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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
引用本文:孙珊珊,朱丽君,胡延喜,刘玉峰,徐亮.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[J].色谱,2018,36(2):150-158.
作者姓名:孙珊珊  朱丽君  胡延喜  刘玉峰  徐亮
作者单位: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
基金项目:国家自然科学基金青-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(r20.99)。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。

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β-受体激素  饲料
收稿时间:2017-10-25

Determination of sedative and β-receptor hormone residues in feed by ultra high performance liquid chromatography-tandem mass spectrometry
SUN Shanshan,ZHU Lijun,HU Yanxi,LIU Yufeng,XU Liang.Determination of sedative and β-receptor hormone residues in feed by ultra high performance liquid chromatography-tandem mass spectrometry[J].Chinese Journal of Chromatography,2018,36(2):150-158.
Authors:SUN Shanshan  ZHU Lijun  HU Yanxi  LIU Yufeng  XU Liang
Institution:1. College of Pharmacy, Liaoning University, Shenyang 110036, China; 2. Natural Products Pharmaceutical Engineering Technology Research Center of Liaoning Province, Shenyang 110036, China
Abstract:An analysis and detection method for eight sedatives and fifteen β-receptor hormones 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) trichloroacetic acid aqueous solution (7:3, v/v), and purified by cationic solid phase extraction column. The extracts were separated on an Agilent Zorbax Eclipse Plus C18 chromatographic column (100 mm×3.0 mm, 1.8 μm) 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 μg/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 μg/kg, and the relative standard deviations (RSDs) were within 4.3%-14.3% (n=6). This method with high purification efficiency and extensive scope of application can be applied to screening and detecting sedatives and β -receptor hormones in feed.
Keywords:cationic solid phase extraction column  ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS)  sedative and β-receptor hormone  feed
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