QuEChERS/HPLC-MS/MS法测定渔用饲料及饵料中地西泮及其代谢物  

QuEChERS/HPLC-MS/MS method for determination of diazepam and its metabolites in fish feed and bait

作　　者：万译文 李小玲[2] 索纹纹[1] 雷琴 杨霄 WAN Yi-wen;LI Xiao-ling;SUO Wen-wen;LEI Qin;YANG Xiao

机构地区：[1]农业农村部渔业产品质量检验测试中心(长沙),湖南长沙410153 [2]湖南省水产科学研究所,湖南长沙410153

出　　处：《饲料研究》2024年第13期124-129,共6页Feed Research

基　　金：湖南省科技重大研发计划项目(项目编号:2023NK4168);湖南省地方标准制定项目(项目编号:2023-94)。

摘　　要：研究建立了一种同时测定渔用饲料及饵料中地西泮及其代谢物的分散型固相萃取(QuEChERS)/高效液相色谱-串联质谱(HPLC-MS/MS)的方法。样品采用乙酸乙酯提取,提取液经50 mg C18和PSA分散固相萃取净化,40℃下氮吹浓缩近干,加入80%乙腈1.0 mL复溶,过滤后采用HPLC-MS/MS法进行测定。目标物采用飞诺美Kinetex C18系列色谱柱(100 mm×2.1 mm,2.6μm)分离,以0.1%体积比甲酸水溶液和乙腈为流动相梯度洗脱。电喷雾离子源(ESI+)、选择反应监测(SRM)模式下进行测定,基质匹配内标法定性定量。结果显示,该方法在0.5~50.0μg/kg范围内线性关系良好,相关系数均大于0.999,检出限和定量下限分别为0.5μg/kg和1.0μg/kg。在3个不同的添加水平下,地西泮及其代谢物的平均回收率为82.3%~109.4%,相对标准偏差为3.62%~6.33%。研究表明,该方法具有快速、准确度高与灵敏度高的优点,可满足渔用饲料及饵料中地西泮及其代谢物的残留检测需求。A study has established a method for the simultaneous determination of diazepam and its metabolites in fish feed and bait using dispersive solid-phase extraction(QuEChERS)coupled with high-performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).Samples were extracted with ethyl acetate,and the extract was purified with 50 mg of C18 and PSA solid-phase extraction.The extract was concentrated to near dryness under nitrogen at 40℃,reconstituted in 1.0 mL of 80%acetonitrile,filtered,and then analyzed using the HPLC-MS/MS method.The target compounds were separated using a Phenomenex Kinetex C18 series chromatographic column(100 mm×2.1 mm,2.6μm)with a gradient elution of 0.1%volume ratio aqueous formic acid and acetonitrile as the mobile phase.Detection was performed in electrospray ionization(ESI+)and selected reaction monitoring(SRM)mode,with a matrix-matched internal standard method for qualitative and quantitative analysis.The results showed that the method had a good linear relationship in the range of 0.5~50.0μg/kg,with correlation coefficients all greater than 0.999,and the limits of detection and quantification were 0.5μg/kg and 1.0μg/kg,respectively.At three different spiking levels,the average recovery rates for diazepam and its metabolites were 82.3%~109.4%,with relative standard deviations of 3.62%~6.33%.The study indicates that this method is rapid,accurate,and highly sensitive,capable of meeting the detection requirements for residues of diazepam and its metabolites in fish feed and bait.

关 键 词：HPLC-MS/MS QUECHERS 地西泮及其代谢物 渔用饲料 饵料 

分 类 号：S816.17[农业科学—饲料科学]