超高效液相色谱-质谱联用法测定人体血清中的金刚烷胺  

Analysis of amantadine in human serum by ultraperformance liquid chromatography tandem mass spectrometry

作　　者：曹杰[1] 王强[2] 郝世轩 宋寅生[1] 蒲彦利[1] 徐虹[1] CAO Jie;WANG Qiang;HAO Shi-xuan;SONG Yin-sheng;PU Yan-li;XU Hong(Zhenjiang Municipal Center for Disease Control and Prevention,Jiangsu Zhenjiang 212004,China;不详)

机构地区：[1]镇江市疾病预防控制中心,江苏镇江212004 [2]江苏大学医学院

出　　处：《江苏预防医学》2022年第5期505-508,共4页Jiangsu Journal of Preventive Medicine

基　　金：2020年度镇江市科技创新资金(重点研发计划—社会发展)项目(SH2020039)。

摘　　要：目的建立人体血清中金刚烷胺的超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法,为人体暴露监测提供可靠的技术支持。方法血清样品经乙腈沉淀后,采用Waters BEH C_(18)色谱柱(2.1 mm×100 mm,1.7μm)分离,以甲醇-0.1%甲酸水溶液为流动相,在电喷雾离子源多反应监测模式下进行检测,采用同位素内标法定量。结果金刚烷胺在质量浓度1.35~1350 ng/ml内线性关系良好,相关系数r为0.9999,方法检出限为0.675 ng/ml,低、中、高3个浓度水平平均回收率为90.8%~105.0%,相对标准偏差(RSD)为2.4%~5.6%。金刚烷胺血清样品短期和长期稳定性良好。金刚烷胺及内标均受基质效应干扰,属于基质抑制。结论建立的方法灵敏、准确、操作简便,符合生物样本测定技术要求,适用于人体血清中金刚烷胺的测定。Objective To establish an ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method for the determination of human serum amantadine;to provide reliable technical support for human exposure surveillance.Methods Serum samples were precipitated with acetonitrile and separated by Waters BEH C_(18) column(2.1 mm×100 mm,1.7μm).Methanol-0.1%formic acid water system was used as mobile phase.Determination was performed under multiple reaction monitoring mode.Quantitative analysis was achieved by internal standard method.Results The linear relationship of amantadine in the mass concentration of 1.35-1350 ng/ml was good,the linear correlation coefficient was 0.9999,the LOD was 0.675 ng/ml,the average recovery rates of three concentration levels(low,medium and high)of amantadine were 90.8%-105%,with RSD of 2.4%-5.6%.Amantadine in serum samples showed good short-term and long-term stability.Amantadine and internal standard content were both interfered by matrix effect by matrix inhibition.Conclusion The established method is sensitive,accurate and simple,satisfying the technical requirements for the determination of biological samples and is suitable for the determination of amantadine in human serum samples.

关 键 词：超高效液相色谱-质谱联用法 金刚烷胺 血清 人体 

分 类 号：R113[医药卫生—公共卫生与预防医学]