超高效液相色谱-串联质谱法测定淡水鱼虾中11种苯并咪唑类药物残留

Determination of 11 kinds of residues of benzimidazole drugs in freshwater fish and shrimp by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  淡水鱼  淡水虾  11种苯并咪唑类药物  超高效液相色谱-串联质谱法

英文关键词:freshwater fish  freshwater shrimp  benzimidazole drugs  ultra performance liquid chromatography- tandem mass spectrometry

中文摘要:

      目的 建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)测定淡水鱼淡水虾中11种苯并咪唑类药物残留量的方法。方法 样品首先进行两次乙腈提取, 利用混合型强阳离子固相萃取柱对提取物进行净化, 接着通过Waters C18色谱柱分离, UPLC-MS/MS进行检测, 并采用内标法进行定量分析。结果 11种苯并咪唑类药物在1.0~50.0 g/L范围内线性关系良好, 相关系数(r2)均大于0.99。3个浓度的鱼肉空白样品加标回收率范围在78.4%~104.3%内, 其相对标准偏差在2.0%~8.8%之间; 3个浓度的虾肉空白样品加标回收率范围在73.3%~107.5%内, 其相对标准偏差在1.5%~8.7%之间。本方法检出限为0.5 g/kg, 定量限为2.0 g/kg。结论 该方法净化效果好, 重现性及回收率稳定, 适用于淡水鱼淡水虾中11种苯并咪唑类药物残留量的测定。

英文摘要:

      Objective To establish a method for the determination of 11 kinds of residues of benzimidazole drugs in freshwater fish and shrimp by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The samples were first extracted by acetonitrile twice, purified by mixed strong cationic solid phase extraction column, then separated by Waters C18 column, detected by UPLC-MS/MS, and the internal standard method was adopted for quantitative analysis. Results The 11 kinds of benzimidazole drugs showed good linear relationships at 1.0–50.0 μg/L, with correlation coefficients (r2) greater than 0.99. The ranges of spiked recovery rates for 3 concentrations of blank fish samples were between 78.4% and 104.3%, and the relative standard deviations of the recovery rates for 3 concentrations were between 2.0% and 8.8%; the recovery rates of 3 concentrations of shrimp meat blank samples ranged from 73.3% to 107.5%, with relative standard deviations between 1.5% and 8.7%. The limit of detection of the method in this study was 0.5 μg/kg, and the limit of quantification of the method was 2.0 μg/kg. Conclusion The method has good purification effect, stable reproducibility and recovery, and is suitable for the determination of 11 kinds of benzimidazole residues in freshwater fish and shrimp.