pubs.acs.org/JAFC Published on Web 03/15/2010 © 2010 American Chemical Society 5884 J. Agric. Food Chem. 2010, 58, 5884–5896 DOI:10.1021/jf903851h Multiresidue Pesticide Analysis of Ginseng Powders Using Acetonitrile- or Acetone-Based Extraction, Solid-Phase Extraction Cleanup, and Gas Chromatography-Mass Spectrometry/Selective Ion Monitoring (GC-MS/SIM) or -Tandem Mass Spectrometry (GC-MS/MS) † JON W. WONG,* ,§ KAI ZHANG, § KATHERINE TECH, # DOUGLAS G. HAYWARD, § ALEXANDER J. KRYNITSKY, § IRENE CASSIAS, ^ FRANK J. SCHENCK, X KAUSHIK BANERJEE, 4 SOMA DASGUPTA, 4 AND DON BROWN ] § Center for Food Safety and Applied Nutrition, U.S. Food and Drug Administration, HFS-706, 5100 Paint Branch Parkway, College Park, Maryland 20740-3835, # Joint Institute for Food Safety and Applied Nutrition, 1122 Patapsco Building, University of Maryland, College Park, Maryland 20742-6730, ^ Office of Regulatory Affairs, Pacific Regional Laboratory Southwest, U.S. Food and Drug Administration, HFR-PA260, 19701 Fairchild, Irvine, California 92612-2506, X Office of Regulatory Affairs, Southeast Regional Laboratory, U.S. Food and Drug Administration, HFR-SE660, 60 Eighth Street N.E., Atlanta, Georgia 30309-3959, 4 National Research Centre for Grapes, P.O. Manjri Farm, Pune, Maharashtra 412 307, India, and ] Exova U.K., 121 Shady Lane, Great Barr, Birmingham B44 9ET, United Kingdom A multiresidue method for the analysis of 168 pesticides in dried powdered ginseng has been developed using acetonitrile or acetone mixture (acetone/cyclohexane/ethyl acetate, 2:1:1 v/v/v) extraction, solid-phase extraction (SPE) cleanup with octyl-bonded silica (C 8 ), graphitized carbon black/primary-secondary amine (GCB/PSA) sorbents and toluene, and capillary gas chromatogra- phy-mass spectrometry/selective ion monitoring (GC-MS/SIM) or -tandem mass spectrometry (GC- MS/MS). The geometric mean limits of quantitation (LOQs) were 53 and 6 μg/kg for the acetonitrile extraction and 48 and 7 μg/kg for the acetone-based extraction for GC-MS/SIM and GC-MS/MS, respectively. Mean percent recoveries and standard deviations from the ginseng fortified at 25, 100, and 500 μg/kg using GC-MS/SIM were 87 ( 10, 88 ( 8, and 86 ( 10% from acetonitrile extracts and 88 ( 13, 88 ( 12, and 88 ( 14% from acetone mixture extracts, respectively. The mean percent recoveries from the ginseng at the 25, 100, and 500 μg/kg levels using GC-MS/MS were 83 ( 19, 90 ( 13, and 89 ( 11% from acetonitrile extracts and 98 ( 20, 91 ( 13, and 88 ( 14% from acetone extracts, respectively. Twelve dried ginseng products were found to contain one or more of the following pesticides and their metabolites: BHCs (benzene hexachlorides, R-, β-, γ-, and δ-), chlorothalonil, chlorpyrifos, DDT (dichlorodiphenyl trichloroethane), dacthal, diazinon, iprodione, quin- tozene, and procymidone ranging from <1 to >4000 μg/kg. No significant differences were found between the two extraction solvents, and GC-MS/MS was found to be more specific and sensitive than GC-MS/SIM. The procedures described were shown to be effective in screening, identifying, confirm- ing, and quantitating pesticides in commercial ginseng products. KEYWORDS: Multiresidue methods; organohalogen pesticides; GC-MS/SIM; GC-MS/MS; acetonitrile; acetone/cyclohexane/ethyl acetate; ginseng INTRODUCTION Panax quinquefolius and Panax ginseng commonly known as American and Asian ginseng, respectively, are botanical dietary supplements widely used for health purposes. Due to its potential health benefits, ginseng root is widely regarded as a valuable agricultural crop, and to prevent economic losses, pesticides may be used against pests such as mold and insects that may damage the plants and the highly valued roots. Despite the usefulness of pesticides in agricultural practices, there are concerns about their excessive use, presence, and levels in plant commodities. Ginseng roots can accumulate pesticides during the growing stage or postharvest treatment, and previous studies have shown that many organochlorine and organophosphorus pesticides have been detected in dried ginseng root products ( 1 -8 ). Therefore, the presence of pesticides in ginseng root and other botanical products requires validated analytical procedures for effective † Part of the Florida Pesticide Residue Workshop 2009. *Author to whom correspondence should be addressed [telephone (301) 436-2172; fax (301) 436-2332; e-mail jon.wong@fda.hhs.gov].