Chinese Journal of Chromatography ›› 2015, Vol. 33 ›› Issue (10): 1080-1089.DOI: 10.3724/SP.J.1123.2015.05015

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Rapid screening and confirmation of 205 pesticide residues in rice by QuEChERS and liquid chromatography-mass spectrometry

CHEN Xi1,2, CHENG Lei2, QU Shichao2, HUANG Daliang2, LIU Jiacheng2, CUI Han2, JIA Yanbo3, JI Mingshan1   

  1. 1. Plant Protection College, Shenyang Agricultural University, Shenyang 110866, China;
    2. Inspection and Quarantine Technical Center of Dalian Entry-Exit Inspection and Quarantine Bureau, Zhuanghe 116400, China;
    3. Shanghai AB SCIEX Analytical Instrument Trading Co., Ltd., Beijing 100015, China
  • Received:2015-05-13 Online:2015-10-08 Published:2012-05-09

Abstract:

A method for rapid screening and confirmation of 205 pesticide residues in rice was developed by combining QuEChERS and high performance liquid chromatography-triple quadrupole-linear ion trap mass spectrometry (LC-Q-TRAP/MS). The rice samples were extracted with acetonitrile, and then cleaned up with primary secondary amine (PSA), anhydrous magnesium sulfate (MgSO4) and C18 adsorbent. Finally, the samples were detected by LC-Q-TRAP/MS in multiple reaction monitoring with information-dependent acquisition of enhanced product ion (MRM-IDA-EPI) mode followed with database searching. A total of 205 pesticide residues were confirmed by retention times, ion pairs and the database searching using EPI library, and quantified by external standard method. All the pesticides showed good linearities with linear correlation coefficients all above 0.995. The limits of quantification (LOQs) for the 205 pesticides were 0.5-10.0 μg/kg. The average recoveries of the 205 pesticides ranged from 62.4% to 127.1% with the relative standard deviations (RSDs) of 1.0%-20.0% at spiked levels of 10 μg/kg and 50 μg/kg, and only 20 min were needed for the analysis of an actual rice sample. In brief, the method is fast, accurate and highly sensitive, and is suitable for the screening and confirmation of pesticide residues in rice.

Key words: confirmation, liquid chromatography-triple quadrupole-linear ion trap mass spectrometry (LC-Q-TRAP/MS), pesticide residues, QuEChERS, rice, screen

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