法医学杂志 ›› 2007, Vol. 0 ›› Issue (6): 441-443.

• 论文 • 上一篇    下一篇

液相色谱-串联质谱法检测血液中的美西律

严慧;向平;卜俊;沈敏;   

  1. 司法部司法鉴定科学技术研究所,司法部司法鉴定科学技术研究所,司法部司法鉴定科学技术研究所,司法部司法鉴定科学技术研究所 上海200063 复旦大学上海医学院法医学系,上海200032,上海200063,上海200063,上海200063
  • 发布日期:2007-12-25 出版日期:2007-12-28

Determination of Mexiletine in Human Blood by Liquid Chromatography-Tandem Mass Spectrometry

YAN HUI1, 2, XIANG PING1, BO JUN1, SHEN MIN1 (1. INSTITUTE OF FORENSIC SCIENCES, MINISTRY OF JUSTICE, SHANGHAI 200063, CHINA; 2. DEPARTMENT OF FORENSIC MEDICINE, SHANGHAI MEDICAL COLLEGE, FUDAN UNIVERSITY, SHANGHAI 200032, CHINA)   

  • Online:2007-12-25 Published:2007-12-28

摘要: 目的建立测定血液中美西律(mexiletine)的液相色谱-串联质谱联用法(LC-MS/MS)。方法采用简便的乙腈蛋白沉淀法对血液进行预处理,应用Allure PFP Propyl液相柱分离,用电喷雾正离子模式离子化,多反应监测模式对美西律进行分析。结果美西律与内标纳洛酮分离良好,在0.02~10.00μg/mL内线性关系良好,相关系数为0.9999,回归方程为y=0.0283x-0.0151,日内与日间精密度的RSD均小于15%,最低检测限为0.01μg/mL。结论建立的LC-MS/MS方法简单、灵敏、可靠,可同时适用于美西律临床药物监测和法医毒物分析的需要。

关键词: LC-MS/MS, 抗心律失常药, 美西律, 血液

Abstract: Objective To establish a liquid chromatography-tandem mass spectrometry(LC-MS/MS) method for detection of mexiletine by liquid chromatography tandem mass spectrometry. Methods After simple protein precipitation of the blood sample with acetonitrile, the organic solvent layer diluted with LC mobile solvent was separated by Allure PFP Propyl column, confirmed and quantified by MS/MS in the multi-reaction monitoring (MRM) mode via positive electrospray ionization. Results Mexiletine and naloxone (internal standard) got ideal resolution under the selected analytical condition. The correlation coeficient of linear calibration curve was over 0.999 9 within the mexiletine concentration range 0.02-10 μg/mL. The relative standard deviations were under 10% for intra-day and under 15% for inter-day, and the detection limit was 0.01 μg/mL. Conclusion The established LC-MS/MS method is simple, rapid, sensitive, unaffected by matrix effect and appropriate for detection of mexiletine in blood in the field of therapeutic drug monitoring and forensic toxicology.

Key words: LC-MS/MS, anti-arrhythmic drugs, mexiletine, blood