Citation: LIU Yong, TANG Yingfei, SONG Jinfeng, HU Zhiwei. Determination of four organophosphorus pesticides and their metabolites in vegetables using solid-phase extraction coupled with liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, ;2014, 32(2): 139-144. doi: 10.3724/SP.J.1123.2013.10008 shu

Determination of four organophosphorus pesticides and their metabolites in vegetables using solid-phase extraction coupled with liquid chromatography-tandem mass spectrometry

LIU Yong ^1,2 ,
TANG Yingfei ^2,3 ,
SONG Jinfeng ^2,, ,
HU Zhiwei ²

1.
1. Technology Center of Heilongjiang Entry-Exit Inspection and Quarantine Bureau, Harbin 150001, China;

Corresponding author: SONG Jinfeng,
Received Date: 11 October 2013
Available Online: 18 December 2013
Fund Project: 国家质检总局课题(2009IK177). (2009IK177)

Organophosphorus pesticides (OPs), malathion, methyl parathion, trichlorfon, and acephate were used frequently in vegetable cultivation, mainly metabolized into O,O-dimethyl dithiophosphate, 4-nitrophenol, dimethyl dichloroviny phosphate (DDVP) and methamidophos, respectively. A method of liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed for the determination of the organophosphorus pesticides and their metabolites. According to the difference of coloring matter contents in vegetable matrix, the pre-treatment for vegetables with high coloring matter contents were performed using activated carbon coupled with a Florisil solid-phase extraction column, and others were purified by a Florisil solid-phase extraction column. A hydrophilic interaction chromatographic column (ACQUITY UPLC BEH HILIC) was used with acetonitrile-5 mmol/L ammonium acetate as mobile phases. The MS/MS detection was performed under positive or negative electrospray ionization (ESI) in multiple reaction monitoring (MRM) mode. The results showed that the matrix effect of the LC-MS/MS was 15.3%-45.1%, the recoveries of the four organophosphorus pesticides and their metabolites were 76.9%-102.8%, the precision ranged from 5.92% to 10.19%, the limits of quantification ranged from 0.001 to 0.01 mg/L, and the linear correlation coefficients were 0.9982-0.9999 in the range of 0.01-1.00 mg/L. This method was applied in the analysis of Chinese cabbages, hot peppers, tomatoes and onions from markets. This method can be applied in rapid detection of the organophosphorus pesticides and their metabolites in vegetables.
- solid-phase extraction (SPE),
- liquid chromatography-tandem mass spectrometry (LC-MS/MS),
- organophosphorus pesticides,
- metabolites,
- vegetables
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