摘要
本文旨在建立一种基于超高效液相色谱-串联质谱(UPLC-MS/MS)检测全血中的东莨菪碱和阿托品的快速检验方法。全血样品经乙腈沉淀蛋白,振荡、离心提取后,上清液过0.22μm有机滤膜,上机检测。UPLC-MS/MS检测方法选用Agilent Eclipse Plus C_(18)色谱柱,以0.1%甲酸水溶液-乙腈为流动相,进行梯度洗脱,流速为0.4mL/min。东莨菪碱和阿托品在1~100ng/mL范围内线性良好,线性系数分别为0.9997、0.9968,平均回收率分别为93.99%、97.71%,日内与日间精密度均小于10%。东莨菪碱与阿托品的最低检出限(LOD S/N=3)均为0.2ng/mL,最低定量限(LOQ S/N=10)均为1ng/mL。该方法快速简便,灵敏度高,可用于人全血中东莨菪碱与阿托品的定性定量检测。
A novel and rapid method was established for the determination of scopolamine and atropine in human blood by ultra-performance liquid chromatography-mass spectrometry（UPLC-MS/MS）.Human blood samples were precipitated with acetonitrile,vibrated and centrifugated.The obtained supernatant was filtered with a 0.22 μm organic membrane for detection.Gradient elution was conducted on an Agilent Eclipse Plus C18 column.The mobile phase,consisted of 0.1%formic acid aqueous solution and acetonitrile,was flowing at a rate of 0.4 mL/min.The column oven was maintained at40 °C.The detection for scopolamine and atropine was linear from 1 to 100 ng/mL with their linear coefficients of 0.9997 and 0.9968.Precision and accuracy were acceptable at any quality control level and the respective average recoveries were93.99%and 97.71%.The limits of detection（LOD S/N = 3） of scopolamine and atropine were all 0.2 ng/mL.The lowest limit of quantification（LOQ S/N = 10） was 1 ng/mL.The method is sensitive,very fast,easy to perform,and cheap as it only requires deproteinization of blood sample with acetonitrile,therefore suitable to be used for identification and quantification of scopolamine and atropine in human whole blood.
出处
《刑事技术》
2017年第2期133-136,共4页
Forensic Science and Technology
基金
国家自然科学基金项目(81273346)
关键词
东莨菪碱
阿托品
液相色谱-质谱联用
快速检验
scopolamine
atropine
liquid chromatography-mass spectrometry
rapid detection
