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

doi:10.3724/SP.J.1123.2017.10025

色谱 ›› 2018, Vol. 36 ›› Issue (2): 150-158.DOI: 10.3724/SP.J.1123.2017.10025

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

孙珊珊¹, 朱丽君¹, 胡延喜¹, 刘玉峰^1,2, 徐亮^1,2

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

收稿日期:2017-10-25 出版日期:2018-02-08 发布日期:2014-01-17
通讯作者: 刘玉峰,E-mail:liuyufeng@bjmu.edu.cn;徐亮,E-mail:13066647080@163.com
基金资助:
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）.

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

SUN Shanshan¹, ZHU Lijun¹, HU Yanxi¹, LIU Yufeng^1,2, XU Liang^1,2

1. College of Pharmacy, Liaoning University, Shenyang 110036, China;
2. Natural Products Pharmaceutical Engineering Technology Research Center of Liaoning Province, Shenyang 110036, China

Received:2017-10-25 Online:2018-02-08 Published:2014-01-17
Supported by:
National Natural Science Foundation of Youth Science Foundation, China (No.81403177);Basic Research for Applications of Shenyang Science and Technology Bureau, China (No.F12-277-1-14).

摘要/Abstract

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 C₁₈色谱柱（100 mm×3.0 mm，1.8 μm）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2.0~200.0 μg/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、50 μg/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: 超高效液相色谱-串联质谱, -受体激素, 饲料, 阳离子固相萃取小柱, 镇静剂类和&beta

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.

Key words: cationic solid phase extraction column, feed, sedative and β-receptor hormone, ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS)

中图分类号:

O658

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.

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.

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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

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

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