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Effectiveness of Accelerated Solvent Extraction Compared to Quechers Method for the Multiresidue Analysis of Pesticides in Organ

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Effectiveness of Accelerated Solvent Extraction Compared to Quechers Method for the Multiresidue Analysis of Pesticides in Organ CUSTOMER APPLICATION NOTE 72442 Effectiveness of accelerated solvent extraction compared to QuEChERS methods for the multiresidue analysis of pesticides in organic honey by GC-MS/MS Authors Goal Fabrizio Galbiati1; Sara Panseri2; Compare in-line ASE methods cleanup conditions for the evaluation of Giuseppe Labella2; pesticides in honey to QuEChERS methods. Domenico Britti3; Roberto Villa2; Francesco Arioli2; Luca Chiesa2 Introduction 1Thermo Fisher Scientific (Schweiz) According to the Council Directive 2001/110/EC,1 honey is considered as AG, Reinach, Switzerland; a “viscous, aromatic, natural, and sweet fluid produced by Apis mellifera 2Department of Health, Animal bees2,3 from the nectar of flowers or secretions of live parts of certain plants Science and Food Safety, or excretions of insects.” It has been used in medicine since ancient times for University of Milan, Milan, Italy; treatment of burns, gastrointestinal disorders, asthma, infected wounds, and 3Department of Health Sciences, skin ulcers.4 University of Catanzaro Magna Graecia, Catanzaro, Italy World production of honey has increased in the last 20 years. In 2014, 1.5 million tons of honey were produced worldwide, with China accounting for 31% of the world total followed by Turkey, the United States, Ukraine, and the Keywords Russian Federation. Pressurized fluid extraction, multiresidue pesticide analysis, in-line clean up, Rocket Evaporator, TSQ 8000 Triple Quadrupole GC-MS, Dionex ASE 350 Accelerated Solvent Extractor There are two main forms of contamination of honey: The high temperature allows a higher rate of extraction cross-contamination as bees collect pollen and nectar due to a reduction of the viscosity and surface tension, and contamination through treatment of hives with and increases the solubility and diffusion rate into the insecticides, fungicides, and acaricides for the protection sample. At the same time, high pressure prevents the from parasites like Varroa destructor, Acarapis woodi, and solvents from reaching their boiling point and promotes Paenibacillus larvae. penetration into the sample. Recent advances using ASE systems are described in several publications,9,10 and Although some organizations, such as the U.S. Food include procedures for selective removal of interferences and Drug Administration (FDA)5 and the Canadian during sample extraction, thus combining extraction and Food Inspection Agency,6 approve the use of certain purification into a single step. veterinary drugs, the European Union does not accept the use of antimicrobial drugs in beekeeping. The use of The methods reported here are applicable for the veterinary medicinal products in beekeeping is regulated determination of 53 pesticides, including acaricides and by the European Council (EC,1804/1999). According insecticides (both chlorinated and non-chlorinated) in to this regulation, the use of allopathic chemically organic honey and in concentrations from 1 to 100 ng/g. synthesized medicinal products for preventive treatments in beekeeping is prohibited, as these fat-soluble and Experimental nonvolatile compounds can accumulate in the stored Honey Samples honey, where they are able to migrate from the wax This study included 45 organic honey samples. In comb. The Council Regulation 1804/1999 EC7 is very particular, 10 orange blossom honey samples were restrictive regarding the production of organic honey from a German beekeeper and 35 were from Italian in terms of the origin of bees, siting of the apiaries, beekeepers of two different regions: Calabria (south Italy, feed, disease prevention, and veterinary treatments. In 15 samples), where intensive citrus orchards are present, particular, it establishes that plants that can be foraged and Trentino-Alto Adige (north Italy, 20 samples), where by bees, either biological or spontaneous, must be at intensive apple orchards are present. All samples were least 3 km from any source of pollution and from any stored at -20°C until analysis to prevent decomposition. non-agricultural production sources, that can possibly lead to contamination, such as industrial areas, urban Equipment centers, or motorways. A Radwag analytical balance was used for weighing the honey samples. The extractions were carried out with The determination of pesticide residues in honey is a a Thermo Scientific™ Dionex™ ASE™ 350 Accelerated considerable analytical challenge, as honey is a mixture Solvent Extractor [P/N 083114 (120 V) or 083146 of more than 300 substances identified mainly as sugars (240 V)], shown in Figure 1A, equipped with 34 mL and waxes, subject to variations arising from the type stainless steel extraction cells. The extracts were of plant(s) where bees collect nectar.8 Its complexity collected in 60 mL vials (Thermo Scientific, P/N 048784), requires a selective sample preparation because treated with sodium sulfate and directly concentrated carbohydrates and other matrix substances can be in a 2 mL autosampler glass vial (Thermo Scientific™ co-extracted with the analytes. These unwanted co- Chromacol™ VAGK ISP: GC 2-SVW + 9-SCK(B)-ST1) extractables can cause buildup of nonvolatile materials with the Thermo Scientific™ Rocket™ Evaporator on the GC injection port and the analytical column, [P/N 075904 (120 V) or 082766 (240 V)], shown in resulting in poor analytical results and high instrument Figure 1B. The samples were analyzed with a maintenance costs. Thermo Scientific™ TRACE™ 1310 Gas Chromatograph equipped Split/Splitless Injector, a fused-silica capillary Among the available extraction techniques, accelerated column Thermo Scientific™ TraceGOLD™ TG-5SilMS solvent extraction (ASE) is characterized by shorter (30 m × 0.25 mm × 0.25 µm), and a Thermo Scientific™ extraction times and reduced solvent consumption. ASE TSQ™ 8000 Triple Quadrupole GC-MS/MS. uses high temperatures combined with high pressure. 2 A B Figure 1. Dionex ASE 350 accelerated solvent extractor (A) and Thermo Scientific Rocket Evaporator (B). Chemicals and reagents column chromatography, 1 mL NORM-JECT® Tuberkulin Acrinathrin, bifenthrin, boscalid, bromopropylate, syringes, and 0.2 μm nylon filters were purchased from buprofezin, chlorfenvinphos, chlorpyrifos-methyl, Fisher Scientific (Schwerte, Germany). chlorothalonil, cyfluthrin, cyhalothrin, cypermethrin, deltamethrin, diazinon dichlorvos, difenoconazole, Diatomaceous earth and ASE cellulose filters were dimethoate, endosulfan (α, β, and sulfate), ethion, purchased from Thermo Fisher Scientific (Waltham, MA, ethoprophos, fenamiphos, fenitrothion, fenpropathrin, USA); ethylacetate (Lichrosolv for LC) was purchased lindane (γ-HCH), iprodion, malathion, methamidophos, from Merck (Darmstadt, Germany); Supelclean™ PSA oxadixyl, permethrin, phosalone, pirimiphos-methyl, (primary-secondary amine) was purchased from Supelco procymidon, propargite, propiconazole, pyridaben, Analytical (Bellofonte, PA, USA). quinoxyfen, tebuconazole, tetradifon, triadimefon, and vinclozolin were purchased from Sigma-Aldrich The stock solution, at a concentration of 10 μg/mL, (St. Louis, MO, USA). was prepared by dissolving the pesticide standards in hexane or acetonitrile for ASE extraction and QuEChERS, QuEChERS extraction tubes (50 mL; 4 g MgSO4, 1 g respectively. Stock solutions were stored at −40°C. NaCl, 1 g sodium citrate dihydrate tribasic, and 500 mg Calibration solutions containing all the investigated sodium citrate dibasic sesquihydrate), 15 mL QuEChERS compounds, in hexane or acetonitrile, were prepared clean-up tubes (1200 mg MgSO4, 400 mg CUPSA/ daily from the stock solutions (10 μg/mL). The appropriate 400 mg CE C18), acetonitrile (LC-MS grade), hexane volume was used as a spiking solution. (pesticide residue grade), Florisil® 60–100 mesh for 3 Accelerated solvent extraction Table 1B. Conditions for accelerated solvent extraction (n-hexane/ A cellulose filter (Thermo Scientific, P/N 056780) was ethyl acetate solvent). placed in the bottom of a 34 mL extraction cell ASE program for n-hexane/ethyl acetate solvent (Figure 2), followed by 2 g of PSA (primary-secondary (4:1, v/v) amine) or Florisil and another cellulose filter. A 5 g Adsorbent: Florisil (2 g) sample of honey was homogenized with an equal weight of Thermo Scientific™ Dionex™ ASE Prep DE Temperature: 100°C (Thermo Scientific P/N 062819), and transferred into Pressure: 1500 psi the cell. One milliliter of acetonitrile solution containing Static Cycles: 2 the internal standard (FBDE, 3-fluoro-2,2,4,4,6 pentabromodiphenyl ether) was added. The remaining Extraction Time: 5 min empty volume was filled with Dionex ASE Prep DE. The Rinse Volume: 90% extractor was programmed according to the conditions Purge Time: 90 s reported in Tables 1A and 1B. The extracts were collected in 60 mL vials and treated with sodium sulfate to remove any possible water. After filtration, the organic phase was concentrated to dryness in the Rocket Evaporator, reconstituted in 1 mL of Cellulose Filter acetonitrile or hexane, and submitted for analysis by Sample GC-MS/MS. The GC conditions are summarized (Honey+ ASE Prep DE) in Tables 2A and 2B, and the MS conditions are Extract Flow Cellulose Filter summarized in Table 3. PSA or Florisil Cellulose Filter Table 2A. Injector conditions. ASE Cell Injector program (PTV, splitless mode) Figure 2. Extraction cell schematic. Injector Temperature: 250°C Liner 2 mm x 2.75 mm x 120 mm, Siltek-deactivated Table 1A. Conditions for accelerated solvent extraction (acetonitrile solvent). Injected Volume: 1 µL Splitless Time: 1 min ASE program for
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