超高效合相色谱-质谱法对甲卡西酮对映异构体的手性分离和定量检测  

Chiral separation and quantitative determination of methcathinone enantiomers by ultra-performance convergence chromatography-mass spectrometry

作　　者：胡爽 武磊[1] 黄钰 杜宇 花镇东[3] HU Shuang;WU Lei;HUANG Yu;DU Yu;HUA Zhendong(Department of Criminal Science and Technology,Beijing Police College,Beijing 102202,China;School of Pharmacy,China Pharmaceutical University,Nanjing 210009,China;Anti-drug Information Technology Center of the Ministry of Public Security,Beijing 100193,China)

机构地区：[1]北京警察学院刑事科学技术系,北京102202 [2]中国药科大学药学院,南京210009 [3]公安部禁毒情报技术中心,北京100193

出　　处：《分析试验室》2024年第3期402-408,共7页Chinese Journal of Analysis Laboratory

基　　金：北京市教育委员会科研项目(KM202114019001);北京警察学院科研项目(2022KZD03)资助。

摘　　要：建立了超高效合相色谱-质谱法(UPC^(2)-MS)对甲卡西酮(MC)对映异构体进行手性分离和定量检测。使用Acquity UPC^(2)Trefoil CEL^(2)(2.5μm,3.0 mm×150 mm)手性色谱柱,以超临界流体CO_(2)为主要流动相,含10 mmol/L甲酸铵和0.1%甲酸的异丙醇为改性剂进行梯度洗脱,可以在13 min内实现2个对映异构体的基线分离。在三重四极杆质谱多反应监测(MRM)模式下,2个对映异构体的检出限为0.5 ng/mL,定量限为1.0 ng/mL,在1~100 ng/mL质量浓度范围内线性关系良好,线性相关系数(R^(2))≥0.999,10种常见毒品和药品对检测均无干扰。对实际缴获毒品的检测结果表明:直接作为毒品销售的MC主要为外消旋体,而非法制造麻黄碱的地下窝点缴获的MC以S构型为主。A chiral separation and quantification method for methcathinone(MC)enantiomers based on ultraperformance convergence chromatography-mass spectrometry(UPC^(2)-MS)was developed.The baseline separation of two enantiomers could be achieved within 13 min under the conditions of acquity UPC^(2) Trefoil CEL2(2.5μm,3.0 mm×150 mm)as chiral column,supercritical fluid CO_(2) as primary mobile phase,isopropanol containing 10 mmol/L ammonium formate and 0.1%formic acid as the modifier for gradient elution.Under the multi reaction monitoring(MRM)mode of triple quadrupole mass spectrometry,the limits of detection were 0.5 ng/mL and the limits of quantification were 1.0 ng/mL for both enantiomers.There were great linear relationships in the concentration range of 1.0-100 ng/mL,and the correlation coefficients(R^(2))were not less than 0.999.10 common drugs did not interfere with the determination of target substances.The seized drug samples were analyzed using this method,and the results showed that the methcathinone products seized in the market as drugs were mainly in racemic form,while that seized from illegal ephedrine manufacturing dens were mainly in S-configuration.

关 键 词：超高效合相色谱-质谱 甲卡西酮 对映异构体 手性分离 

分 类 号：O656.2[理学—分析化学]