血液中硫化氢的LC-MS/MS法检验
Determination of hydrogen sulfide in Blood by LC-MS/MS
吴小军 1秦歌 2魏春明 1赵鹏 1李佳宜 1常靖 1张云峰1
作者信息
- 1. 公安部鉴定中心,北京 100038
- 2. 公安部鉴定中心,北京 100038;中国人民公安大学侦查学院,北京 100038
- 折叠
摘要
目的 建立一种用于测定血液中硫化氢的方法,并将其应用于实际案例中.方法 取0.2 mL血液样品,并加入0.8mL饱和硼砂溶液进行稀释.在试管中取1mL含有0.1％甲酸的乙腈溶液,依次加入0.1mL稀释液和0.1 mL1％三嗪水溶液.混合均匀后,静置30min.之后,通过离心和膜过滤,样品供LC-MS/MS分析.结果 在10～2 000 ng/mL浓度范围内,硫化氢呈良好的线性关系,R2为0.998 5.检出限为5 ng/mL,定量下限为10 ng/mL.在3例硫化氢中毒案例中,检测出3名死者血液中存在硫离子,浓度在0.17～0.56 μg/mL之间.结论 本研究首次建立了用于测定血液中硫化氢的LC-MS/MS方法,可满足硫化氢中毒案件的检测需求.
Abstract
Objective To establish a method for determining hydrogen sulfide(H2S)in blood and apply it to practical cases.Methods A delute solution was achieved by adding 0.8 mL saturated borax solution into 0.2 mL blood sample was diluted with.1 mL acetonitrile solution containing 0.1％formic acid was then taken in a test tube,followed by adding 0.1 mL dilute solution and 0.1 mL thiozine aqueous solution(1％).After thorough mixing,the mixture was left to stand for 30 minutes.Subsequently,the sample was subjected to liquid chromatography-tandem mass spectrometry(LC-MS/MS)analysis after centrifugation and membrane filtration.Results The results showed that H2S exhibited good linearity within the concentration range of 10～2 000 ng/mL,with the R2 value of 0.998 5.The detection limit was 5 ng/mL,and the quantification limit was 10 ng/mL.In three cases of H2S poisoning,sulfur ions were detected in the blood of the deceased individuals,with concentrations ranging from 0.17 to 0.56 μg/mL.Conclusion For the first time,this study established a LC-MS/MS method for determining H2S in blood,which can meet the detection needs of H2S poisoning cases.
关键词
血液/H2S/LC-MS/MS/气体毒物/法医毒物Key words
Blood/H2S/LC-MS/MS/Gaseous poison/Forensic toxicology引用本文复制引用
基金项目
中央级公益性科研院所基本科研业务费专项(2023jb008)
出版年
2024
NETL
NSTL
万方数据