UPLC-MS/MS检测全血中13种麻痹性贝类毒素  

Detection of 13 Paralytic shellfish toxins in human whole blood by high-performance liquid chromatography-tandem mass spectrometry

作　　者：马秀琴 接强 栾玉静 王泽宇 王芳琳 Ma Xiuqin;Jie Qiang;Luan Yujing;Wang Zeyu;Wang Fanglin(l.School of Forensic Medicine,Shanxi Medical University,030600,Shanxi,China;Institute of Forensic Science Ministry of Public Security,100038,Beijing,China)

机构地区：[1]山西医科大学,山西晋中030600 [2]公安部鉴定中心,北京100038

出　　处：《中国法医学杂志》2024年第4期458-461,466,共5页Chinese Journal of Forensic Medicine

基　　金：公安部技术研究计划(2021jsz16);法庭科学领域食药环检验技术标准体系研究(2020JB007)。

摘　　要：目的 建立全血中13种麻痹性贝类毒素(PSTs)的超高效液相色谱-串联质谱(UPLC-MS/MS)的检测方法。方法 用1%乙酸︰乙腈(1︰3,v︰v)溶液提取全血中的13种PSTs,采用UPLC BEH Amide色谱柱(100mm×2.1 mm,1.7μm)分离,电喷雾(ESI)正、负离子多反应监测(MRM)模式检测,基质匹配曲线外标法定量。结果 13种PSTs在1~100 ng/mL质量浓度范围内线性关系良好,相关系数(r~2)>0.995,检出限为0.5~2 ng/mL,定量限为1~4 ng/mL,回收率为65.55%~114.12%。结论 本方法灵敏度高,具有良好的重现性,可以准确定性定量13种PSTs,适用于全血中PSTs的快速检测。Objective To establish the analysis method of 13 Paralytic shellfish toxins(PSTs)in human whole blood by high-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Methods 13 kinds of PSTs were extracted from the whole blood using acetonitrile with 1%acetate(1︰3,v︰v)solution,and separated by UPLC BEH Amide chromatographic column(100mm×2.1mm,1.7μm).The samples were detected by an electrospray ionization source(ESI)and positive and negative ion multiple reaction monitoring(MRM)mode,and quantified by matrix matching curve external standard method.Results The results showed that 13 kinds of PSTs in blood samples were linear well in the ranges of 1~100 ng/mL,with the correlation coefficient(r2)>0.995.The limit of detection(LODs)of the method were 0.5~2 ng/mL,the limit of quantitation(LOQs)were 1~4 ng/mL,and the recoveries of the method were 65.55%~114.12%.Conclusion The method is highly sensitive,reproducible,and can qualify and quantify thirteen toxins at the same time,which is suitable for the rapid detection of PSTs in whole blood samples.

关 键 词：法医毒物分析 全血 超高效液相色谱-串联质谱 麻痹性贝类毒素 

分 类 号：D918.93[政治法律—法学]