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超高效液相色谱-四极杆飞行时间质谱同时检测血样中4种卡西酮类新精神活性物质
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刘静,何洪源,倪春芳,曹芳琦,赵海波,徐琳 1.中国人民公安大学侦查与刑事科学技术学院2.上海市公安局物证鉴定中心上海市现场物证重点实验室3.上海市刑事科学技术研究院上海市现场物证重点实验室4.太原市公安局迎泽分局 
基金项目:国家重点研发计划课题(2017YFC0822001);中国人民公安大学基本科研业务费(2020GKF102);中国人民公安大学2019年拔尖人才培养专项资助硕士研究生科研创新资助项目(2019ssky007)
中文摘要:建立了同时检测血样中3,4-亚甲二氧基甲卡西酮(Methylone)、3,4-亚甲二氧基乙卡西酮(Ethylone)、4-氯甲卡西酮(4-CMC)、4-氯乙卡西酮(4-CEC)4种卡西酮类新精神活性物质的超高效液相色谱-四极杆飞行时间质谱法(UHPLC-QTOF MS/MS)。取0.5 mL血液,按体积比5∶2∶13将血液、水和乙腈混合,涡旋振荡1 min,以12 000 r/min离心15 min将蛋白沉淀,取上清液待测。采用Acquity UPLC-BEH C18色谱柱(2.1 mm×100 mm,1.7 μm)分离,0.1%甲酸-水(5 mmol/L乙酸铵)和乙腈作为流动相进行梯度洗脱,采用多反应监测(MRM)模式,正离子[M+H]+扫描检测。结果表明,4种目标药物在5~500 ng/mL 质量浓度范围内线性关系良好,检出限为2 ng/mL,定量下限为5 ng/mL,回收率为87.3%~111%,日内和日间相对标准偏差分别不大于81%和86%。该方法可同时检测血样中4种卡西酮类新精神活性物质,满足实际检验需要。
中文关键词:超高效液相色谱-四极杆飞行时间质谱  卡西酮类新精神活性物质  沉淀蛋白  血样
 
Simultaneous Determination of Four New Psychoactive Substances of Cathinone in Blood Samples by Ultra-high Performance Liquid Chromatography-Quadrupole-Time-of-flight Mass Spectrometry
Abstract:An ultra high performance liquid chromatography-quadrupole-time of flight mass spectrometry(UHPLC-QTOF MS/MS) was established for the simultaneous determination of 4 kinds of new psychoactive substances of cathinone in blood samples,including 1-(3,4-methylenedioxyphenyl)-2-methylaminopropan-1-one(methylone),1-(3,4-methylenedioxyphenyl)-2 ethylaminopropan 1-one(ethylone),1-(4-chlorophenyl)-2-methylaminopropan-1-one(4 CMC) and 1-(4-chlorophenyl)-2-ethylaminopropan-1-one(4-CEC).0.5 mL blood sample was mixed with water and acetonitrile by a volume ratio of 5∶2∶13,vortex oscillated for 1 min,and centrifuged at 12 000 r/min for 15 min to precipitate the protein.The supernatant was separated on an Acquity UPLC-BEH C18 column(2.1 mm×100 mm,1.7 μm),with 0.1% formic acid-water(5 mmol/L ammonium acetate) and acetonitrile as mobile phases by gradient elution,and detected in positive ion[M+H]+ scanning under multiple reaction monitoring(MRM) mode.Results showed that there were good linear relationships for four target drugs in the concentration range of 5-500 ng/mL,with the limits of detection and limits of quantitation of 2 ng/mL and 5 ng/mL,respectively.The recoveries ranged from 87.3% to 111% with the intra day precision and inter day precision not more than 8.1% and 8.6%,respectively.The method could be used for the simultaneous detection of 4 new psychoactive substances of cathinone in blood samples to meet the needs of actual inspection work.
Key Words:ultra-high performance liquid chromatography-quadrupole-time-of-flight mass spectrometry(UHPLC-QTOF MS/MS)  new psychoactive substances of cathinone  precipitated protein  blood sample
引用本文:刘静,何洪源,倪春芳,曹芳琦,赵海波,徐琳.超高效液相色谱-四极杆飞行时间质谱同时检测血样中4种卡西酮类新精神活性物质[J].分析测试学报,2020,39(12):1521-1526.
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