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
马秀琴 1接强 2栾玉静 2王泽宇 1王芳琳2
作者信息
- 1. 山西医科大学,山西晋中 030600
- 2. 公安部鉴定中心,北京 100038
- 折叠
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(100 mm×2.1 mm,1.7 μm)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(r2)>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.
Abstract
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Key words
Forensic toxicological analysis/Blood/UPLC-MS/MS/Paralytic shellfish toxins引用本文复制引用
基金项目
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)
出版年
2024
NETL
NSTL
万方数据