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自动顶空固相微萃取和纤维上衍生化结合气相色谱-质谱联用测定肉制品中的克伦特罗

Automated headspace solid-phase microextraction and on-fiber derivatization for the determination of clenbuterol in meat products by gas chromatography coupled to mass spectrometry.

作者信息

Jiang Yong, Ni Yongnian

机构信息

School of Life Science, Jiangxi Science and Technology Normal University, Nanchang, P. R. China.

出版信息

J Sep Sci. 2015 Feb;38(3):418-25. doi: 10.1002/jssc.201400634. Epub 2014 Dec 23.

Abstract

A method was developed for the determination of clenbuterol in meat using stable-isotope-dilution gas chromatography with mass spectrometry coupled with solid-phase microextraction and on-fiber derivatization. The samples were first homogenized with hydrochloric acid followed by protein deposition. After headspace solid-phase microextraction and on-fiber derivatization, the content of clenbuterol was measured with the aid of stable-isotope dilution. The condition of solid-phase microextraction was optimized by central composite design. The relative standard deviations, limit of detection, and recoveries for clenbuterol were 4.2-9.2%, 0.48 μg/kg, and 96-104%, respectively. The proposed method was satisfactory for analysis of real samples as compared with the Chinese standard method.

摘要

建立了一种采用稳定同位素稀释气相色谱-质谱联用技术结合固相微萃取和纤维上衍生化测定肉类中克伦特罗的方法。样品先用盐酸匀浆,然后进行蛋白质沉淀。经过顶空固相微萃取和纤维上衍生化后,借助稳定同位素稀释法测定克伦特罗的含量。采用中心复合设计对固相微萃取条件进行了优化。克伦特罗的相对标准偏差、检测限和回收率分别为4.2-9.2%、0.48μg/kg和96-104%。与中国标准方法相比,该方法用于实际样品分析效果良好。

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