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Citation: SONG Ning-Hui, XU Huai-Zhou, JI Gui-Xiang, ZHANG Sheng-Hu, ZHANG Qin, GUO Min, SHI Li-Li. Identification and Quantification of Chlorpyrifos Metabolites in Urine Samples by Ultra Performance Liquid Chromatography-Triple Quadrupole-Linear Ion Trap Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, ;2018, 46(5): 796-802. doi: 10.11895/j.issn.0253-3820.171282 shu

Identification and Quantification of Chlorpyrifos Metabolites in Urine Samples by Ultra Performance Liquid Chromatography-Triple Quadrupole-Linear Ion Trap Mass Spectrometry

Nanjing Institute of Environmental Sciences, Nanjing 210042, China

Received Date: 30 September 2017
Revised Date: 13 February 2018

Fund Project: This work was supported by the National Natural Science Foundation of China (No.41101307) and the Central Public Scientific Research Institutions Basal Research Fund Special Funds (No.20160210).

A method was established for the determination of chlorpyrifos metabolites employing QuEChERS method and ultra performance liquid chromatography-triple quadrupole-linear ion trap mass spectrometry (UPLC-QTRAP). The urine samples were extracted by acetonitrile and then cleaned up with PSA and GCB. The samples were separated with the gradient elution of acetonitrile-0.2% ammonia water on ZORBAX Eclipse Plus C₁₈ column. The analytes were detected by tandem mass spectrometry under negative ion mode with electrospray ionization (ESI) source and MRM-IDA-EPI mode. Under the optimized conditions, the calibration curve was linear in range of 1.0-100.0 μg/L, and the limits of detection were 0.10-0.73 μg/L. The average recoveries were 80.3%-90.1%, and RSDs were all within 10%. The developed method was simple, sensitive, accurate, and repeatable, and could avoid false positive result of samples effectively. The established method was successfully applied to determine the exposure level of chlorpyrifos metabolites in real samples of human health risk analysis. The results showed that the maximum concentration of chlorpyrifos metabolites was 54.6 μg/L. This method provided technic support for simultaneous identification and quantification of chemicals in complex matrix.
- Chlorpyrifos,
- Metabolite,
- Ultra performance liquid chromatograph-triple quadrupole-linear ion trap mass spectrometry,
- Urine
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