在线固相萃取-超高效液相色谱-串联质谱法同时测定血液样品中12种卡西酮类毒品  

Simultaneous Determination of 12 Cathinones in Blood Samples by Online Solid Phase Extraction Coupled to UPLC-MS/MS

作　　者：孙立敏[1] 王松才[1] 林贤文[1] 朱焕慧[1] 刘悦 谭莉 SUN Limin;WANG Songcai;LIN Xianwen;ZHU Huanhui;LIU Yue;TAN Li(Guangzhou Institute of Criminal Science and Technology,Guangzhou 510030,China)

机构地区：[1]广州市刑事科学技术研究所,广东广州510030

出　　处：《中国司法鉴定》2023年第2期55-60,共6页Chinese Journal of Forensic Sciences

基　　金：广州市民生科技攻关重大专项(2019030009)。

摘　　要：目的建立一种同时测定血液样品中12种卡西酮类毒品的在线固相萃取-超高效液相色谱-串联质谱法。方法血液样品用乙腈沉淀蛋白,经离心、稀释、过滤后上样,采用PLRP-S在线固相萃取柱(2.1 mm×12.5 mm,15~20μm)富集纯化,Poroshell 120 EC-C_(18)色谱柱(3.0 mm×150 mm,2.7μm)进行分离,在线固相萃取柱以乙腈-5%(体积分数)甲醇作为流动相进行流速1.0 mL/min的梯度洗脱,色谱柱以5 mmol/L乙酸铵缓冲液[含0.1%(体积分数)甲酸]-乙腈作为流动相进行流速0.4 mL/min的梯度洗脱。离子源为电喷雾离子源,采用多反应监测模式进行测定。结果12种卡西酮类毒品线性关系良好,相关系数均大于0.998,方法检出限为0.1~0.5 ng/mL,定量限为0.3~1.5 ng/mL。12种卡西酮类毒品在3个不同质量浓度条件下的回收率为70.9%~108%,日内精密度和日间精密度分别为1.5%~8.9%、5.1%~44.5%(n=6)。结论该方法操作简单方便、样品需求量少、灵敏度高、检出限低,可用于血液样品中卡西酮类毒品的测定。Objective To establish an ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method combined with online solid phase extraction for the simultaneous determination of 12 cathinones in blood samples.Methods The blood samples were first purified by adding acetonitrile.The samples were then centrifuged,diluted,filtered,and loaded on PLRP-S online solid phase extraction column(2.1 mm×12.5 mm,15-20μm)for enrichment and purification.The online solid phase extraction used acetonitrile-5%methanol(volume fraction)as the mobile phase for gradient elution,and the flow rate was 1.0 mL/min.A Poroshell 120 EC-C_(18) column(3.0 mm×150 mm,2.7μm)was used for chromatography separation.5 mmol/L ammonium acetate buffer[containing 0.1%formic acid(volume fraction)]-acetonitrile was used as the mobile phase for gradient elution,with a flow rate of 0.4 mL/min.The mass spectrometer used electrospray ionization source,and multi reaction monitoring mode was used for analysis.Results The linear relationships of 12 cathinones were good,as the correlation coefficients were more than 0.998.The detection limits of the analytes were 0.1-0.5 ng/mL,and the quantitative limits were 0.3-1.5 ng/mL.The recoveries of 12 cathinones at three different concentrations were 70.9%-108%.The intra-day and inter-day precisions were 1.5%-8.9%and 5.1%-44.5%,respectively(n=6).Conclusion The proposed method is simple,convenient,of less sample demand and highly sensitive.It can be used for the determination of cathinones in blood samples.

关 键 词：在线固相萃取 超高效液相色谱-串联质谱法 卡西酮 血液样品 毒物分析 

分 类 号：DF795.4[医药卫生—法医学]