Citation: 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. doi: 10.3724/SP.J.1123.2018.12026 shu

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

1.
Lianyungang Customs, Lianyungang 222042, China;
2.
Technology Center of Hainan Entry-Exit Inspection and Quarantine Bureau, Haikou 570311, China

Received Date: 17 December 2018

Fund Project: Science and Technology Plan Project of Nanjing Customs (No. 2017KJ12)

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.
- high-performance liquid chromatography (HPLC),
- triple quadrupole mass spectrometry (MS/MS),
- pesticide residues,
- shellfish
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1.
沈阳化工大学材料科学与工程学院沈阳 110142