超高效液相色谱-串联质谱测定饲料中镇静剂类和β-受体激素类药物残留  

Determination of sedative and β-receptor hormone residues in feed by ultra high performance liquid chromatography-tandem mass spectrometry

作　　者：孙珊珊[1] 朱丽君[1] 胡延喜[1] 刘玉峰[1,2] 徐亮 

机构地区：[1]辽宁大学药学院,辽宁沈阳110036 [2]辽宁省天然产物制药工程技术研究中心,辽宁沈阳110036

出　　处：《色谱》2018年第2期150-158,共9页Chinese Journal of Chromatography

基　　金：国家自然科学基金青年科学基金项目(81403177);沈阳市科技局应用基础项目(F12-277-1-14)~~

摘　　要：采用超高效液相色谱-串联质谱技术,建立了饲料中8种镇静剂类和15种β-受体激素类药物残留的分析检测方法。样品采用乙腈-1%(体积分数)三氯乙酸水溶液(7∶3,v/v)提取,目标物通过阳离子固相萃取柱净化,经Agilent Zorbax Eclipse Plus C_(18)色谱柱(100 mm×3.0 mm,1.8μm)分离,液相色谱-串联质谱进行检测,标准曲线内标法定量。结果表明:23种目标物在2.0~200.0μg/L内线性关系良好(r2>0.99)。在饲料样品基质中,目标化合物在5.0、10、50μg/kg 3个加标水平下的平均回收率为75.1%~102.4%,相对标准偏差(RSD)为4.3%~14.3%(n=6)。该方法净化效率高,适用范围广,可用于饲料中镇静剂类和β-受体激素类药物残留筛查和检测。An analysis and detection method for eight sedatives and fifteen ^ S-receptor hor-mones in feed was established by ultra high performance liquid chromatography-tandem mass spectrometry （UHPLC-MS/MS）. The sample was extracted with acetonitrile-1% （v/v ） trichlo-roacetic acid aqueous solution （ 7：3, v/v）T and purified by cationic solid phase extraction col-umn. The extracts were separated on an Agilent Zorbax Eclipse Plus C,8 chromatographic col-umn （100 mmx3. 0 mm,1. 8 pm） and then quantified via internal standard method. The results showed that the linear relationships of the 23 targets were good in the range of 2. 0-200. 0 pg^L （r2〉 0.99）. The average recoveries of the targets spiked in the matrix of feed samples were within 75. 1%-102. 4% in three spiked levels of 5. 0,10,50 pg/kg,and the relative standard deviations （RSDs） were within 4. 3% -14. 3% （n = 6）. This method with high purification effi-ciency and extensive scope of application can be applied to screening and detecting sedatives and S-receptor hormones in feed.

关 键 词：阳离子固相萃取小柱 超高效液相色谱-串联质谱 镇静剂类和洚受体激素 饲料 

分 类 号：O658[理学—分析化学]