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中国药学(英文版) ›› 2015, Vol. 24 ›› Issue (10): 690-694.DOI: 10.5246/jcps.2015.10.089

• 【研究论文】 • 上一篇    下一篇

高效液相色谱-串联质谱法对猪肉中氯丙嗪的检测

张露, 黄雯, 蒋心惠*   

  1. 重庆医科大学 药学院, 重庆 400016
  • 收稿日期:2015-06-16 修回日期:2015-07-07 出版日期:2015-10-21 发布日期:2015-08-07
  • 通讯作者: Tel./Fax: 86-23-68485161, E-mail: Jiangxinhui3@hotmail.com
  • 基金资助:
    Chongqing Natural Science Foundation (Grant No. CSCT2013jcyjA10040).

Determination of chlorpromazine in porcine muscle using high performance liquid chromatography-tandem mass spectrometry

Lu Zhang, Wen Huang, Xinhui Jiang*   

  1. School of Pharmacy of Chongqing Medical University, Key Laboratory of Biochemistry and Molecular Pharmacology, Chongqing 400016, China
  • Received:2015-06-16 Revised:2015-07-07 Online:2015-10-21 Published:2015-08-07
  • Contact: Tel./Fax: 86-23-68485161, E-mail: Jiangxinhui3@hotmail.com
  • Supported by:
    Chongqing Natural Science Foundation (Grant No. CSCT2013jcyjA10040).

摘要:

建立了高效、准确的测定猪肉样品中氯丙嗪残留量的高效液相色谱-串联质谱法。碱化的样品混悬液由乙腈沉淀蛋白后再由特丁基甲醚萃取, 经冷冻离心分离15分钟后注入高效液相色谱-串联四极杆质谱仪进行分析。色谱柱为5 µm Agilent XDB-C18, 流动相由A-0.01 mol/L甲酸铵缓冲液(pH = 4)B-乙腈组成, 0.8 mL/min的流速进行梯度洗, 以电喷雾离子源正离子(ESI+)多反应监测模式(MRM)进行定量。氯丙嗪在0.4040–8.080 µg/kg范围内线性关系良好, 线性相关系数为0.999, 加标回收率在80.0%以上, 定量下限为0.052 µg/kg。该方法简便、快速、灵敏、专一, 适用于动物组织中的氯丙嗪研究。

关键词: 高效液相色谱-串联质谱, 氯丙嗪, 猪肉, 残留量

Abstract:

A rapid and accurate high performance liquid chromatography tandem mass spectrometry (HPLS-MS) method was established for quantification of chlorpromazine in pork. The porcine samples were pretreated with acetonitrile to precipitate proteins and followed by extraction with tert-butyl methyl ether (TBME). The separation was performed on a 5 µm Agilent XDB-C18 column with gradient elution. The mobile phase A was 0.01 mol/Lammonium formate in water and mobile phase B was acetonitrile. The flow rate was at 0.8 mL/min. Quantification was performed on a triple-quadrupole tandem mass spectrometer using the multiple selected reaction monitoring (MRM) mode. Transition of m/z +319.1 to 58.1 was used for the quantification of chlorpromazine. The method was validated at the concentration range of 0.4040 µg/kgto 8.080 µg/kg for chlorpromazine with correlation coefficient of 0.9999. The spiked recoveries were more than 80.0% and the limit of detection (LOD) was 0.052 µg/kg.The developed method, which offers advantages of convenience, rapid, specificity and higher sensitivity, can be used for determination of chlorpromazine hydrochloride in porcine muscles.

Key words: High performance liquid chromatography-tandem mass spectrometry, Chlorpromazine hydrochloride, Porcine muscle, Residual quantification

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