PMID- 16912982
OWN - NLM
STAT- MEDLINE
DCOM- 20070830
LR  - 20191210
IS  - 0951-4198 (Print)
IS  - 0951-4198 (Linking)
VI  - 20
IP  - 18
DP  - 2006
TI  - Determination of chlorpyrifos and its metabolites in rat brain tissue using 
      coupled-column liquid chromatography/electrospray ionization tandem mass 
      spectrometry.
PG  - 2689-95
AB  - A method has been developed to quantify chlorpyrifos 
      (O,O-diethyl-O-[3,5,6,-trichloro-2-pyridyl] phosphorothionate) and its 
      metabolites chlorpyrifos-oxon (O,O-diethyl-O-[3,5,6,trichloro-2-pyridinyl] 
      phosphate) and TCP (3,5,6,-trichloro-2-pyridinol) in rat brain tissue by 
      coupled-column liquid chromatography/electrospray ionization tandem mass 
      spectrometry (LC/LC/ESI-MS/MS). Rat brains were homogenized and treated by 
      protein precipitation using ice-cold acetonitrile. The supernatant was directly 
      injected onto the coupled-column system. Sample clean-up was achieved on a Zorbax 
      Extend-C(18) column (2.1 x 50 mm, 5 microm) using a mobile phase of 
      acetonitrile/water with 0.0025% formic acid (40:60, v/v). The compounds were 
      separated isocratically on a Zorbax Eclipse XDB C(8) column (2.0 x 150 mm, 5 
      microm) using a mobile phase of acetonitrile/water with 0.0025% formic acid 
      (75:25, v/v). Chlorpyrifos and chlorpyrifos-oxon were detected in positive ion 
      mode using multiple reaction monitoring (MRM). TCP was detected in negative ion 
      mode using precursor-to-precursor transition monitoring. The method was validated 
      and the specificity, linearity, limit of quantitation (LOQ), precision, accuracy, 
      stability, and recoveries were determined. Calibration curves for all three 
      analytes yielded correlation coefficients of 0.993 or greater. The LOQs were 25.3 
      ng/g for chlorpyrifos and 6.3 ng/g for chlorpyrifos-oxon and TCP. All precision 
      relative standard deviations (RSDs) were less than 16% for the LOQ and less than 
      11% for the other QC samples. This method was successfully applied to six rats 
      that were injected subcutaneously with chlorpyrifos.
CI  - Copyright 2006 John Wiley & Sons, Ltd.
FAU - Williamson, Leah N
AU  - Williamson LN
AD  - Department of Pharmaceutical and Biomedical Sciences, College of Pharmacy, The 
      University of Georgia, Athens, GA 30602-2352, USA.
FAU - Terry, Alvin V Jr
AU  - Terry AV Jr
FAU - Bartlett, Michael G
AU  - Bartlett MG
LA  - eng
PT  - Journal Article
PT  - Validation Study
PL  - England
TA  - Rapid Commun Mass Spectrom
JT  - Rapid communications in mass spectrometry : RCM
JID - 8802365
RN  - 0 (Insecticides)
RN  - 0 (Pyridones)
RN  - 5598-15-2 (O,O-diethyl O-3,5,6-trichloro-2-pyridyl phosphate)
RN  - 6515-38-4 (3,5,6-trichloro-2-pyridinol)
RN  - JCS58I644W (Chlorpyrifos)
SB  - IM
MH  - Animals
MH  - Brain Chemistry
MH  - Chlorpyrifos/analogs & derivatives/*analysis
MH  - *Chromatography, High Pressure Liquid
MH  - Insecticides/*analysis
MH  - Pyridones/analysis
MH  - Rats
MH  - Reproducibility of Results
MH  - Sensitivity and Specificity
MH  - Spectrometry, Mass, Electrospray Ionization/instrumentation/*methods
MH  - Tandem Mass Spectrometry/instrumentation/*methods
EDAT- 2006/08/17 09:00
MHDA- 2007/08/31 09:00
CRDT- 2006/08/17 09:00
PHST- 2006/08/17 09:00 [pubmed]
PHST- 2007/08/31 09:00 [medline]
PHST- 2006/08/17 09:00 [entrez]
AID - 10.1002/rcm.2647 [doi]
PST - ppublish
SO  - Rapid Commun Mass Spectrom. 2006;20(18):2689-95. doi: 10.1002/rcm.2647.