PMID- 23534560
OWN - NLM
STAT- MEDLINE
DCOM- 20131205
LR  - 20130628
IS  - 1520-6882 (Electronic)
IS  - 0003-2700 (Linking)
VI  - 85
IP  - 9
DP  - 2013 May 7
TI  - Multiresidue pesticide analysis of botanical dietary supplements using salt-out 
      acetonitrile extraction, solid-phase extraction cleanup column, and gas 
      chromatography-triple quadrupole mass spectrometry.
PG  - 4686-93
LID - 10.1021/ac400481w [doi]
AB  - Dietary supplements form an increasing part of the American diet, yet broadly 
      applicable multiresidue pesticide methods have not been evaluated for many of 
      these supplements. A method for the analysis of 310 pesticides, isomers, and 
      pesticide metabolites in dried botanical dietary supplements has been developed 
      and validated. Sample preparation involved acetonitrile:water added to the 
      botanical along with anhydrous magnesium sulfate and sodium chloride for 
      extraction, followed by cleanup with solid-phase extraction using a tandem 
      cartridge consisting of graphitized carbon black (GCB) and primary-secondary 
      amine sorbent (PSA). Pesticides were measured by gas chromatography-tandem mass 
      spectrometry. Accuracy and precision were evaluated through fortifications of 24 
      botanicals at 10, 25, 100, and 500 mug/kg. Mean pesticide recoveries and relative 
      standard deviations (RSDs) for all botanicals were 97%, 91%, 90%, and 90% and 
      15%, 10%, 8%, and 6% at 10, 25, 100, and 500 mug/kg, respectively. The method was 
      applied to 21 incurred botanicals. Quinoxyfen was measured in hops (100-620 
      mug/kg). Tetraconazole (48 mug/kg), tetramethrin (15 mug/kg), methamidophos (50 
      mug/kg), and chlorpyrifos (93 mug/kg) were measured in licorice, mallow, tea, and 
      tribulus, respectively. Quintozene, its metabolites and contaminants 
      (pentachloroaniline, pentachlorobenzene, pentachloroanisole, and 
      pentachlorothioanisole and hexachlorobenzene and tecnazene, respectively), with 
      hexachlorocyclohexanes and DDT were identified in ginseng sources along with 
      azoxystrobin, diazinon, and dimethomorph between 0.7 and 2800 mug/kg. Validation 
      with these botanicals demonstrated the extent of this method's applicability for 
      screening 310 pesticides in a wide array of botanical dietary supplements.
FAU - Hayward, Douglas G
AU  - Hayward DG
AD  - US Food and Drug Administration, Center for Food Safety and Applied Nutrition, 
      College Park, Maryland 20740-3835, United States. douglas.hayward@fda.hhs.gov
FAU - Wong, Jon W
AU  - Wong JW
FAU - Shi, Feng
AU  - Shi F
FAU - Zhang, Kai
AU  - Zhang K
FAU - Lee, Nathaniel S
AU  - Lee NS
FAU - DiBenedetto, Alex L
AU  - DiBenedetto AL
FAU - Hengel, Mathew J
AU  - Hengel MJ
LA  - eng
PT  - Journal Article
PT  - Research Support, N.I.H., Extramural
DEP - 20130415
PL  - United States
TA  - Anal Chem
JT  - Analytical chemistry
JID - 0370536
RN  - 0 (Acetonitriles)
RN  - 0 (Pesticide Residues)
RN  - Z072SB282N (acetonitrile)
SB  - IM
MH  - Acetonitriles/*isolation & purification
MH  - Dietary Supplements/*analysis
MH  - Gas Chromatography-Mass Spectrometry
MH  - Molecular Structure
MH  - Pesticide Residues/*analysis
MH  - *Solid Phase Extraction
EDAT- 2013/03/29 06:00
MHDA- 2013/12/16 06:00
CRDT- 2013/03/29 06:00
PHST- 2013/03/29 06:00 [entrez]
PHST- 2013/03/29 06:00 [pubmed]
PHST- 2013/12/16 06:00 [medline]
AID - 10.1021/ac400481w [doi]
PST - ppublish
SO  - Anal Chem. 2013 May 7;85(9):4686-93. doi: 10.1021/ac400481w. Epub 2013 Apr 15.