期刊
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
卷 406, 期 12, 页码 2899-2907出版社
SPRINGER HEIDELBERG
DOI: 10.1007/s00216-014-7717-8
关键词
Chlorpyrifos; 3,5,6-Trichloro-2-pyridinol; Derivatisation; QuEChERS; GC-MS/MS; Duck muscle
资金
- Zhejiang Provincial Science and Technology Project [2011C12024]
- International Cooperation Project of Ministry of Science and Technology [2013DFA31450]
- International Cooperation Project of Zhejiang Province [2013C24021]
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 A 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 mu g/kg) and TCP (from 1 to 1,000 mu g/kg) were equal to or higher than 0.998. The limits of detection (LODs) were 0.3 and 0.15 mu g/kg, and the limits of quantification (LOQs) were 1.0 and 0.5 mu g/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.
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