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

作　　者：李云萱 王璐璐 陈颖 施元旭 张水锋 LI Yun-Xuan;WANG Lu-Lu;CHEN Ying;SHI Yuan-Xu;ZHANG Shui-Feng(Zhejiang Fangyuan Test Group Co.,Ltd.,Hangzhou 310018,China)

机构地区：[1]浙江方圆检测集团股份有限公司,杭州310018

出　　处：《食品安全质量检测学报》2025年第5期207-214,共8页Journal of Food Safety and Quality

基　　金：浙江方圆检测集团股份有限公司科技项目(ZL202301)。

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1.0~50.0μg/L范围内线性关系良好,相关系数(r^(2))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0.5μg/kg,定量限为2.0μg/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。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 1.0–50.0μg/L,with correlation coefficients(r^(2))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 0.5μg/kg,and the limit of quantification of the method was 2.0μg/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.

关 键 词：淡水鱼 淡水虾 苯并咪唑类药物 超高效液相色谱-串联质谱法 

分 类 号：O657.63[理学—分析化学] TS254.7[理学—化学]