Analysis of organophosphorus pesticides in dried ground ginseng root by capillary gas chromatography-mass spectrometry and -flame photometric detection.
A method was developed to determine organophosphorus pesticides (OPs) in dried ground ginseng root. Pesticides were extracted from the sample using acetonitrile/water saturated with salts, followed by solid-phase dispersive cleanup, and analyzed by capillary gas chromatography with electron ionization mass spectrometry in selective ion monitoring mode (GC-MS/SIM) and flame photometric detection (GC-FPD) in phosphorus mode. The detection limits for most of the pesticides were 0.025-0.05 microg/g using GC-FPD but were analyte-dependent for GC-MS/SIM, ranging from 0.005 to 0.50 microg/g. Quantitation was determined from 0.050 to 5.0 microg/g with r 2 > 0.99 for a majority of the pesticides using both detectors. Recovery studies were performed by fortifying the dried ground ginseng root samples to concentrations of 0.025, 0.1, and 1.0 microg/g, resulting in recoveries of >90% for most pesticides by GC-FPD. Lower (<70%) and higher (>120%) recoveries were most likely from complications of pesticide lability or volatility, matrix interference, or inefficient desorption from the solid-phase sorbents. There was difficulty in analyzing the ginseng samples for the OPs using GC-MS at the lower fortification levels for some of the OPs due to lack of confirmation. GC-FPD and GC-MS/SIM complement each other in detecting the OPs in dried ground ginseng root samples. This procedure was shown to be effective and was applied to the analysis of OPs in ginseng root samples. One particular sample, a ground and dried American ginseng (Panax quinquefolius) root sample, was found to contain diazinon quantified at approximately 25 microg/kg by external calibration using matrix-matched standards or standard addition using both detectors. The advantage of using both detectors is that confirmation can be achieved using GC-MS, whereas the use of a megabore column in GC-FPD can be used to quantitate some of the nonpolar OPs without the use of matrix-matched standards or standard addition.
Wong
Jon W
JW
Center for Food Safety and Applied Nutrition, Office of Plant and Dairy Foods, HFS-336, U.S. Food and Drug Administration, 5100 Paint Branch Parkway, College Park, MD 20740-3835, USA. jon.wong@fda.hhs.gov
Hennessy
Michael K
MK
Hayward
Douglas G
DG
Krynitsky
Alexander J
AJ
Cassias
Irene
I
Schenck
Frank J
FJ
D003890:Desiccation; D019587:Dietary Supplements; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D009943:Organophosphorus Compounds / Q000032:analysis*; D005894:Panax / Q000737:chemistry*; D010575:Pesticides / Q000032:analysis*; D010783:Photometry / Q000379:methods*; D010936:Plant Extracts / Q000737:chemistry; D018517:Plant Roots / Q000737:chemistry*
D009943:Organophosphorus Compounds; D010575:Pesticides; D010936:Plant Extracts