色谱

色谱 ›› 2014, Vol. 32 ›› Issue (7): 687-692.DOI: 10.3724/SP.J.1123.2014.04013

• 研究论文 • 上一篇    下一篇

自动固相萃取-液相色谱-飞行时间质谱法快速筛查与确证血液中抗抑郁类药物

石银涛1, 郭璟琦1, 王绘军1, 段杰1, 喻洪江2, 郑经1, 王俊伟1   

  1. 1. 重庆市公安局物证鉴定中心, 重庆 400021;
    2. 重庆警察学院禁毒系, 重庆 401331
  • 收稿日期:2014-04-08 修回日期:2014-05-07 出版日期:2014-07-08 发布日期:2014-06-25
  • 通讯作者: 王俊伟，E-mail：wjwry@tom.com.
  • 基金资助:

    重庆市公安局科技攻关计划项目（G2013-04）.

Rapid screening and confirmation of antidepressants in blood using automated solid phase extraction and liquid chromatography-time-of-flight mass spectrometry

SHI Yintao1, GUO Jingqi1, WANG Huijun1, DUAN Jie1, YU Hongjiang2, ZHENG Jing1, WANG Junwei1   

  1. 1. Chongqing Institute of Forensic Science, Chongqing 400021, China;
    2. Drug Exhibition Department, Chongqing Police College, Chongqing 401331, China
  • Received:2014-04-08 Revised:2014-05-07 Online:2014-07-08 Published:2014-06-25

PDF

263

被引次数

13

摘要：

建立了血液中抗抑郁类药物快速筛查的自动固相萃取-液相色谱-飞行时间质谱（ASPE-LC-Q-TOF/MS）方法。样品经HLB固相萃取柱提取后，采用LC-Q-TOF/MS进行测定，外标法定量。结果表明：目标物的线性范围为1~500 μg/L，相关系数为0.9976~0.9997，检出限为0.01~0.5 μg/L。在10、100和500 μg/L 3个添加水平的平均回收率为79.6%~96.4%，相对标准偏差为4.1%~6.4%。利用Agilent MassHunter PCDL Manager软件建立了抗抑郁类药物数据库，并应用于加标样品的筛查分析，本方法能够全部筛查出样品中添加的抗抑郁类药物，鉴定准确度达到100%，且保留时间偏差均小于0.1 min，质量偏差均小于1 mDa，同位素丰度匹配得分、同位素间距得分和MS匹配得分均大于95，MS/MS图谱匹配得分均大于70。利用本方法对实际案例进行筛查分析，检出阿米替林、卡马西平和多虑平，说明该方法可用于法庭与临床毒物分析。

关键词: 飞行时间质谱, 抗抑郁类药物, 确证, 筛查, 血液, 液相色谱, 自动固相萃取

Abstract:

A high-throughput method was developed for screening antidepressants in blood by automated solid phase extraction and liquid chromatography with high resolution quadrupole-time-of-flight mass spectrometry (ASPE-LC-Q-TOF/MS). The samples were cleaned up by an HLB solid phase extraction cartridge and analyzed by LC-Q-TOF/MS under electrospray ionization (ESI) mode with scanning range of m/z 50-1000 Da. The chromatographic separation was performed on an Agilent Eclipse Plus C18 column (50 mm×2.1 mm, 1.8 μm) with gradient elution using methanol and 5 mmol/L ammonium formate aqueous solution (containing 0.2% formic acid) as mobile phases. Rapid screening and confirmation can be achieved using MS matching scores, deviation of retention time, measured mass, isotopic abundance matching scores, isotope space matching scores and MS/MS matching scores. The quantitative analysis was carried out by correlating the extracting peak area with accurate mass. Good linearities were observed in the range of 1-500 μg/L with the correlation coefficients from 0.9976 to 0.9997. The limits of detection were 0.01-0.5 μg/L. The spiked recoveries were 79.6%-96.4% with the relative standard deviations of 4.1%-6.4%. The result screening database was built using Agilent MassHunter PCDL Manager software and then used for the analysis of spiked samples. MS matching scores, isotopic abundance matching scores, isotope space matching scores (all > 95 points) and MS/MS matching scores (> 70 points) were applied to identify the analytes. The results showed that all the spiked antidepressants could be correctly identified with low deviation of retention time (< 0.1 min) and mass (< 1 mDa). The developed method was further applied for the analysis of poisoning cases, and amitriptyline, carbamazepine, doxepin were detected. In brief, the method is rapid, sensitive, simple, reliable, and suitable for the screening and confirmation of antidepressants in forensic and clinical analytical toxicology.

Key words: antidepressants, automated solid phase extraction (ASPE), blood, confirmation, liquid chromatography (LC), screening, time-of-flight mass spectrometry (TOF/MS)

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