Determination of Multiresidue Pesticides in Botanical Dietary Supplements Using Gas Chromatography-Triple-Quadrupole Mass Spectrometry (GC-MS/MS).
A simplified sample preparation method in combination with gas chromatography-triple-quadrupole mass spectrometry (GC-MS/MS) analysis was developed and validated for the simultaneous determination of 227 pesticides in green tea, ginseng, gingko leaves, saw palmetto, spearmint, and black pepper samples. The botanical samples were hydrated with water and extracted with acetonitrile, magnesium sulfate, and sodium chloride. The acetonitrile extract was cleaned up using solid phase extraction with carbon-coated alumina/primary-secondary amine with or without C18. Recovery studies using matrix blanks fortified with pesticides at concentrations of 10, 25, 100, and 500 μg/kg resulted in average recoveries of 70-99% and relative standard deviation of 5-13% for all tested botanicals except for black pepper, for which lower recoveries of fortified pesticides were observed. Matrix-matched standard calibration curves revealed good linearity (r(2) > 0.99) across a wide concentration range (1-1000 μg/L). Nine commercially available tea and 23 ginseng samples were analyzed using this method. Results revealed 36 pesticides were detected in the 9 tea samples at concentrations of 2-3500 μg/kg and 61 pesticides were detected in the 23 ginseng samples at concentrations of 1-12500 μg/kg.
Center for Food Safety and Applied Nutrition, U.S. Food and Drug Administration , 6502 South Archer Road, Bedford Park, Illinois 60501, United States.
Yang
Y
Chen
Institute for Food Safety and Health, Illinois Institute of Technology , 6502 South Archer Road, Bedford Park, Illinois 60501, United States.
Salvador
S
Lopez
Center for Food Safety and Applied Nutrition, U.S. Food and Drug Administration , 5100 Paint Branch Parkway, College Park, Maryland 20740-3835, United States.
Douglas G
DG
Hayward
Center for Food Safety and Applied Nutrition, U.S. Food and Drug Administration , 5100 Paint Branch Parkway, College Park, Maryland 20740-3835, United States.
Hoon Yong
HY
Park
Center for Food Safety and Applied Nutrition, U.S. Food and Drug Administration , 5100 Paint Branch Parkway, College Park, Maryland 20740-3835, United States.
Jon W
JW
Wong
Center for Food Safety and Applied Nutrition, U.S. Food and Drug Administration , 5100 Paint Branch Parkway, College Park, Maryland 20740-3835, United States.
Suyon S
SS
Kim
Institute for Food Safety and Health, Illinois Institute of Technology , 6502 South Archer Road, Bedford Park, Illinois 60501, United States.
Jason
J
Wan
Center for Food Safety and Applied Nutrition, U.S. Food and Drug Administration , 6502 South Archer Road, Bedford Park, Illinois 60501, United States.
Ravinder M
RM
Reddy
Thermo Fisher Scientific , 2215 Grand Avenue Parkway, Austin, Texas 78728, United States.
Daniel J
DJ
Quinn
Thermo Fisher Scientific , 2215 Grand Avenue Parkway, Austin, Texas 78728, United States.
David
D
Steiniger
D019587:Dietary Supplements / Q000032:analysis*; D004340:Drug Contamination; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D020441:Ginkgo biloba / Q000737:chemistry; D005894:Panax / Q000737:chemistry; D010573:Pesticide Residues / Q000032:analysis* / Q000302:isolation & purification; D029222:Piper nigrum / Q000737:chemistry; D010936:Plant Extracts / Q000737:chemistry; D028321:Plant Preparations / Q000032:analysis*; D028024:Serenoa; D052616:Solid Phase Extraction
D010573:Pesticide Residues; D010936:Plant Extracts; D028321:Plant Preparations; C040972:saw palmetto extract
Carbon X/PSA; Carbon X/PSA/C18 SPE; botanicals; dual-phase SPE; multipesticide residue; triple-phase SPE GC-MS/MS