液相色谱-串联质谱法同时测定饲料中6种镇静剂的含量  

Simultaneous Determination of Six Sedatives in Feed by Liquid Chromatography-Tandem Mass Spectrom

作　　者：王威利 林雪贤 刘振妮 林奕云 崔泽锋 丁晨红 万凯 WANG Wei-li;LIN Xue-xian;LIU Zhen-ni;LIN Yi-yun;CUI Ze-feng;DING Chen-hong;WAN Kai(Institute of Quality Standard and Monitoring Technology for Agro-products of Guangdong Academy of Agricultural Sciences,Guangzhou 510640,China;Key Laboratory of Testing and Evaluation for Agro-products Safety and Quality,Ministry of Agriculture and Rural Affairs,Guangzhou 510640,China;Guangdong Provincial Key Laboratory of Quality&Safety Risk Assessment for Agro-products,Guangzhou 510640,China;Guangdong Agricultural Monitoring Technology Co.,Ltd.,Guangzhou 510640,China)

机构地区：[1]广东省农业科学院农业质量标准与监测技术研究所,广东广州510640 [2]农业农村部农产品质量安全检测与评价重点实验室,广东广州510640 [3]广东省农产品质量安全风险评估重点实验室,广东广州510640 [4]广东农科监测科技有限公司,广东广州510640

出　　处：《分析测试学报》2025年第4期652-659,共8页Journal of Instrumental Analysis

基　　金：2022年质标所团队启动项目(DWJJ-202202);农兽药残留风险评估实验室建设(DWJJ-202304);国家标准制修订项目(20232779-T-469);江门市科技特派员科研项目(2023760100490008106)。

摘　　要：建立了一种利用混合型阳离子交换固相萃取净化结合液相色谱-串联质谱(LC-MS/MS)测定饲料中安眠酮、地西泮、奋乃静、盐酸硫利达嗪、盐酸氯丙嗪和盐酸异丙嗪的方法。试样(配合饲料、浓缩饲料、添加剂预混合饲料和精料补充料)经0.5 mol/L盐酸溶液-乙腈(体积比1∶9)提取,采用混合型阳离子交换固相萃取柱净化,LC-MS/MS测定。目标物采用C18色谱柱(100 mm×2.1 mm,2.6μm)分离,以乙腈和0.1%甲酸水溶液进行洗脱,采用电喷雾离子源(ESI)正离子多反应监测(MRM)模式检测,外标法定量。不同饲料基质标准溶液中,6种镇静剂在0.2~50μg/L质量浓度范围内线性关系良好,相关系数(r^(2))均大于0.98,检出限为0.05 mg/kg,定量下限为0.1 mg/kg。饲料中6种镇静剂在0.1、1.0、100 mg/kg加标水平下的回收率为73.2%~104%,相对标准偏差(RSD)为1.0%~11%。该方法灵敏度高,准确度及重现性好,能够满足饲料中6种镇静剂的检测要求。A simultaneous determination method was established of methaqualone,diazepam,perphenazine,thioridazine hydrochloride,chlorpromazine hydrochloride and promethazine hydrochlorine in feeds using mixed cation exchange solid-phase extraction(SPE)by liquid chromatography tandem mass spectrometry(LC-MS/MS).The samples(compound feed,concentrated feed,additive premixed feed and concentrate supplement)were extracted with 0.5 mol/L hydrochloric acid solutionacetonitrile(1∶9),purified by a mixed cation exchange SPE column and then injected into LC-MS/MS.The chromatographic separation of six sedatives were conducted on a C18 chromatographic column(100 mm×2.1 mm,2.6μm)utilizing acetonitrile and 0.1%formic acid aqueous solution as mobile phases.Six sedatives were detected by using positive-ion electrospray tandem mass spectrometry via multiple reaction monitoring(MRM)scan mode,and the samples were quantified by external standard method.The results indicated that the calibration curves of six sedatives in different feed matrix showed good linear relationships in the concentration of 0.2-50μg/L with correlation coefficients(r^(2))all above 0.98.The limit of detection was 0.05 mg/kg and the limit of quantitation was 0.1 mg/kg.The recoveries of six sedatives in feed ranged from 73.2%to 104%at the spiked levels of 0.1,1.0,100 mg/kg,with relative standard deviations(RSDs)of 1.0%to 11%.The method was sensitive,accurate and suitable for the simultaneous determination of six sedatives in feeds.

关 键 词：液相色谱-串联质谱法 镇静剂 饲料 固相萃取 

分 类 号：O657.7[理学—分析化学] S816.17[理学—化学]