法医学杂志

法医学杂志 ›› 2011, Vol. 27 ›› Issue (5): 350-352.DOI: 10.3969/j.issn.1004-5619.2011.05.009

• 论著 • 上一篇    下一篇

固相萃取-液相色谱-串联质谱法测定全血中多塞平

龚飞君，严松茂，吴忠平，张润生   

  1. （上海市公安局物证鉴定中心 上海市现场物证重点实验室，上海 200083）
  • 发布日期:2011-10-25 出版日期:2011-10-28
  • 通讯作者: 通信作者：张润生，男，主任法医师，主要从事毒物分析工作和研究；E-mail：zhangrs@sh163.net
  • 作者简介:龚飞君（1977—），女，上海人，主检法医师，主要从事毒物分析工作和研究；E-mail：kallikrein@sina.com

Determination of Doxepin in Whole Blood by SPE-LC-MS/MS

GONG FEI-JUN, YAN SONG-MAO, WU ZHONG-PING, ZHANG RUN-SHENG   

  1. （Shanghai Key Laboratory of Crime Scene Evidence, Institute of Forensic Science, Shanghai Public Security Bureau, Shanghai 200083, China）
  • Online:2011-10-25 Published:2011-10-28

被引次数

2

摘要： 目的 建立固相萃取-液相色谱-串联质谱（SPE-LC-MS/MS）分析全血中多塞平的方法。 方法 以阿米替林为内标，全血样品经固相萃取处理后，通过液相色谱-串联质谱技术进行检测（电喷雾离子源正离子方式，多反应监测模式）。监测离子对m/z多塞平为280→107、280→235、280→220，阿米替林为278→233。多塞平和阿米替林的保留时间分别为15.15 min和16.94 min。 结果 全血中多塞平在0.005~1.00 μg/mL质量浓度范围内呈线性关系，线性方程为y=3.204 7 x+0.033 9，相关系数（r）=0.999 6，检出限为0.001 μg/mL；平均提取回收率为78.0%～82.9%，日内精密度<2.55%，日间精密度<5.90%。 结论 本方法快速简便、灵敏、重现性好，适用于全血中多塞平的检测。

关键词: 法医毒理学, 固相萃取, 液相色谱-串联质谱法, 多塞平, 血液

Abstract: Objective To develop a method of SPE-LC-MS/MS for the determination of doxepin in whole blood. Methods After solid phase extraction, the samples were identified by LC-MS/MS. Positive ion electrospray ionization mode and multiple reaction monitoring（MRM） mode was selected. Amitriptyline was used as internal standard. The m/z of doxepin： 280→107, 280→235 and 280→220. The m/z of amitriptyline： 278→233. The retaining time of doxepin and amitriptyline were 15.15 and 16.94 min, respectively. Results The calibration curve was linear among the concentration of doxepin range from 0.005 to 1.00 μg/mL. The linear correlation equation was y=3.204 7 x+0.033 9, the correlation coefficient was 0.999 6. The detection limit of doxepin was 0.001 μg/mL and average recovery rate was 78.0%-82.9%. The relative standard precision for within-day and between-day were less than 2.55% and 5.90%, respectively. Conclusion The method is effective, simple, reliable and can be used in the determination of doxepin in whole blood.

Key words: forensic toxicology, solid phase extraction, LC-MS/MS, doxepin, blood

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