摘要
随着新精神活性物质(NPS)种类不断增加、滥用越来越广泛,其兴起给各国禁毒机构带来严峻挑战。该文建立了实时直接分析串联质谱(DART-MS/MS)检测尿液中12种苯二氮卓类新精神活性物质(DBZDs)的方法。优化了质谱条件、进样量、载气加热器温度和前处理方法,并进行了方法学验证。结果表明:使用乙酸乙酯进行液液萃取后,移取5μL上清液至玻璃棒下端,采用DART 12Dip-ItTM玻璃棒自动进样装置进样,载气加热器温度为300℃,在正离子模式下使用多反应监测(MRM)模式分析时可得到最佳响应。采用地西泮-D5作为内标进行定量分析,该方法在0.05~5μg/mL范围内线性关系良好,相关系数(r2)> 0.99;检出限为0.5~20 ng/mL,定量下限为1~50 ng/mL;基质效应为-11.1%~12.6%,回收率为94.7%~115%,高、中浓度的日内及日间相对标准偏差(RSD)均不大于15%,定量下限浓度的日内及日间RSD均不大于17%。方法的重复性良好,符合实战工作要求。
As the variety of new psychoactive substances(NPS)continues to increase and their abuse becomes more and more widespread,their rising popularity poses a serious challenge to national antidrug agencies.Herein,a direct analysis of real time-tandem mass spectrometry(DART-MS/MS)was developed for the detection of 12 NPS of benzodiazepines(DBZDs)in urine.The MS conditions,including injection volume,carrier gas heater temperature and pretreatment method were optimized.Methodological validation was performed.The results showed that the best pretreatment effect was ob⁃tained by liquid-liquid extraction using ethyl acetate.Then,5μL supernatant was pipetted into the bottom of a glass rod,and a DART 12Dip-It™sampler was used for sampling.The best response was obtained by analysis in positive ionization mode under multiple reaction monitoring(MRM)mode at a carrier gas heater temperature of 300℃.The quantitation analysis of DBZDs was performed by internal standard method with diazepam-D5 as the internal standard.The linear relationships for 12 DBZDs were good in the range of 0.05-5μg/mL,with correlation coefficients(r2)great than 0.99.The limits of detection and the limits of quantitation were in the range of 0.5-20 ng/mL and 1-50 ng/mL,respectively.The average matrix effects were in the range of-11.1%-12.6%.The av⁃erage recoveries ranged from 94.7%to 115%,with intra-day relative standard deviations(intra-RS⁃Ds)and inter-RSDs for high and medium concentrations both not more than 15%,as well as the intra-RSDs and inter-RSDs for concentration of quantitative limit not more than 17%.The method is rapid,simple and reproducible,and could meet the requirements for rapid detection of 12 NPS BZDs in urine in the public security field.
作者
刘富邦
王继芬
张瑛
LIU Fu-bang;WANG Ji-fen;ZHANG Ying(School of Investigation,People’s Public Security University of China,Beijing 100038,China;Forensic Science Service of Beijing Public Security Bureau,Key Laboratory of Forensic Toxicol,Ministry of Public Security,Beijing 100192,China)
出处
《分析测试学报》
CAS
CSCD
北大核心
2023年第6期684-691,共8页
Journal of Instrumental Analysis
基金
中国人民公安大学拔尖创新人才培养经费支持研究生科研创新重点项目(2022yjsky013)
毒物基础数据库的建设项目(2022SJKJS07)。
