PMID- 24691719 OWN - NLM STAT- MEDLINE DCOM- 20150416 LR - 20191210 IS - 1618-2650 (Electronic) IS - 1618-2642 (Linking) VI - 406 IP - 12 DP - 2014 May TI - Simultaneous determination of chlorpyrifos and 3,5,6-trichloro-2-pyridinol in duck muscle by modified QuEChERS coupled to gas chromatography tandem mass spectrometry (GC-MS/MS). PG - 2899-907 LID - 10.1007/s00216-014-7717-8 [doi] AB - A rapid, specific, and sensitive method based on modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) coupled to gas chromatography tandem mass spectrometry (GC-MS/MS) was developed and validated for simultaneous determination of chlorpyrifos (CP) and its metabolite 3,5,6-trichloro-2-pyridinol (TCP) in duck muscle. The residues of CP and TCP were extracted by acidified acetonitrile. The fat layer of the extract was removed under -20 degrees C, then the organic layer was evaporated. The analytes were derivatized by N-(tert-butyldimethylsilyl)-N-methyltrifluoroacetamide (MTBSTFA) and cleaned up by a mixture of 150 mg MgSO4, 25 mg graphitized carbon black (GCB), and 50 mg N-propylethylenediamine (PSA) to remove interference. The final extract was analyzed by GC-MS/MS. Recovery values at the spiking concentrations ranged from 86.2 to 92.3 % for CP and from 74.8 to 81.8 % for TCP, with relative standard deviations (RSDs) lower than 9.5 and 12.3, respectively. The correlation coefficients of CP (from 2 to 2,000 mug/kg) and TCP (from 1 to 1,000 mug/kg) were equal to or higher than 0.998. The limits of detection (LODs) were 0.3 and 0.15 mug/kg, and the limits of quantification (LOQs) were 1.0 and 0.5 mug/kg for CP and TCP in duck muscle, respectively. The average intra- and inter-day accuracy ranged from 84.6 to 91.2 % for CP and 75.6 to 82.3 % for TCP, and the intra- and inter-day precisions were from 5.8 to 8.2 % for CP and 6.5 to 11.9 % for TCP. Furthermore, the CP and TCP residues in duck muscle samples were detected for dietary risk assessment using the validated method. FAU - Li, Rui AU - Li R AD - State Key Laboratory Breeding Base for Zhejiang Sustainable Plant Pest Control; Agricultural Ministry Key Laboratory for Pesticide Residue Detection; Zhejiang Province Key Laboratory for Food Safety; Institute of Quality and Standard for Agro-products, Zhejiang Academy of Agricultural Sciences, 310021, Hangzhou, Zhejiang, China. FAU - He, Liang AU - He L FAU - Zhou, Ting AU - Zhou T FAU - Ji, Xiaofeng AU - Ji X FAU - Qian, Mingrong AU - Qian M FAU - Zhou, Yu AU - Zhou Y FAU - Wang, Qiang AU - Wang Q LA - eng PT - Evaluation Study PT - Journal Article PT - Research Support, Non-U.S. Gov't DEP - 20140402 PL - Germany TA - Anal Bioanal Chem JT - Analytical and bioanalytical chemistry JID - 101134327 RN - 0 (Pesticides) RN - 0 (Pyridones) RN - 6515-38-4 (3,5,6-trichloro-2-pyridinol) RN - JCS58I644W (Chlorpyrifos) SB - IM MH - Animals MH - Chemical Fractionation/*methods MH - Chlorpyrifos/*analysis/isolation & purification MH - Ducks MH - Food Contamination/*analysis MH - Gas Chromatography-Mass Spectrometry/*methods MH - Meat/*analysis MH - Muscle, Skeletal/*chemistry MH - Pesticides/*analysis/isolation & purification MH - Pyridones/*analysis/isolation & purification MH - Tandem Mass Spectrometry/methods EDAT- 2014/04/03 06:00 MHDA- 2015/04/17 06:00 CRDT- 2014/04/03 06:00 PHST- 2013/11/03 00:00 [received] PHST- 2014/02/20 00:00 [accepted] PHST- 2014/02/18 00:00 [revised] PHST- 2014/04/03 06:00 [entrez] PHST- 2014/04/03 06:00 [pubmed] PHST- 2015/04/17 06:00 [medline] AID - 10.1007/s00216-014-7717-8 [doi] PST - ppublish SO - Anal Bioanal Chem. 2014 May;406(12):2899-907. doi: 10.1007/s00216-014-7717-8. Epub 2014 Apr 2.