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| Simultaneous Determination of 105 Residues of Pesticides and Veterinary Drugs in Sea Cucumber by Filtered Solid Phase Extraction-UPLC-MS/MS |
| XU Bingwen, SUN Chengpeng, GE Xiangwu, WANG Jiaojuan |
| Technology Innovation Center of Rapid Screening and Traceability for Edible Agricultural Product Safety, State Administration for Market Regulation, Dalian Center for Certification and Food and Drug Control, Dalian 116037, China |
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Abstract An ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was established for the simultaneous determination of 53 pesticides and 52 veterinary drugs residues in sea cucumber Apostichopus japonicus. The samples were extracted with 80% acetonitrile water solution containing 0.5% formic acid (by volume). After centrifugation, the extraction was purification by PRiME HLB cartridge, and then the cartridge was eluted by acetonitrile containing 0.5% formic acid. A Waters Acquity UPLC BEH C18 column was selected as the separation column, the detection was conducted in positive ion mode (ESI+) and multiple reaction monitoring (MRM) scanning, and then quantified by external standard method using a matrix-matched standard. After optimizing, 97% compounds satisfied the detection requirements (60.0%—110.9%) at the LOQs. The limits of quantitation (LOQs) of 105 compounds were 1.0—50.0 μg/kg. The tested compounds showed great linearity at 0.2—50.0 μg/L with the correlation coefficients of higher than 0.99. The relative standard deviations were 0.3%—21.6% (n=6) with the samples spiked at LOQs, 2 LOQs and 10 LOQs. The finding indicates that the method above has high sensitivity and great recoveries and could be used for the determination of pesticides and veterinary drugs residues in sea cucumber.
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Received: 29 April 2024
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