Citation: HUANG Meng-Ying, WANG Na, GUO Xin-Yan, QIU Pan-Zi, TANG Wei-Guo, ZHANG Zun-Jian. Simultaneous Determination of Four Organophosphate Pesticide Metabolites in Urine Using Solid Phase Extraction Coupled with Gas Chromatography-Tandem Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, ;2016, 44(5): 723-730. doi: 10.11895/j.issn.0253-3820.150932 shu

Simultaneous Determination of Four Organophosphate Pesticide Metabolites in Urine Using Solid Phase Extraction Coupled with Gas Chromatography-Tandem Mass Spectrometry

1.
Key Laboratory of Drug Quality Control and Pharmacovigilance, China Pharmaceutical University, Ministry of Education, Nanjing 210009, China;
2.
Nanjing Institute of Environmental Science, Ministry of Environmental Protection, Nanjing 210042, China;
3.
Jinling Pharmaceutical Co., Ltd, Nanjing 210009, China

Received Date: 21 November 2015
Revised Date: 27 January 2016

A method for quantifying four urinary metabolites of organophosphorus pesticides using gas chromatography-tandem mass spectrometry (GC-MS/MS) was developed. The metabolites were extracted and enriched from urine samples with WCX solid phase extraction (SPE) cartridges, followed by liquid-liquid extraction with ethyl acetate-acetonitrile (70:30, V/V). The analytes were chemically derivatized with N-tert-butyldimethylsilyl-N-methyltrifluoroacetamide after the derivatives were concentrated by drying and dissolved in phenylmethane. The separation was performed on a HP-5MS capillary column (30 m×0.25 mm×0.25 μm) with temperature programming and the detection was performed in multiple reaction monitoring (MRM) mode using GC-MS/MS. The internal standard method was used for quantification. The extraction solvents, types of SPE cartridges and eluents were optimized by comparing the sample recoveries under different conditions. The result showed that the calibration curves of four metabolites were linear in the range of 0.2-200 μg/L (R² ≥ 0.992). The limits of detection (LODs) and the limits of quantification (LOQs) of the four metabolites were 0.083-0.667 μg/L and 0.2-2.0 μg/L, respectively. The recoveries of four metabolites ranged from 54.1% to 68.6% (RSD<8.5%, n=6). The established method whichs avoid using large amount of organic solvents in liquid-liquid extraction is stable, reliable and efficient, and is suitable for the analysis of large amounts of samples. Therefore, the method can be applied to assess the exposure level of organophosphorus pesticide in general population.
- Solid phase extraction,
- Gas chromatography-tandem mass spectrometry,
- Organophosphorus pesticides metabolites,
- Urine
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1.
沈阳化工大学材料科学与工程学院沈阳 110142