气相色谱-质谱法同时检测尿液中8种卡西酮类新精神活性物质

Simultaneous Determination of Eight Cathinones New Psychoactive Substances in Urine by Gas Chromatography-Mass Spectrometry

卡西酮类新精神活性物质是在诸多国家滥用较为广泛的一类人工合成的新精神活性物质。该文采用气相色谱-质谱法建立了尿液中8种卡西酮类新精神活性物质同时定性、定量的分析方法。取尿液试样适量,加入内标N,N-二甲基苯胺,经环己烷溶剂萃取,离心取上清液进样分析。结果表明,尿液中8种目标物在各自浓度范围内线性关系良好,检出限(LOD)为0.002~0.01μg/mL,定量下限(LOQ)为0.005~0.02μg/mL,平均回收率为92.4%~99.4%,日内精密度不高于7.8%,日间精密度不高于8.8%。所建立的方法具有快速、灵敏、高效、准确等特点,不仅能为涉毒案件相关物证的鉴定、案件侦破与诉讼等提供一定的科学理论与技术支持,而且能为打击毒品违法犯罪提供一定帮助。

In recent years,new psychoactive substances(NPS)are popular rapidly on the illicit drug market,which have attracted a great concern all over the world.The surge in abuse of NPS has become a serious social problem.As one of the largest growing class of NPS,synthetic cathinones have been widely abused for their cocaine and amphetamine-like pharmacological effects,and have received a widespread attention in many countries.In this article,a gas chromatography-mass spectrometry(GC-MS)with liquid-liquid extraction was developed for the simultaneous determination of eight synthetic cathinones,i.e.methcathinone(MC),4-chloroethcathinone(4-CEC),4-methylpentedrone(4-MPD),3,4-methylenedioxy-N-methylcathinone(MDMC),4′-methyl-α-pyrrolidinopropiophenone(4-MePPP),3,4-methylenedioxy-N-ethylcathinone(MDEC),4′-chloro-α-pyrrolidinopropiophenone(4-Cl-α-PPP)and 3,4-methylenedioxypyrovalerone(MDPV).Firstly,the extraction factors influencing the extraction efficiency were investigated,and the optimal procedures of liquid-liquid extraction were as follows:5.00 mL blank urine was added with 5μL internal standard N,N-dimethylaniline standard solution(1.00 mg/mL),0.50 mL Na2CO3-NaHCO3 buffer solution(pH 10.80),50 mg sodium chloride and 0.5 mL cyclohexane were vortex-oscillated for 3 min,and then centrifuged at 5000 r/min for 10 min,the supernatant was injected and analyzed on GC-MS spectrometer.Secondly,the instrumental conditions for GC-MS including GC and MS parameters for simultaneously determining eight synthetic cathinones were optimized in details,and then the qualitative and quantitative analysis of these target compounds in urine were performed by GC-MS,the characteristic ions for qualitative and quantitative analysis were both obtained while the GC-MS spectra were recorded at the same time,then the regression equations,limits of detection(LODs),limits of quantitation(LOQs),inter-day and intra-day precisions and average recoveries for eight synthetic cathinones in urine were examined,respectively.Experimental results showed that the analytical approach developed was sensitive in qualitative analysis and accurate in quantitative analysis of synthetic cathinones in urine.MC,4-CEC,MDMC and MDEC exhibited good linearity in the concentration range of 0.02-5.00μg/mL with their LODs and LOQs of 0.01μg/mL and 0.02μg/mL,respectively.Their recoveries ranged from 93.2%to 98.5%with the intra-day precision and inter-day precision not more than 7.8%and 8.8%,respectively.4-MPD,4-MePPP and 4-Cl-α-PPP exhibited good linearity in the concentration range of 0.01-5.00μg/mL with their LODs and LOQs of 0.005μg/mL and 0.01μg/mL,respectively.Their recoveries ranged from 93.6%to 99.4%with the intra-day precision and inter-day precision not more than 6.0%and 7.4%,respectively.MDPV exhibited good linearity in the concentration range of 0.005-5.00μg/mL with its LODs and LOQs of 0.002μg/mL and 0.005μg/mL,respectively,Its recoveries ranged from 92.4%to 97.2%with the intra-day precision and inter-day precision not more than 4.4%and 5.3%,respectively.Therefore,the developed method could not only offer a certain scientific and technical support for the relevant material evidence identification and litigation cases,but also provide a tool to combat drug crime in our country.