Determination of 22 pesticide residues in shellfish by high performance liquid chromatography-tandem mass spectrometry

doi:10.3724/SP.J.1123.2018.12026

Abstract

Abstract:

A method for the simultaneous determination of 22 pesticide residues in shellfish by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was developed. The pesticides in the samples were extracted with 0.1% (v/v) formic acid in acetonitrile, cleaned up with primary secondary amine (PSA) and graphitized carbon black (GCB), and then separated on an ACE UltraCore 2.5 Super C18 column (100 mm×2.1 mm, 2.5 μm) by elution with a methanol-0.1% (v/v) formic acid solution at a flow rate of 0.4 mL/min. The analytes were detected by electrospray ionization in the positive ion mode and the multiple reaction monitoring mode. Good linear relationships were obtained, and the correlation coefficients (r²) of the 22 pesticides were all higher than 0.997. The limits of detection and limits of quantification were 0.1-0.3 μg/kg and 0.3-1.0 μg/kg, respectively. The mean recoveries varied from 65.2% to 109.4% at three spiked levels, and the relative standard deviations ranged from 1.3% to 15.2% (n=6). The proposed method is simple, accurate, and sensitive, and is effective for the simultaneous determination of 22 pesticide residues detected in shellfish.

Key words: high-performance liquid chromatography (HPLC), pesticide residues, shellfish, triple quadrupole mass spectrometry (MS/MS)

CLC Number:

O658

FAN Guangyu, TANG Xiu, ZHANG Yunqing, MENG Xianglong, LIANG Zhengang. Determination of 22 pesticide residues in shellfish by high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2019, 37(6): 612-618.

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