QuEChERS-超高效液相色谱串联质谱法同时检测水产品中11种四环素类药物  

Simultaneous Determination of 11 Tetracyclines Antibiotics in Aquatic Products by QuEChERS-Ultra High Performance Liquid Chromatography-Mass Spectrometry

作　　者：白俊露 曾军杰 何鹏飞 李佩佩[2] BAI Junlu;ZENG Junjie;HE Pengfei(School of Food and Pharmacy of Zhejiang Ocean University,Zhoushan 316022;Zhejiang Marine Fisheries Research Institute,Zhoushan 316021,China)

机构地区：[1]浙江海洋大学食品与药学学院,浙江舟山316022 [2]浙江省海洋水产研究所,浙江舟山316021

出　　处：《浙江海洋大学学报（自然科学版）》2024年第4期335-345,共11页Journal of Zhejiang Ocean University：Natural Science

基　　金：浙江省科技计划项目(LGC22B050032,LGN22C200018)。

摘　　要：以各类水产品作为研究对象,通过改进QuEChERS提取法的萃取和吸附条件,优化UPLC-MS/MS的各参数条件,建立了一种可以同时快速检测水产品中11种四环素类药物的检测方法。水产品样品采用冰乙酸-乙腈-水溶液(0.5:84:15.5,v/v/v)提取,新型去杂质吸附剂Bond Elut EMR-Lipid净化。分析物采用ACQUITY UPLC BEH C18色谱柱分离,0.1%甲酸水和乙腈作为流动相进行梯度洗脱,质谱电喷雾离子源多反应监测模式检测。结果表明:11种四环素类药物在各自的线性范围内线性关系良好(R^(2)>0.998),方法检出限(LOD,S/N=3)为0.21~1.70μg·kg^(-1),定量限(LOQ,S/N=10)为0.69~5.68μg·kg^(-1),在LOQ加标水平下响应良好,在5倍和10倍LOQ加标水平下平均回收率为72.54%~93.59%,RSD为2.11%~8.34%,最后将方法应用于实际样品检测中。方法具有简便快捷、选择性好、定性准确,重复性好等特点,适用于水产品中11种四环素类药物残留的准确快速检测。In this study,an analytical method using ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)coupled with QuEChERS(quick,easy,cheap,effective,rugged,and safe)procedure for sample preparation was developed to determine 11 tetracycline residues in aquatic products,by improving the extraction and adsorption conditions of QuEChERS and the optimizing the parameters of UPLC-MS/MS.The aquatic samples were extracted by glacial acetic acid-acetonitrile-aqueous solution(0.5:84:15.5 v/v/v),adsorbed and purified by a new type of decontamination adsorbent Bond Elut EMR-Lipid.The target analytes were separated on an ACQUITY UPLC BEH C18 column with gradient elution using a mobile phase containing acetonitrile and 0.1%(v/v)formic acid aqueous solution.Mass spectrometry was performed using an electrospray ionization source in the multiple reaction monitoring(MRM)mode.The results showed that the linearities of 11 tetracyclines were good with all correlation coefficients(R^(2))>0.998.The limits of detection(LOD,S/N=3)and limits of quantitation(LOQ,S/N=10)were in the range of 0.21-1.70μg·kg^(-1)and 0.69-5.68μg·kg^(-1),respectively.The average recoveries were 72.54%-93.59%at the spiked levels of two-fold and five-fold LOQ with relative standard deviation(RSDs)of 2.11%-8.34%.This method has the advantages of simple,fast,selective,accurate and repeatable,and can be applied to the simultaneous detection of 11 tetracycline residues in aquatic products.

关 键 词：水产品 QUECHERS 超高效液相色谱串联质谱法 四环素类 

分 类 号：O657.63[理学—分析化学] S859.84[理学—化学]