色谱

色谱 ›› 2019, Vol. 37 ›› Issue (1): 80-86.DOI: 10.3724/SP.J.1123.2018.08004

• 研究论文 • 上一篇    下一篇

超高效液相色谱-串联质谱法检验腐败血中吗啡和6-单乙酰吗啡

吕昱帆1, 王继芬1, 常靖2, 李超1, 彭山珊1   

  1. 1. 中国人民公安大学刑事科学技术学院, 北京 100038;
    2. 公安部物证鉴定中心, 北京 100038
  • 收稿日期:2018-08-02 出版日期:2019-01-08 发布日期:2014-11-29
  • 通讯作者: 王继芬,Tel:(010)83901370,E-mail:wangjifen58@126.com;常靖,E-mail:changjing73@126.com.
  • 基金资助:

    国家重点研发计划（2017YFC0803604-2）.

Determination of morphine and 6-monoacetylmorphine in putrefied blood using ultra performance liquid chromatography-tandem mass spectrometry

LYU Yufan1, WANG Jifen1, CHANG Jing2, LI Chao1, PENG Shanshan1   

  1. 1. School of Criminal Science and Technology, People's Public Security University of China, Beijing 100038, China;
    2. Institute of Forensic Science, Ministry of Public Security, Beijing 100038, China
  • Received:2018-08-02 Online:2019-01-08 Published:2014-11-29
  • Supported by:

    National Key Research and Development Program (No.2017YFC0803604-2).

PDF

47

摘要：

采用改良的QuEChERS前处理方法，建立了同时检验腐败血中吗啡和6-单乙酰吗啡的超高效液相色谱-串联质谱（UPLC-MS/MS）方法。腐败血中加入乙腈-水（4：1，v/v）混合溶液、30 mg NaCl和60 mg MgSO4盐析促进相分离，最后经25 mg N-丙基乙二胺（PSA）和25 mg MgSO4净化。选用ZORBAX Eclipse Plus C18色谱柱分离，0.01%（v/v）氨水和乙腈作为流动相进行梯度洗脱，电喷雾电离正离子（ESI+）模式扫描，多反应监测（MRM）模式检测。结果表明，吗啡和6-单乙酰吗啡在5~200 μg/L范围内线性关系良好，相关系数（r2）≥ 0.9957，检出限（S/N=3）均为1 μg/L，定量限（S/N=10）均为5 μg/L。3个加标水平（5、100和200 μg/L）下，吗啡和6-单乙酰吗啡的平均加标回收率分别为81.84%~103.44%和81.03%~104.46%，日内和日间精密度（RSD）均小于12%，基质效应为83.04%~107.61%。方法简便、灵敏、可靠，可实现腐败血中吗啡和6-单乙酰吗啡的快速定性定量检验。

关键词: 6-单乙酰吗啡, QuEChERS, 超高效液相色谱-串联质谱, 腐败血, 吗啡

Abstract:

This study was performed to develop an ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) method to detect and quantify morphine and 6-monoacetylmorphine in putrefied blood for forensic toxicological purposes. A modified QuEChERS method was implemented as follows:extraction of morphine and 6-monoacetylmorphine from putrefied blood was performed with an acetonitrile-water (4:1, v/v) mixture, and 30 mg NaCl and 60 mg anhydrous MgSO4 were subsequently added as salting out agents to induce phase separation. The supernatant was cleaned by adding 25 mg primary secondary amine sorbent (PSA) and 25 mg anhydrous MgSO4. Separation of the target compounds was performed using a ZORBAX Eclipse Plus C18 column by UPLC over a 4 min gradient elution where 0.01% (v/v) ammonium hydroxide buffer (A) and acetonitrile (B) were used as the mobile phase. MS/MS was used in positive electrospray ionization (ESI+) mode and multiple-reaction monitoring (MRM) was performed to detect the target drugs. This method achieved satisfactory recoveries (R) for morphine and 6-monoacetylmorphine with mean recovery values ranging from 81.84% to 103.44% and 81.03% to 104.46% respectively. The developed method also provided efficient purification of the sample from endogenous interferences with matrix effect (ME) ranging from 83.04% to 107.61%. The method was validated and the limit of detection (LOD) and limit of quantification (LOQ) were 1 and 5 μg/L, respectively, for both compounds and the precision with RSD ranged from 1% to 12%. This method proved to be quick, sensitive, rugged, and suitable for the analysis of illegal drugs in putrefied whole blood.

Key words: 6-monoacetylmorphine, morphine, putrefied blood, QuEChERS, ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

中图分类号: