色谱

色谱

• 研究论文 • 上一篇    下一篇

高效液相色谱-串联质谱法同时测定血液中的15种减肥药物

车宝泉1,2, 黄晓君2, 张喆2, 王志斌2, 邓玉林1*   

  1. 1. 北京理工大学生命学院, 北京 100081; 2. 北京市药品检验所, 北京 100035
  • 收稿日期:2011-04-12 修回日期:2011-06-28 出版日期:2011-08-28 发布日期:2011-09-28
  • 通讯作者: 邓玉林,博士,教授,研究方向为生命科学. Tel: (010)68915995
  • 基金资助:

    国家“十一五”科技支撑计划项目(No. 2009BAK59B01)

Simultaneous determination of 15 anti-obesity drugs in blood by high performance liquid chromatography-tandem mass spectrometry

CHE Baoquan1,2, HUANG Xiaojun2, ZHANG Zhe2, WANG Zhibin2, DENG Yulin1*   

  • Received:2011-04-12 Revised:2011-06-28 Online:2011-08-28 Published:2011-09-28

PDF

592

摘要： 建立了一种专属、灵敏的同时测定血液中咖啡因、盐酸西布曲明等15种减肥药的高效液相色谱-串联质谱(HPLC-MS/MS)分析方法。样品经乙腈沉淀后,进入HPLC-MS/MS中分析检测。以甲醇和含0.1%(v/v)冰醋酸的20 mmol/L醋酸铵溶液作为流动相,采用梯度洗脱方式,以UltimateXB-C18为色谱柱进行HPLC分析;质谱分析采用电喷雾离子源,正负离子快速切换扫描,选择反应监测模式检测。15种减肥药的定量限在0.001～0.05 mg/L内,各种药物的灵敏度较高,各成分的线性相关系数均大于0.99,精密度均小于12.3%,回收率范围为77.3%～110.8%。研究了这15种药物的质谱特征。该方法灵敏、简便、快捷、专属性强,可用于动物实验样品中减肥药物的含量测定,并且对其他药品、食品中目标减肥药物的测定具有借鉴意义。

关键词: 减肥药物, 血液, 液相色谱-串联质谱

Abstract: An analytical method for the simultaneous determination of 15 anti-obesity drugs (caffeine, sibutramine, phenformin, etc.) in blood sample was developed using high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). After a simple protein precipitation step, the HPLC separation was performed on an UltimateXB-C18 column with methanol and 20 mmol/L ammonium acetate (containing 0.1%(v/v) of glacial acetic acid) as the mobile phases in a gradient elution mode. The MS/MS detection was achieved by electrospray ionization in both positive and negative modes by rapid switching with selective reaction monitoring (SRM). The results showed that the limits of quantification of all anti-obesity drugs were in the range of 0.001~0.05 mg/L. The calibration curves of all anti-obesity drugs showed good linearity and the correlation coefficients were more than 0.99. The recoveries of all anti-obesity drugs at 3 spiked levels were in the range of 77.3%~110.8% with the intra-day and inter-day precisions less than 12.3%. The mass spectrum characterizations of 15 anti-obesity drugs were studied. The method is sensitive and reproducible for the detection of the 15 anti-obesity drugs in blood, and can also be applied to the determination of the anti-obesity drugs in pharmaceuticals or foods.

Key words: anti-obesity drugs, blood, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS)