100 MULTI-RESIDUE ANALYSIS for PESTICIDES Multi-Residue Method for Pesticides in the U.S

100 MULTI-RESIDUE ANALYSIS FOR PESTICIDES Multi-Residue Method for Pesticides in the U.S. and European Pharmacopeias—Method Summary

This method is applicable, but not limited, to dietary supplement products and raw materials for the analysis of pesticides listed in the U.S. (USP <561> and <565>) and European Pharmacopeias (EP).1-3 The sample extraction and clean-up are based on the QuEChERS method.4,5 The final extract is split for the analysis of GC- and LC-amenable pesticides using gas chromatography-tandem mass spectrometry (GC-MS/MS) and liquid chromatography-tandem mass spectrometry (LC-MS/MS), respectively. The reporting limits are based on the limits specified in the USP and EP pesticide residue monographs.

USP <561> Limit Pesticide * (mg/kg) Acephate 0.1 Alachlor 0.05 Aldrin and dieldrin (sum of) 0.05 Azinphos-ethyl 0.1 Azinphos-methyl 1 Bromide, inorganic (calculated as bromide ion)** 125 Bromophos-ethyl 0.05 Bromophos-methyl 0.05 Bromopropylate 3 Chlordane (sum of cis- and trans- isomers and oxychlordane) 0.05 Chlorfenvinphos 0.5 Chlorpyrifos-ethyl 0.2 Chlorpyrifos-methyl 0.1 Chlorthal-dimethyl 0.01 Cyfluthrin (sum of isomers) 0.1 Cyhalothrin, λ- 1 Cypermethrin (sum of isomers) 1 DDT (sum of o,p’-DDT, p,p’-DDT, o,p’-DDE, p,p’-DDE, o,p’-DDD and p,p’-DDD) 1 Deltamethrin 0.5 Diazinon 0.5 Dichlofluanid 0.1 Dichlorvos 1 Dicofol 0.5 Dimethoate and omethoate (sum of) 0.1 Dithiocarbamates (expressed as CS2)*** 2 Endosulfan (sum of isomers and endosulfan sulfate) 3 Endrin 0.05 Ethion 2 Etrimphos 0.05 Fenchlorphos (sum of fenchlorphos and fenchlorphos-oxon) 0.1 Fenitrothion 0.5 Fenpropathrin 0.03 USP <561> Limit Pesticide * (mg/kg) Fensulfothion (sum of fensulfothion, fensulfothion-oxon, fensulfothion-oxon sulfone and 0.05 fensulfothion sulfone) Fenthion (sum of fenthion, fenthion-oxon, fenthion-oxon sulfone, fenthion-oxon sulfoxide, 0.05 fenthion sulfone and fenthion sulfoxide) Fenvalerate 1.5 Flucythrinate 0.05 Fluvalinate, τ- 0.05 Fonofos 0.05 Heptachlor (sum of heptachlor and cis- and trans-heptachlor epoxides) 0.05 Hexachlorobenzene 0.1 Hexachlorocyclohexane isomers (sum of isomers, except γ) 0.3 Lindane (γ-hexachlorocyclohexane) 0.6 Malathion and malaoxon (sum of) 1 Mecarbam 0.05 Methacriphos 0.05 Methamidophos 0.05 Methidathion 0.2 Methoxychlor 0.05 Mirex 0.01 Monocrotophos 0.1 Parathion-ethyl and paraoxon-ethyl (sum of) 0.5 Parathion-methyl and paraoxon-methyl (sum of) 0.2 Pendimethalin 0.1 Pentachloranisol 0.01 Permethrin (sum of isomers) 1 Phosalone 0.1 Phosmet 0.05 Piperonyl butoxide 3 Pirimiphos-ethyl 0.05 Pirimiphos-methyl (sum of pirimiphos-methyl and N-desethyl-pirimiphos-methyl) 4 Procymidone 0.1 Profenophos 0.1 Prothiophos 0.05 Pyrethrum (sum of cinerin I, cinerin II, jasmolin I, jasmolin II, pyrethrin I and pyrethrin II) 3 Quinalphos 0.05 Quintozene [sum of quintozene, pentachloroaniline and methyl pentachlorophenyl sulfide 1 (MPCPS)] S-421 0.02 Tecnazene 0.05 Tetradifon 0.3 Vinclozolin 0.4

* USP <565> limits are variable and are calculated as follows: If E ≤ 10: Limit (mg/kg) = L × E If E > 10: Limit (mg/kg) = AM/100B where L is the limit listed in the above table; E is the client provided plant to extract ratio (i.e., the ratio between the quantity of botanical article used in the manufacture of the extract and the quantity of the extract obtained); A is the acceptable daily intake (ADI), as published by FAO-WHO, in mg/kg of body weight; M is body weight, in kg (60 kg); and B is the daily dose of the extract, in kg. For compounds without a published ADI, 10 x L will be used. ** Bromide is determined using a different method. Bromide is only required by the USP and no longer required by the EP. *** Dithiocarbamates (EBDCs) are determined using different methods. REFERENCES

1. The United States Pharmacopeia, General Chapter 561: Articles of Botanical Origin. 2. The United States Pharmacopeia, General Chapter 565: Articles of Botanical Origin. 3. The European Pharmacopoeia, General Chapter 2.08.13: Pesticide Residues. 4. AOAC Official Method 2007.01, Pesticide Residues in Foods by Acetonitrile Extraction and Partitioning with Magnesium Sulfate. 5. CEN Standard Method EN 15662: Food of plant origin - Determination of pesticide residues using GC-MS and/or LC-MS/MS following acetonitrile extraction/partitioning and clean-up by dispersive SPE - QuEChERS method.

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