法医学杂志

法医学杂志 ›› 2020, Vol. 36 ›› Issue (2): 216-222.DOI: 10.12116/j.issn.1004-5619.2020.02.013

• 论著 • 上一篇    下一篇

8种常见药（毒）物LC-MS/MS定性分析的保留时间和离子丰度比

闵涛1， 刘少丹2， 辛国斌3， 张大明1，3   

  1. 1. 山西医科大学法医学院，山西 太原 030001； 2. 迪安鉴定科学研究院，浙江 杭州 310000； 3. 北京市公安司法鉴定中心，北京 100192
  • 发布日期:2020-04-25 出版日期:2020-04-28
  • 通讯作者: 张大明，男，博士，教授，主要从事法医毒物分析鉴定及研究；E-mail：zdm64880@163.com
  • 作者简介:闵涛（1992—），女，硕士，主要从事法医毒物分析研究；E-mail：15600907967@163.com
  • 基金资助:
    公安部科技强警基础工作专项资助项目（2017GABJC06）

Retention Time and Ion Abundance Ratio of 8 Common Drugs （Poisons） by LC-MS/MS Qualitative Analysis#br#

MIN Tao1, LIU Shao-dan2, XIN Guo-bin3, ZHANG Da-ming1,3   

  1. 1. School of Forensic Medicine, Shanxi Medical University, Taiyuan 030001, China; 2. Dian Institute of Forensic Science, Hangzhou 310000, China; 3. Forensic Judicial Appraisal Center of Beijing Public Security Bureau, Beijing 100192, China
  • Online:2020-04-25 Published:2020-04-28
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摘要： 目的 探讨法医毒物分析中液相色谱-串联质谱（liquid chromatography-tandem mass spectrometry，LC-MS/MS）法检测血液中毒品类（甲基苯丙胺、吗啡、氯胺酮）、苯二氮[蓝][卓]类（艾司唑仑、咪达唑仑、地西泮、氯硝西泮）和巴比妥类（苯巴比妥）共3大类8种常见药（毒）物的保留时间和离子丰度比的最大允许偏差。 方法 在2根色谱柱、3种色谱条件下，经液液萃取后采用LC-MS/MS进行检测，分析质量浓度在检出限（limit of detection，LOD）、2倍检出限（2LOD）、定量限（limit of quantitation，LOQ）、1.5倍定量限（1.5LOQ）、2倍定量限（2LOQ）、4倍定量限（4LOQ）和6倍定量限（6LOQ）共7个较低质量浓度时保留时间和离子丰度比的偏差。 结果 血液添加样品中8种药（毒）物绝对保留时间的偏差在±0.05 min范围内的占98.11%，相对保留时间的偏差在±0.4%范围内的占96.21%。离子丰度比的最大偏差与质量浓度存在高度关联：药（毒）物质量浓度为LOQ及以上时，离子丰度比的绝对偏差和相对偏差都有95%以上分别在±25%和±40%范围内；质量浓度为LOQ以下时，范围可分别扩大至±35%和±50%。 结论 建议8种常见药（毒）物绝对保留时间的偏差判定范围为±0.1 min，相对保留时间的偏差判定范围为±1.0%。质量浓度在LOQ及以上时离子丰度比的绝对偏差判定范围为±25%，相对偏差为±40%，质量浓度在LOQ以下时偏差判定范围可分别扩大至±35%和±50%。

 

关键词: 法医毒理学, 液相色谱-质谱法, 保留时间, 离子丰度比, 甲基苯丙胺, 吗啡, 氯胺酮, 艾司唑仑, 咪达唑仑, 地西泮, 氯硝西泮, 苯巴比妥

Abstract: Objective To investigate the maximum allowable deviations of retention time and ion abundance ratio of the 8 common drugs （poisons） from 3 categories, poisons （methamphetamine, morphine, ketamine）, benzodiazepines （estazolam, midazolam, diazepam, clonazepam） and barbiturates （phenobarbital） in blood, by liquid chromatography-tandem mass spectrometry （LC-MS/MS） in forensic toxicology analysis. Methods The deviations of retention time and ion abundance ratio at 7 low mass concentrations, limit of detection （LOD）, 2LOD, limit of quantitation （LOQ）, 1.5LOQ, 2LOQ, 4LOQ and 6LOQ, were tested by LC-MS/MS after liquid-liquid extraction under the conditions of two chromatographic columns and three chromatographs. Results The deviation of absolute retention time of 98.11% of 8 drugs （poisons） in the blood samples was within the range of ±0.05 min, and that of the relative retention time of 96.21% was within the range of ±0.4%. The maximum deviation of the ion abundance ratio was highly correlated with the mass concentration. When the mass concentration of drugs （poisons） was LOQ or above, more than 95% of the absolute deviation and relative deviation of the ion abundance ratio were in the range of ±25% and ±40%, respectively; when the mass concentration was below LOQ, the range could be expanded to ±35% and ±50%, respectively. Conclusion It is recommended for the determination range of the absolute retention time deviation of 8 common drugs （poisons） to be ±0.1 min and that of the relative retention time deviation to be ±1.0%. The determination range of absolute deviation of the ion abundance ratio should be ±25% when the mass concentration is LOQ or above, and the relative deviation should be ±40%. When the mass concentration is below LOQ, the deviation determination range can be expanded to ±35% and ±50%, respectively.

Key words: forensic toxicology, liquid chromatography-mass spectrometry, retention time, ion abundance ratio, methamphetamine, morphine, ketamine, estazolam, midazolam, diazepam, clonazepam, phenobarbital

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