| 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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| 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) |
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| 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81%和86%。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 |
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| Simultaneous Determination of Four New Psychoactive Substances of Cathinone in Blood Samples by Ultra-high Performance Liquid Chromatography-Quadrupole-Time-of-flight Mass Spectrometry |
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| 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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