and Feed 11,1% In EU amount of pesticides residues in food gas chromatography) are used for pesticides Fruits, vegetables 17,0 % Dairy products 17,2 % is regulated by Regulation (EC) No 396/2005. monitoring with a special attention towards Oils and fats 6,0% This Regulation completes the harmonization m e t h o d o l o g i e s w h i c h a l l o w s c r e e n i n g a n a l y s i s Meat and meat products 0,8%
and provides a unification of Maximum Residue of a number of pesticides by a single cycle analysis. Dried fruits and nuts 7,0 % Levels (MRLs) for particular pesticides. Limits for M o n i t o r i n g o f p e s t i c i d e s i s n o t o n l y r e g u l a t e d Oil seeds 0,6% pharmaceutical products (such as drugs, herbs and by governmental supervisory schemes, but Confectionery 7, 8 % Water 0,4% herb products) are listed and regulated by European is also responsibility of food producers and traders. Other 3,1% Pharmacopoeia, United States Pharmacopoeia Hence the need for testing foodstuffs to prove their or by individual national Pharmacopoeias. compliance with current legislation.
There are also limits and regulations for pesticides J.S. Hamilton Poland Ltd. laboratories have been residues in water (particularly in drinking water), analyzing pesticide residues for many years. air and soil. This mostly in cereals, fresh fruits, vegetables, processed fruit and dairy products. Details for years 2005-2010 are presented in Table 1 below.
40 Chromatograms of cheese sample and pesticides standard u
H Analytical methods A 50 000 µV or pest_gc-wz-56-1.DATA hl an HC DE H rd ac a 'D CH lo pt
40 000 HC H pp or mm ch he a B hl fa an s lt in d ga al
rd J.S. Hamilton Poland Ltd. laboratories apply both dr ac an HC de
30 000 sy lo na tr in pt in en ok ry dr CH dr DT DD he s ch DE DT al ep
od standard methods as well as our own validated H el 20 000 DD 'D 'D ci iz 'D 'D di ta 'D pp pp op op be 10 000 op procedures. In general, we use various methods 0 RT [min] dedicated for different types of samples and/or
0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 32 34 36 different compounds, as follows:
B 50 000 µV pest_9688-1.DATA - “simple” method (for 18 compounds) is based on
40 000 an liquid-solid extraction, purification on sorbent and rd lo
30 000 ch gas chromatographic separation with electron s an na 20 000 tr capture detector. In case of fatty matrices - the first ry od
10 000 iz step is fat extraction. 0 RT [min]
0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 32 34 36
50 000 µV pest_9688-2.DATA 40 000 an rd 30 000 lo ch s an 20 000 na tr ry od
10 000 iz
0 RT [min]
0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 32 34 36 Fig 1.Chromatograms of pesticides standard (A) and extract of cheese sample (B). Chromatographic conditions: column capillary; type 1701-P; oven temperature- programmed; split injection; detector ECD; 300ºC.
41 • screening method (for about 120 compounds, The extract is separated in the system gas depending on matrix). chromatograph coupled with tandem mass The method is applicable to the determination spectrometer GC MS-MS. of residues of pesticides (and PCBs) in agri-food • analysis of pesticide residues in herbs (according samples. to European Pharmacopoeia). Preparation of the sample based on the standard The method consists of three parts - inorganic DFG S-19 contains sample extraction with a suitable bromide analysis, dithiocarbamates analysis and solvent followed by purification using gel permeation other herbicides, listed in Ph.Eur. chromatography and solid phase extraction. The extract (corresponding fractions) is then The principle of method inorganic bromides separated in the system gas chromatograph - mass determination is the extraction of inorganic bromides spectrometer (GC-MS, SIM) or gas chromatograph and convertion to 2-bromoethanol in aqueous test - tandem mass spectometer (GC-MS/MS, MRM sample solution, acidified with sulfuric acid in presents mode). of ethylene oxide. Derivatives are extracted into ethyl acetate and determined by gas chromatography • screening method according to PQ lists (for about with electron capture detector. 250 compounds, depending on matrix). The method is applicable for determination I n t h e c a s e o f d i t h i o c a r b a m a t e s d e t e r m i n a t i o n of residues of pesticides (and PCBs) especially in fresh as carbon disulphide gas chromatograph with head- vegetables, fruits and cereals. Preparation of the space autosampler is used. sample is based on EN 15662:2008 using QuEChERS method.
42 Chromatograms 4 7 7 8 5 4 7 4 85 58 48 67 75 8, 8, 8, 8, 8, 8, 8, 8, 8, 57 8, 8,46 8,82 60 450
400 50 100
350
40
80 300
30 250
60 ] V] V] m mV [ [m
[ e sponse 20 sponse 200 espons R Re Re
-P 40 150
10 +P
100
20 0 -P
+P 50 +P -10 -P 0 0 OM OM OM BR BR BR 2- 2- A B C 2-
7 , 0 7 , 2 7 , 4 7 , 6 7 , 8 8,0 8,2 8,4 8,6 8,8 9 , 0 9 , 2 9 , 4 9 , 6 9 , 8 10,0 10,2 10,4 6,8 7, 0 7, 2 7, 4 7, 6 7, 8 8,0 8,2 8,4 8,6 8,8 9,0 9,2 9,4 9,6 9,8 10,0 7 , 50 7 , 60 7 , 70 7 , 80 7 , 90 8,00 8,10 8,20 8,30 8,40 8,50 8,60 8,70 8,80 8,90 9 , 00 9 , 10 9 , 20 9 , 30 9 , 40 9 , 50 9 , 60 9 , 70 9 , 80 9 , 90 Time [min] Time [min] Time [min] Chromatograms of inorganic bromides extraxted from herb sample (A), spiked herb sample (B) and standard solution (C). Chromatographic conditions: GC Column: Wax; 30m x 0,32mm x 0,1µm; column temperature: programmed; split/splitless injector; detector ECD, 350ºC; carrier gas: helium. 13 9, 260 12 9, 220
240 210
200 220
190 In a case of other herbicides analysis a compilation
200 180
170 of techniques for purification with gel permeation 180
160
160 150 chromatography based on the standard DFG S-19,
140 140
130 and QuEChERS method is applied.
120 120 ] mV [
] 11 0 mV
sponse 100 e [ Re 100 spons Re 80 90 The extract is separated in gas chromatograph
80 60
70 coupled with tandem mass spectrometer
40 60
50 (GC MS-MS, MRM mode). 20 -P +P 40
0 30
20 -20
10 -P +P
-40 0 2
CS -10 2 A B CS 7, 5 8,0 8,5 9,0 9,5 10,0 10,5 Time [min] 6,0 6,5 7, 0 7, 5 8,0 8,5 9, 0 9, 5 10,0 10,5 11,0 11,5 Time [min] Chromatograms of dithiocarbamates as CS2 extracted from standard (A), spiked herb sample (B). Chromatographic conditions: GC Column: 1701; 30m x 0,25mm x 0,1µm; column temperature: programmed; detector ECD, 350ºC; carrier gas: helium.
43 Allergens & GMO Allergens
Allergic reactions can be caused by even small J.S. Hamilton Poland Ltd. laboratories offer traces of allergenic substances in food. Nowadays, comprehensive analysis scope including following correct labeling and a safe recognition of cross allergens (available qualitative and quantitative contaminations in food production lines is of high methods): importance in quality control.
To protect consumers prone to allergy, Directive 2000/13/EC and amendments identify allergens • Gluten, in ingredients of processed foods which must be • Soya, presented on their labels. • Fish,
• Total milk, Food industry is not capable to guarantee food • Nuts, products completely free from allergens. Quality • Celery, management systems minimize risk of cross contamination, but need to be verified on on-going • Mustard, basis. • Sesame, • Hen´s egg protein Therefore laboratory outsourcing of allergens and others. detection and quantification in a diverse range of matrixes is essential for many food producers.
45 Method applied - real-time PCR is a method for the Allergen PCR LOD LOQ Our allergen testing services are complemented specific an sensitive detection of a defined DNA Gluten ≤ 0.5 ppm 1 ppm by high quality protein ELISA and enzymatic sequence by a strong increase (amplification) of this Crustacean ≤ 2 ppm 3 ppm assays for parameters that cannot be analysed Fish ≤ 0.5 ppm 1 ppm target sequence. by real-time PCR such as: Peanut ≤ 1.5 ppm 3 ppm
Soya ≤ 2 ppm 7 ppm
The PCR technology is using the potential Almond ≤ 3 ppm 25 ppm • Gluten, of an enzyme that is basically present in any living Hazelnut ≤ 2 ppm 16 ppm • Hen´s egg protein, organism in the world: DNA polymerase. This protein Walnut ≤ 10 ppm 40 ppm • Hazelnut, Cashew nut ≤ 2 ppm 10 ppm completes a DNA single strand by production • Peanut, Pecan nut ≤ 4 ppm 22 ppm of a complementary strand to a double strands • Almond, Brazil nut ≤ 0.5 ppm 1 ppm
molecule. Thereby the amount of target molecule Pistachio ≤ 0.5 ppm 1 ppm • Total milk - detection of caseinates is increased. Macadamia nut ≤ 1 ppm 6.5 ppm and milk protein. Celery ≤ 0.5 ppm 5 ppm
Mustard ≤ 1 ppm 2 ppm To get an information for allergen labeling Sesame ≤ 0.5 ppm 1 ppm it is important to particularly quantify low allergen Lupin ≤ 1 ppm 2 ppm
contents from 1 ppm to 400 ppm. J.S. Hamilton Molluscs ≤ 0.5 ppm 1 ppm Poland Ltd. laboratories provide reliable quantitative i n f o r m a t i o n o n a l l e r g e n c o n t e n t i n t h e r a n g e of 1 ppm to 400 ppm, see the Table on the right:
46 GMO
Genetically Modified Organisms (GMO) are Like in other countries, also EU has a legislation organisms whose genetic material has been concerning the approval of cultivation and use artificially modified by genetic techniques. of GMO.
Nowadays, rather simple microorganisms are most For seeds, food and feed stuffs, a use of often genetically modified, however, also there are non-approved GMO is forbidden (zero tolerance). techniques available to do the same with complex The use of authorized GMO in food and feed animals and plants. products must be labeled. An important exemption is unintended and technically unavoidable traces Most common applications of GMO techniques below 0.9 % which do not need to be labeled. concern corn, rice, soya and cotton. Mostly, genes r e s i s t a n t t o p e s t s a n d h e r b i c i d e s a r e i n t r o d u c e d in these plants.
47 GMO screening GMO identification
Any GMO – authorized and non-authorized Next step is to exactly identify respective genetically in the EU – must be detected to answer the question modified organism. It is necessary for classification if a sample contains GMO. as an authorized or unauthorized GMO event.
Since it is not possible to detect all existing GMO Since in EU, there is a “zero tolerance” for species, the solution is to apply screening method unapproved GMO, even smallest traces of them are in GMO analysis. forbidden. Especially helpful information is therefore k n o w l e d g e a b o u t i n g r e d i e n t s i n t e s t e d s a m p l e With that method, the presence of as much to exclude possible GMO - a number of respective as possible GMO is detected with as less as possible GMO can be limited. analytical work. Further, specific PCR system can confirm the A negative result of a proper screening means p r e s e n c e o f a p a r t i c u l a r G M O . P C R m e t h o d a GMO free sample. A positive screening result is unique to identify each GMO event. generally needs a subsequent identification of the present GMO.
48 GMO quantification J.S. Hamilton Poland Ltd. laboratories offer all methods of GMO testing and provide reliable results Unintended and/or technically unavoidable in short time by real-time PCR method: presence of approved GMO below 0.9 % is an • GMO-Screening (Customer-specific GMO exemption in EU-regulation concerning GMO screening, qualitative method); labeling of food and feed products. Consequently, • Single Screening (detection of the 35S promoter); possibility of quantitative determination of GMO • Single Screening (detection of the NOS amount is important for food and feed producers to terminator); decide about the necessity of labeling. • Double screening – (detection of the 35S promoter and the NOS terminator); Quantification refers to the relative GMO • Triple Screening – (detection of the 35S promoter, content in relation to the total species content, NOS terminator and the 34S FMV promoters); e.g. the amount of GMO corn relative to total corn • Identification of specific GMO event, in percent. qualitative method; • Quantification of specific GMO event , quantitative method.
Our analysts cooperate with GMO experts in Europe who may assist providing professional advice to our Customers.
49 Miscellaneous Chemical Contaminants: Dioxines, PCBs, PAHs, Melamine, Acrylamide General principles and requirements of food NITRATES law have been laid down in the Regulation (EC) No 178/2002 of the European Parliament and Regulation (EC) No 1881/2006 set the maximum o f t h e C o u n c i l . T h e R e g u l a t i o n d e c l a r e s t h a t levels of nitrates in fresh and processed spinach, “it is necessary to ensure that consumer confidence in lettuce, in processed cereal-based foods and and the confidence of trading partners is secured” baby foods for infants and young children. In addition and general public should be informed “where to their use in agricultural practice, the nitrates are there are reasonable grounds to suspect that a food also applied as preservatives in foodstuffs. may present a risk to health”. Their legislation is then joined with that of other According to the article 14 of the Regulation “food additives (see chapter: PRESERVATIVES, DYES, shall not be placed on the market if it is unsafe”. SWEETENERS & OTHER ADDITIVES). Commission Regulation (EC) No 1881/2006 of 19 December 2006 set maximum levels for certain J.S. Hamilton Poland Ltd. laboratories carry out contaminants in foodstuffs. In Annex to this Regulation analysis of nitrates according to the following the following groups of substances are listed: nitrates, validated and accredited methods: mycotoxins, metals, 3-monochloropropane-1,2-diol • PN-92/A-75112 for fresh and processed fruits (3-MCPD), dioxins and PCBs dioxin-like, polycyclic and vegetables aromatic hydrocarbons (PAHs). Testing of mycotoxins • PN-EN ISO 14673-1:2004+Ap1:2007; and metals was presented in previous chapters of ISO 14673-1:2004; IDF-FIL 189-1:2004 – for milk this brochure. and milk products.
51 Dioxins and dioxin-like polychlorinated biphenyls In order to be able to sum up the toxicity of different Congener TEF value Congener TEF value (PCBs) congeners, the concept of toxic equivalency factors Dibenzo-p-dioxins (PCDDs) Dioxin-like PCBs (TEFs) has been introduced. Non-ortho PCBs + Mono-ortho PCBs According to the scientific opinion of WHO 2,3,7,8-TCDD 1 1,2,3,7,8-PeCDD 1 Nono-ortho PCBs cited by the Regulation (EC) No 1881/2006, the 1,2,3,4,7,8-HxCDD 0,1 PCB 77 0,0001 g r o u p o f d i o x i n s c o n t a i n s 7 5 p o l y c h l o r i n a t e d The analytical results relating to the individual dioxin 1,2,3,6,7,8-HxCDD 0,1 PCB 81 0,0001
dibenzo-p-dioxin (PCDD) congeners and 135 and dioxin-like PCB congeners of toxicological 1,2,3,7,8,9-HxCDD 0,1 PCB 126 0,1 polychlorinated dibenzofuran (PCDF) congeners, concern are expressed in terms of a quantifiable 1,2,3,4,6,7,8-HpCDD 0,01 PCB 169 0,01 of which 17 are of toxicological concern. unit, namely the TCDD toxic equivalent (TEQ). OCDD 0,0001
Dibenzofurans Mono-ortho PCBs Polychlorinated biphenyls (209 congeners) can The TEF values for dioxins and dioxin-like PCBs, (PCDFs) be divided into two groups according to their according to the Regulation (EC) No 1881/2006, are 2,3,7,8-TCDF 0,1 PCB 105 0,0001 1,2,3,7,8-PeCDF 0,05 PCB 114 0,0005 toxicological properties: 12 congeners exhibit presented in following table. 2,3,4,7,8-PeCDF 0,5 PCB 118 0,0001 toxicological properties similar to dioxins and are 1,2,3,4,7,8-HxCDF 0,1 PCB 123 0,0001
therefore named dioxin-like PCBs. The other PCBs 1,2,3,7,8,9-HxCDF 0,1 PCB 156 0,0005 have a different toxicological profile. Each congener 1,2,3,6,7,8-HxCDF 0,1 PCB 157 0,0005 of dioxins or dioxin-like PCBs exhibits a different level 2,3,4,6,7,8-HxCDF 0,1 PCB 167 0,00001 1,2,3,4,6,7,8-HpCDF 0,01 PCB 189 0,0001 of toxicity. 1,2,3,4,7,8,9-HpCDF 0,01
OCDR 0,0001
Abbreviations used: T = tetra; ‘Pe’ = penta; ‘Hx’ = hexa; ‘Hp’ = hepta; ‘O’ = octa; ‘CDD’ = chlorodibenzodioxin; ‘CDF’ = chlorodibenzofuran; ‘CB’ = chlorobiphenyl.
52 Polycyclic Aromatic Hydrocarbons (PAHs). J.S. Hamilton Poland Ltd. laboratories carry out analyses of benzo(a)pyrene by HPLC with According to the opinion of the Joint FAO/WHO fluorescence detection. Export Committee on Food Additives (JECFA) a number of polycyclic aromatic hydrocarbons The method is accredited for fats and oils of both (PAH) were found to be genotoxic carcinogens. vegetable and animal origin. The analyses can be PAHs can contaminate food mainly during smoking performed on both delivered samples of fats and or drying processes with use of combustion oils as well as on fat extracted from any foodstuff. gases and through the environmental pollution (in particular fish and fishery products). J.S. Hamilton Poland Ltd. laboratories develop a m e t h o d f o r d e t e r m i n a t i o n o f n e x t t h r e e One of the group - benzo(a)pyrene - is used as PAHs (benz(a)anthracene, benzo(b)fluoranthene, a marker for the occurrence and effect of all chrysene) listed in Commission Regulation (EU) carcinogenic PAHs in food. No 835/2011 of 19 August 2011. This Regulation will apply from 1st September 2012. The Regulation (EC) No 1881/2006 set the maximum levels of benzo(a)pyrene for the following foodstuffs: In the Regulation (EC) No 1881/2006 the following carcinogenic PAHs are listed: oils and fats, smoked meat and meat products, muscle meat of fish and fishery products, crustaceans, benzo(a)pyrene cyclopenta(c,d)pyrene cephalopods, bivalve mollusks, processed cereal- benz(a)anthracene dibenz(a,h)anthracene, based foods and baby foods. benzo(b)fluoranthene dibenzo(a,e)pyrene
benzo(j)fluoranthene, dibenzo(a,h)-pyrene
benzo(k)fluoranthene dibenzo(a,i)pyrene
benzo(g,h,i)perylene, dibenzo(a,l)pyrene,
chrysene indeno(1,2,3-cd)pyrene
5-methylchrysene
53 Melamine J.S. Hamilton Poland Ltd. laboratories have validated The range of realization of the method is and accredited own method for determination 100 μg/kg up to 20 000 μg/kg. Melamine is an organic compound, rich in nitrogen of melamine in food and feed based on gas Typical chromatograms are presented below. (66 % by mass), which was implicated as contaminant chromatography coupled with mass spectrometry. in Chinese protein adulteration incidents. High
levels of melamine in food result in very severe Chromatograms of melamine
health effects. In order to counter the risk for health, Abundance TIC: wz1-3.D Abundance TIC: crm1.D 1450000 1900000 the European Commission has imposed special 1400000 1350000 1800000
conditions governing import of products containing 1300000 1700000 1250000
milk or milk products originating or consigned from 1200000 1600000
1150000 1500000 Melamine (TMS derivative) China (Decision 757 of 26 September 2008). 1100000
1050000 1400000
1000000 Melamine (TMS derivative) 1300000 950000
The Commission requires that “Member States should 900000 1200000 ) 850000 1100000 ensure that all composite products containing 800000
750000 1000000 )
at least 15 % of milk product, originating from 700000 900000 China, are systematically tested before import 650000 600000 800000 DACP - IntStnd (di-TMS derivatve 550000 into the Community and that all such products 700000 500000
450000 600000 w h i c h a r e s h o w n t o c o n t a i n m e l a m i n e i n e x c e s s o f DACP - IntStnd (di-TMS derivatve 400000 500000 2,5 mg/kg are immediately destroyed. (…) Composite 350000 300000 400000
250000 products, whose milk product content cannot be 300000 200000 established, should also be tested.” 150000 200000 100000 100000 50000
Time--> 9.50 10.0010.50 11.0011.50 12.0012.50 13.0013.50 14.0014.50 15.0015.50 16.0016.50 17.0017.50 18.0018.50 19.0019.50 20.00 Time--> 9.50 10.0010.50 11.0011.50 12.0012.50 13.0013.50 14.0014.50 15.0015.50 16.0016.50 17.0017.50 18.0018.50 19.0019.50 20.00 Standard solution. CRM, feed. Found value = 13 mg/kg. Chromatographic conditions: GC-MS; column type DB-5, 30 m x 0,25 mm x 0,25 µm; programmed gradient temperature; split injection 280ºC; carrier gas: helium.
54 Acrylamide This monitoring has been extended by Commission FAO/WHO Codex Alimentarius Commission has Recommendation 2010/307/EU of 3 June 2010. Data p u b l i s h e d t h e C o d e o f P r a c t i c e f o r t h e R e d u c t i o n In April 2002, the Swedish National Food Authority from 2007 – 2008 have been used to set indicative of Acrylamide in Foods (CAC/RCP 67-2009). r e p o r t e d t h e p r e s e n c e o f e l e v a t e d l e v e l s a c r y l a m i d e v a l u e s t h a t a r e i n c l u d e d t o A n n e x o f a c r y l a m i d e i n c e r t a i n t y p e s o f f o o d p r o c e s s e d to the Commission Recommendation of 10.01.2011 Soon after the Swedish report on acrylamide at high temperatures. Since then, acrylamide has on investigations into the levels of acrylamide presence in food, was published, J.S. Hamilton been found in a range of cooked and heat-processed in food. Poland Ltd. laboratories have validated and foods in other countries, including Netherlands, accredited own method for determination of this Norway, Switzerland, United Kingdom and United The following foodstuffs are listed (in brackets – contaminant. States. Acrylamide is a naturally occurring chemical indicative values): compound, formed from sugars and aminoacids • French fries ready-to-eat (600 μg/kg), found in many plant-based, high-carbohydrate • Potato crisps (1000 μg/kg), foods after they are heated to high temperatures. • Soft bread (150 μg/kg), It is believed to cause cancer by damaging DNA. • Breakfast cereals (excl. muesli and porridge) Certain doses of acrylamide are toxic to the nervous (400 μg/kg), system of both animals and humans. • Biscuits, crackers, wafers, crisp bread and similar, excl. ginger bread (500 μg/kg), Till now, the acrylamide maximum levels in food are • Roast coffee (450 μg/kg), not established. In order to get a better overview, • Instant (soluble) coffee (900 μg/kg), acrylamide contents in food have been monitored • Baby foods, other than processed cereal based by EU countries from 2007 – 2009 under Commission foods (80 μg/kg). Recommendation 2007/331/EC of 3 May 2007.
55 Acrylamide analyses carried out by J.S. Hamilton Poland Ltd. in 2005 - 2008 Chromatograms of acrylamide
Abundance TIC: wz3-2.D
Number of Acrylamide contents [µg/kg] 75000 75000 analyzed samples maximum minimum average 70000 70000 processed potato 22 1269 77 238 65000 65000 roasted chicory 7 3491 297 1647
60000 60000 breakfast cereal 41 408 103 205 products 55000 55000 d confectionery 29 1079 17 156 50000 50000 roasted cereals drink 11 726 688 707 45000 Metakrylami 45000 glucose syrup 29 all results below the limit of quantification
40000 Akrylami d 40000 other below the limit of 5 710 34 quantification 35000 35000
30000 30000 Acrylamide analyses are performed by means of gas chromatography coupled with mass 25000 25000 id
spectrometry. Typical chromatograms are presented on the right: 20000 am
20000 yl takr Me
15000 15000 d mi
10000 10000 la ry Ak
5000 5000
Time--> 6.00 7.00 8.00 9.00 10.0011.00 12.0013.00 14.0015.00 16.00 Time--> 6.00 7.00 8.00 9.00 10.0011.00 12.0013.00 14.0015.00 16.00 Acrylamide standard solution. Acrylamide (310 µg/kg) in cereal snacks (saltletts) Chromatographic conditions: GC-MS/PCI; column type: Wax, 30 m x 0,32 mm x 0,25 µm; programmed gradient temperature; split injection 260ºC; carrier gas: helium.
56 Chloramphenicol J.S. Hamilton Poland Ltd. laboratories have validated and accredited own method for determination C h l o r a m p h e n i c o l i s a p r o t o t y p i c a l a n t i b i o t i c of chloramphenicol in food of animal origin by gas of a broad spectrum. Due to resistance and safety chromatography coupled with mass spectrometry. concerns it is included to the list of pharmacologically The range of that analysis is 0,1 μg/kg to 10 μg/kg. active substances for which no maximum levels can be fixed (Annex IV to the Council Regulation EEC 2377/90 of 26 June 1990 laying down a Community procedure for the establishment of maximum residue limits of veterinary medicinal products in foodstuffs of animal origin).
57 Sensory Analysis & Consumer Preference Testing There are different concepts of quality, one of them The standard defines general requirements being so called sensory quality, i.e. the objective concerning: evaluation using the senses, as well as perceived • statement of objectives, q u a l i t y t h r o u g h c o n s u m e r ’ s s e n s e s i n d i c a t i n g • choice of test, his/her positive or negative perception of • choosing and training assessors, a product. • material to be tested, • test room, That latter evaluation of quality is subjective - it reflects • planning and conducting of tests. perceived emotional relationship of an individual consumer. The tests are divided into three groups: • discrimination tests used to determine Sensory quality should be tested in standardized the probability of difference conditions, using standardized methods, or similarity between products, by competent qualified and calibrated assessors. • tests using scales and categories to estimate ISO 6658:2005 standard provides general guidance order or size of differences, on the sensory analysis. This international standard • descriptive tests to identify specific attributes describes methodology for the examination of foods of a sample. by the sense organs.
59 Sensory profile of chocolate sample Consumer preference testing - sensory attributes of instant coffee samples
6,00
5,50
5,00
4,50
4,00
3,50 a e ce es sion te as fe om n ha an rt es r t Ar ar te Af nt cof nt impr l eshe ta Appe al s fr ns
er r i te Ov as he
ot It t brewed ground coffe It tastes like freshly Sample 7470 Sample 7471 Product A Product B Product C Standard
60 The consumers preference testing allows you Tests conducted by J.S. Hamilton Poland Ltd. to get know consumers opinion on tested products. laboratories are performed on a wide selection Thanks to this research an information is obtained, of programmed consumer panels with regard why do consumers choose certain products from t o s e x , a g e , s o c i o - p r o f e s s i o n a l c a t e g o r i e s , f r e q u e n c y among others. Hence allow you to design or modify of consumption etc., in isolated environment, free the product, its packaging, appearance, colour, from noise, extraneous odors, etc. texture, flavour and odours, taste and smell, to reach the maximum possible market success. Consumer responses are evaluated using specific statistical methods. Conclusions drawn from studies of consumer preference may allow to create such a product, J.S. Hamilton Poland Ltd. sensory laboratory has which is motivating to its purchase and positively been designed to meet all requirements of PN-EN affects consumer’s loyalty to a given product ISO 8589:2010 Standard which provides general or brand. guidance for the design of test rooms intended for the sensory analysis of products.
61 Migration From Packagings As a result of contact of food with packaging The Regulation set out the upper limit of overall or other material, undesirable substances can migration to be 10 milligrams of total constituents migrate to foodstuffs. European legislation protects released from plastic materials and articles consumers’ health by banning materials and articles p e r s q u a r e d e c i m e t e r o f f o o d c o n t a c t s u r f a c e in packaging which may transfer their constituents (mg/dm2). to foodstuffs. This applies both to substances affecting directly human health but also causing By derogation, plastic materials and articles substantial changes of foodstuffs, deteriorating their intended to be brought into contact with food organoleptic characteristics. intended for infants and young children, shall not transfer their constituents in quantities exceeding The last EU act concerning migration is the 60 milligrams of total of constituents released per C o m m i s s i o n R e g u l a t i o n ( E U ) N o 1 0 / 2 0 1 1 o f kg of food simulant. 14 January 2011 on plastic materials and articles intended to come into contact with food. S p e c i fi c m i g r a t i o n l i m i t s ( S M L ) a r e s e t o u t i n A n n e x I to the Regulation and are expressed in mg According to the Regulation “overall migration limit’ of substance released from plastic materials and ( O M L ) m e a n s t h e m a x i m u m p e r m i t t e d a m o u n t articles per kg of food (mg/kg). of non-volatile substances released from a material or article into food simulants”, while “specific migration limit’ (SML) means the maximum permitted amount of a given substance released from a material or article into food or food simulants”.
63 Basic rules necessary for testing migration J.S.Hamilton Poland Ltd. laboratories apply a wide of constituents of plastic materials and articles range of analytical methods for analyses of food intended to come into contact with foodstuffs were packaging: laid down in the Council Directives 78/142/EEC and 8 2 / 7 1 1 / E E C o f 1 8 O c t o b e r 1 9 8 2 . T h e u p d a t e d r u l e s • Analysis of overall migration (OML) of harmful on food simulants and migration testing are provided substances from plastic materials and articles into by the Commission Regulation 10/2011 of 14 January food. 2011. The food simulants are listed in point 3 of Annex The following simulant liquids are involved: III to this Regulation. ◦◦ distilled water, ◦◦ 3 % acetic acid, Although the EU legislation is focused mainly ◦◦ isooctane, on plastics, it is to be noted that also such materials ◦◦ 10 % ethyl alcohol, as paper, metals, ceramics which are commonly ◦◦ 95 % ethyl alcohol. u s e d f o r t h e m a n u f a c t u r i n g o f f o o d p a c k a g i n g as well as kitchenware, cutlery and food processing Accredited methods in accordance with PN-EN 1186 equipments should be checked to assure that are applied for overall migration testing. d u r i n g c o n t a c t t h e r e i s n o m i g r a t i o n o f u n s a f e l e v e l s of chemical substances from the material to the • Packaging materials and ready made food. packagings are also tested by sensory assessment for taste and odour transferred in direct contact, using accredited multi-comparative method described in DIN 10955 and PN-EN 1230-1; PN-EN 1230-2.
64 • The specific migration (SML) - determination • Determination of heavy metals Pb, Cd, Hg, Cr of content of such residual substances such in accordance with the requirements of Directive as phenol and formaldehyde in packaging, 94/62/EC (manufacturers of packagings are in specified test conditions using selected food obliged to reduce content of heavy metals in their simultants. These analyses are performed by means products). of gas chromatography, liquid chromatography, mass spectrometry and other.
• Microbiological tests of packaging materials and ready packages for total count of bacteria, molds and yeast and other pathogens in all types of packaging.
65 Microbiology According to the Commission Regulation (EC) No Presence of the following micro-organisms 2073/2005 of 15 November 2005 on microbiological constitutes food safety criteria: c r i t e r i a f o r f o o d s t u f f s , m i c r o b i o l o g i c a l h a z a r d s • Salmonella, in foodstuffs cause a major source of food-borne • Listeria monocytogenes, diseases in humans. • Enterobacter sakazaki, This Regulation as well as the amending • Escherichia coli, Commission Regulation (EC) No 1441/2007 of • Staphylococcal enterotoxins. 5 December 2007 establishes harmonized safety criteria on acceptability of food, particularly Criteria for assessment of production process in relation to presence of certain pathogenic hygiene are following: micro-organisms. Criteria can be used in validation • Aerobic colony count, and verification of HACCP procedures and other • Enterobacteriaceae, hygiene control measures. • Salmonella, • Escherichia coli, Regulation specifies: • Coagulase-positive staphylococci, • “food safety criterion” defining acceptability • Presumptive Bacillus cereus. of a product or a batch of foodstuff applicable to products placed on the market, • “process hygiene criterion” indicating the acceptable functioning of the production process. Such a criterion is not directly applicable to products placed on the market.
67 J.S. Hamilton Poland Ltd. microbiological laboratories Other microbiological analyses are carried out located in Gdynia, Poznań, Katowice and Maków as well, namely: Mazowiecki (near capital city of Warsaw) are • Bacillus subtilis, fully equipped for a wide range of food analysis • Molds and yeast, and provide monitoring services at each stage • Lactic acid bacteria, of production process. The offer includes • Spore-forming and non-forming anaerobic, environmental control applying methodology • Clostridium perfringens described in Polish Standards, generally harmonized • Enterococcus with European and ISO standards. • Pathogenic bacteria in yoghurt, • Camphylobacter sp. • Osmophyllic yeast and molds, • Halophyllic bacteria, • Shelf life tests by tghermostatic method.
68 Apart from classical standard procedures BAX® automated DNA-based pathogen detection Microbiological purity of drinking water is also tested J.S. Hamilton Poland Ltd. microbiological system is also offered by J.S. Hamilton Poland Ltd. in our laboratory network to prove the compliance laboratories assure validated and accredited laboratories. with current legislation, namely with the Council less-time-consuming (results available even after Directive 98/83/EC and with corresponding Polish 24h!) alternative methods - TEMPO® and BAX® The BAX® system can be applied for: regulations. systems. • Milk and dairy products, • Meat and meat products, The Directive sets quality standards for drinking Using TEMPO® system the following analyses are • Sea food, water (microbiological, chemical and organoleptic carried out: • Fresh and processed fruits and vegetables, parameters). J.S. Hamilton Poland Ltd. laboratories • Total Viable Count (TVC), • Feed, have been approved by State Sanitary Inspection • Total Coliforms (TC), • Spices for sampling and for testing of drinking water. • Escherichia coli (EC), • Chocolate • Enterobacteriaceae (EB), • Pet foods • Staphylococcus aureus (STA). • Environmental samples.
Correlation between TEMPO and classical methods is high enough (with correlation factor in a region of 0.90 to 0.99), thus providing quick and efficient testing tool.
69 Training & Consultancy Training Services Training topics are tailored to meet the needs and expectations of our customers, and may be arranged In the dynamic and variable market place well- at any suitable location across the country. educated and trained staff, capable to cope with challenging environment, is a unique value for each Our offer covers following areas: company. • Sensory analysis of food products and water, J.S. Hamilton Poland Ltd. laboratories helps its • Microbiological testing of food raw material and customers in this respect by provision of professional final product as well as water, training, workshops and consultancy for all aspects • Streamlining of food production process, of quality related issues, laboratory techniques and • Food safety management, legislative requirements. • Environment.
Our mission is to provide a high quality training 2-3 days trainings in sensory analysis provided and education services together with consultancy by our sensory laboratory and dedicated for services to our customers who are operating in food various food processing industries are particularly processing and trading industries, and are targeting recommended. Our training offer also includes a successful business in a high level of quality. trainings for microbiological laboratory staff or quality managers. Trainings are conducted by our most experienced staff members but also by guest lecturers being leading specialists in their fields of expertise. Trainings are carried out in such a way that participants are provided with not only knowledge but also practical skills.
71 Typical training topics include: • Rice. Characteristics and quality control; • Herbs and spices - necessary ingredients General Food Sector: of food ; • Various aspects of food labeling. • Quality and sensory control of cheese. The information required, allowed and forbidden on the packaging; Food Safety Management Food modeling. Theory and practice; • HACCP as a method of food safety • Authenticity and adulteration of food; management; • Safety food packaging - requirements, testing, • The internal auditor of food safety management new solutions; according to system (ISO 22000: 2005); • Microbiology for “non-microbiologists”; • Control of measurement and test equipment; • Hygiene in the production process; • Audit in microbiological laboratory. • Microbiological contamination of feeding stuffs ; • Safety of cereal in the light of law; Environmental Protection • Sampling of raw materials and interpretation of • Management of sewage sludge. analytical results; Theory and practice; • Sampling of food samples from the production • Waste management. surface, tools, hands and air samples; Producers responsibilities • Determination of ochratoxin A in spices; and legal requirements; • Sensory analysis and quality checking of fish and • Microbiological analysis of water. fish products; • Sensory group leader;
72 Consulting And Audits Our team of auditors provides also a wide range of auditing services focused on food industry, food We provide a wide range of consultancy services retailers and catering sector. with regard to food quality and safety (chemistry, biochemistry, microbiology, veterinary, food legislation).
This may cover: • specific requirements for quality of raw materials and products (technology, food hygiene, HACCP, GMP, traceability and food safety risk assessment), • assessment and interpretation of the results of current quality control and long-term quality monitoring, • labeling of foodstuff – verification, • risk assessment and crisis management.
73 Laboratory Staff
With 50 years of experience of J.S. Hamilton Poland Ltd., trained and skilled laboratory staff allows us to provide high scientific standards. Strong customer focus is led by our Business Development and Sales Team. Responsive to our customers, the team is committed to delivering a tailor made, one-stop service that is dedicated to ensuring that our customers receive the highest standard of service at all times.
200ml
150ml
100ml
50ml Accreditation
The majority of J.S. Hamilton Poland Ltd. food testing services are covered by PCA accreditation (No. AB079) and as such we have one of the most extensive scopes in Poland and Europe. We are also GAFTA and FOSFA approved. In addition to this, we are flexible and can work to your preferred methods.
75 How to submit samples
Samples should be shipped to the following address: J.S. Hamilton Poland Ltd. Laboratories ul. Indyjska 13 81-336 GDYNIA/ POLAND
Following information should be attached to each sample/set of samples: • description of sample/samples; • list of tests required; • required turnaround time: standard or express; • company name, name of contact person, address, phone and e-mail for Reporting; • invoice address; • our offer Ref. number (if received).
For additional information : Contact us: Phone: + 48 58 660 27 51 e-mail: [email protected]
76 24h Check your results on-line www.hamilton.com.pl
At Hamilton laboratories, we understand how important is for our Customers easy access to test results. Our dedicated on-line, web-based IT system offers an easy-to-use tool to obtain ongoing information on testing progress and test results. Hamilton on-line service ensures: • confirmation that your samples have been delivered to laboratory, • status of sample check, • access to in-process results before all analyses are completed, • easy available archive files of tested samples and obtained results.
By simple logging in on our website you may get above information from any place in the world.
www.hamilton.com.pl Standard Terms and Conditions
Sample collection Results Reporting
We offer collection of samples at any location and All Test Reports are generated electronically and their delivery to our laboratories on the following signed with a certified electronic signature. working day. To order sample collection please contact us: phone +48 58 660 2751 or e-mail: General Conditions of Business [email protected]. All services provided by are performed Sample Storage in accordance with General Conditions of Business, copy available on our website Unless otherwise agreed samples will be stored www.hamilton.com.pl for thirty (30) days after completion of tests in appropriate conditions relevant to their nature. Confidentiality In case of their shorter durability storage time will be limited to their shelf life . All services, analyses and reports are provided to exclusive use of our customers on a confidential Turnaround Time basis.
S t a n d a r d t u r n a r o u n d t i m e i s 1 0 w o r k i n g d a y s . We offer a quick option of 5 working days. Such an express option entails 50% surcharge.
78 www.hamilton.com.pl
79 J.S. Hamilton Poland Ltd.
HEAD OFFICE OTHER BRANCHES ul. Świętojańska 134 Braniewo 81-404 Gdynia phone: +48 603 460 029 phone: +48 58 660 77 20 e-mail: [email protected] e-mail: [email protected] Dorohusk phone: +48 83 375 00 41 e-mail:[email protected] Gdańsk FOOD TESTING LABORATORIES phone: +48 58 737 70 72 Central Laboratory e-mail: [email protected] ul. Indyjska 13 Hrubieszów 81-336 Gdynia phone: +48 85 711 99 00 phone: +48 58 660 27 51 e-mail: [email protected] e-mail: [email protected] Małaszewicze
Katowice phone: +48 83 375 00 41 ul. Modelarska 12 e-mail: [email protected] 40-142 Katowice Siemianówka phone: +48 32 730 27 01 phone: +48 85 685 71 51 e-mail: [email protected] e-mail: [email protected] Sokółka Maków Mazowiecki phone: +48 85 711 99 00 ul. Przemysłowa 5 e-mail: [email protected] 06-200 Maków Mazowiecki Szczecin phone: +48 29 71 73 009 phone: 48 91 820 36 33 e-mail: [email protected] e-mail: [email protected] Warszawa Poznań phone: +48 22 460 49 20 ul. Dożynkowa 9, Blok G e-mail: [email protected] 61-660 Poznań Wrocław phone: +48 61 862 16 73 phone: +48 605 720 277 e-mail: [email protected] e-mail: [email protected] Żurawica phone: +48 83 375 00 41 e-mail: [email protected]