超高效液相色谱串联质谱法检测水产品中的地西泮残留  

Detection of Diazepam Residues in Aquatic Products by Ultra High Performance Liquid Chromatography Tandem Mass Spectrometry

作　　者：苏焕斌 王思琦 毛云枫 杨柱荣 丘东蔚 黄钟标 SU Huanbin;WANG Siqi;MAO Yunfeng;YANG Zhurong;QIU Dongwei;HUANG Zhongbiao(Guangdong Provincial Product Quality Supervision and Inspection Institute,Foshan 528300,China)

机构地区：[1]广东产品质量监督检验研究院,广东佛山528300

出　　处：《食品安全导刊》2024年第35期64-68,共5页China Food Safety Magazine

摘　　要：本文建立一种超高效液相色谱串联质谱法检测水产品中地西泮残留的方法。样品采用乙腈提取,经增强型脂质吸附去除剂EMR-Lipid和Cleanert LipoNo组合净化,采用正离子多反应监测模式扫描,内标法定量。结果表明,地西泮浓度在1~500 ng·L^(-1)线性关系良好,R^(2)=0.9992;方法的检出限为0.23μg·kg^(-1),定量限为0.43μg·kg^(-1);地西泮在鲈鱼、草鱼、鲢鱼及鲫鱼4种水产品中的基质效应在0.85~1.15,基质效应不明显;样品的平均回收率为87.3%~120.2%,相对标准偏差为3.27%~11.02%。该方法可以实现水产品中地西泮的快速定量检测,为水产品兽药残留的定量分析提供技术支持。An ultra-high performance liquid chromatography-tandem mass spectrometry method for the determination of diazepam residues in aquatic products was developed.The sample was extracted by acetonitrile,purified by a combination of enhanced lipid removal agent EMR-Lipid and Cleanert LipoNo,and quantified by internal standard method using positive ion multi-reaction monitoring mode.The results showed that the linear relationship was good when the concentration of diazepam was 1 ng·L^(-1) to 50 ng·L^(-1),R^(2)=0.9992;the limits of detection and quantification were 0.23μg·kg^(-1) and 0.43μg·kg^(-1),respectively;the matrix effect of diazepam on perch,grass carp,silver carp and crucian fish was 0.85 to 1.15,and the matrix effect was not obvious;the average recoveries of samples were 87.3%to 120.2%,and the relative standard deviations were 3.27%to 11.02%.The method can achieve rapid quantitative detection of diazepam in aquatic products,and provide technical support for quantitative analysis of veterinary drug residues in aquatic products.

关 键 词：水产品 地西泮 加标 定量 

分 类 号：O657.63[理学—分析化学] TS254.7[理学—化学]