Citation: YIN Peng, GUO Gui-Yi, DAI Jin-Xia, ZHU Li, GAO Guan-Wei, CHEN Hong-Ping, LIU Xin. Determination of Chlorpyrifos and Its Main Metabolite in Tea by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, ;2019, 47(2): 306-314. doi: 10.19756/j.issn.0253-3820.171266 shu

Determination of Chlorpyrifos and Its Main Metabolite in Tea by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry

YIN Peng ^1,2, ,
GUO Gui-Yi ¹ ,
DAI Jin-Xia ^2,3 ,
ZHU Li ^2,3 ,
GAO Guan-Wei ^2,3 ,
CHEN Hong-Ping ^2,3,4 ,
LIU Xin ^2,3,4

1.
Department of Tea Science, Xinyang Agriculture and Forestry University, Henan Key Laboratory of Tea Plant Comprehensive Utilization in South Henan, Xinyang 464000, China;
2.
Key Laboratory of Tea Quality and Safety Control, Ministry of Agriculture and Rural Affairs, Hangzhou 31008, China;
3.
Tea Research Institute, Chinese Academy of Agricultural Sciences, Hangzhou 31008, China;
4.
Tea Quality and Safety and Risk Assessment, Ministry of Agriculture and Rural Affairs, Hangzhou 31008, China

Received Date: 24 September 2017
Revised Date: 5 December 2018

Fund Project: This work was supported by the Open Fund of Key Laboratory of Tea Quality and Safety, Ministry of Agriculture and Rural Affairs (No.TRI20180101), the Science & Technology Project of Henan Province (No.182102110225), the National Tea Industry Technology System Foundation of China (CARS-23) and the Earmarked Fund for Innovative Research Team in Chinese Academy of Agricultural Sciences (CAAS-ASTIP-2014-TRICAAS).

A sensitive method was developed for simultaneous determination of chlorpyrifos (CPF) and its main metabolite 3,5,6-trichloro-2-pyridinol (TCP) in tea samples by QuEChERS and ultra-high performance liquid chromatography coupled with tandem mass spectrometry. Tea samples were extracted with acidic acetonitrile (containing 5% acetic acid), and cleaned up by the mixture of adsorbents containing 100 mg of graphitized carbon black (GCB) and 200 mg of C₁₈. The extracts were diluted with deionized water equally in volume prior to instrumental analysis. Scheduled multiple reaction monitoring in positive ion mode was applied to detection of chlorpyrifos and selected ion recording in negative mode was applied to detection of TCP. The matrix-matched internal standard method was used for quantification. The results showed that the method provided linear ranges from 0.4 to 400 μg/kg and 0.4 to 80 μg/kg for CPF and TCP respectively with the correlation coefficients of larger than 0.99. The limits of detection (S/N=3) were 0.06 μg/kg for CPF and 0.04-0.08 μg/kg for TCP, while the limits of quantification (S/N=10) were 0.20 μg/kg for CPF and 0.14-0.26 μg/kg for TCP. The recoveries were ranged from 93.9% to 111.4% for CPF and 92.4% to 118.4% for TCP respectively with the relative standard deviations (RSD, n=6) of 3.2%-11.1%. This method was sensitive, rapid, simple and had good reproducibility, indicating that it was suitable for simultaneous determination of CPF and TCP in tea samples.
- Tea,
- Chlorpyrifos,
- 3,5,6-Trichloro-2-pyridinol,
- Ultra-high performance liquid chromatography coupled with tandem mass spectrometry
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