UPLC-TRIPLE QUAD-MS/MS法检测水产品中14种喹诺酮类药物残留研究  

Study on detection of 14 quinolone drug residues in aquatic products by UPLC-TRIPLE QUAD-MS/MS method

作　　者：张乐 顾娟娟 徐加兵[1,2] 杨海峰 秦枫[1] 孙晨欣[1] 熊良伟 ZHANG Le;GU Juan-juan;XU Jia-bing;YANG Hai-feng;QIN Feng;SUN Chen-xin;XIONG Liang-wei

机构地区：[1]江苏农牧科技职业学院,江苏省兽用生物制药高技术研究重点实验室,江苏泰州225300 [2]泰州市药品检验院,江苏泰州225300

出　　处：《饲料研究》2024年第24期129-135,共7页Feed Research

基　　金：江苏农牧科技职业技术学院科研课题(项目编号:NSF2022ZR13);江苏高校“青蓝工程”资助项目(项目编号:苏教师函[2022]29号、苏教师函数[2023]27号)。

摘　　要：试验旨在建立1种超高效液相色谱-三重四级杆串接质谱联用(UPLC-TRIPLE QUAD-MS/MS)技术快速分析水产品中14种喹诺酮类药物(QNs)多残留的方法。使用2%甲酸的乙腈溶液提取两次,QuEChERS法前处理,以甲醇-乙腈溶液和0.2%甲酸溶液为流动相,利用UPLC-TRIPLE QUAD-MS/MS进行检测。结果显示:试验建立的标准曲线相关系数为0.99744~0.99933,方法检出限为0.07~1.18μg/kg,定量限为0.25~3.94μg/kg;平均加标回收率为89.9%~109.4%,相对标准偏差为0.5%~4.5%。对水产品等14种样品进行了抽样筛查,昂刺鱼、鲫鱼和基围虾中检出喹诺酮类药物,鱼丸、虾丸、小龙虾中未检出。研究表明,UPLC-TRIPLE QUAD-MS/MS技术灵敏度高、回收率好、专属性强,适用检测水产品及其加工品中喹诺酮类药物。The experiment aimed to establish a method for the rapid analysis of multiple residues of 14 quinolone drugs(QNs)in aquatic products using ultra-performance liquid chromatography-tandem triple quadrupole mass spectrometry(UPLC-TRIPLE QUAD-MS/MS).The samples were extracted twice with an acetonitrile solution containing 2%formic acid,preprocessed using the QuEChERS method,and the mobile phase consisted of a mixture of methanol-acetonitrile solution and a 0.2%formic acid solution.Detection was carried out using UPLC-TRIPLE QUAD-MS/MS.The results showed that the correlation coefficients of the standard curves established by the experiment ranged from 0.99744 to 0.99933,the method detection limits were between 0.07 and 1.18μg/kg,and the quantification limits were between 0.25 and 3.94μg/kg.The average spiked recovery rate was between 89.9%and 109.4%,and the relative standard deviation was between 0.5%and 4.5%.In a sampling screening of 14 types of samples,quinolone drugs were detected in sharpsnout catfish,crucian carp,and river prawns,while no detection was found in fish balls,shrimp balls,and crayfish.The study indicates that the UPLC-TRIPLE QUAD-MS/MS technology has high sensitivity,good recovery rate,and strong specificity,making it suitable for detecting quinolone drugs in aquatic products and their processed goods.

关 键 词：喹诺酮类药物 超高效液相色谱-三重四级杆串接质谱联用 水产品 

分 类 号：S816.17[农业科学—饲料科学]