基于UPLC-MS/MS技术测定大鼠血浆中的氨甲环酸  

Determination of tranexamic acid in rat plasma by UPLC-MS/MS

作　　者：王雪[1,2] 杨玉婷 赵立春 廉洁 赵小峪[1] 高学旺 高云华 张锁慧[1,4] WANG Xue;YANG Yuting;ZHAO Lichun;LIAN Jie;ZHAO Xiaoyu;GAO Xuewang;GAO Yunhua;ZHANG Suohui(Technical Institute of Physics and Chemistry Chinese Academy of Sciences,Beijing 100190,China;Guangxi University of Chinese Medicine,Nanning 530200,Guangxi,China;People s Public Security University of China,Beijing 100038,China;Beijing CAS Microneedle Technology Ltd,Beijing 102600,China)

机构地区：[1]中国科学院理化技术研究所,北京100190 [2]广西中医药大学药学院,广西南宁530200 [3]中国人民公安大学,北京100038 [4]中科微针(北京)科技有限公司,北京102600

出　　处：《化学研究》2022年第3期236-244,共9页Chemical Research

基　　金：国家重点研发计划(项目号2016YFC1000902);中国科学院STS计划(项目号KFJ-STS-QYZD-182)资助项目。

摘　　要：基于UPLC-MS/MS技术建立了大鼠血浆中氨甲环酸定量分析方法,探讨了不同血浆样品处理方法对方法灵敏度、基质效应的影响,考察了溶剂效应对色谱峰型的影响。选择以顺式-4-氨基环己烷羧酸为内标(Internal standard,I.S.),色谱柱为Nano ChromcoreHilic-Amide柱(150 mm×2.1 mm,3μm),流动相为10 mmol/L甲酸铵(pH 3.8)-乙腈(95∶5,体积比)等度洗脱,采用ESI+离子源、Targeted-MS^(2)扫描模式对血浆样品中氨甲环酸进行定量分析。氨甲环酸在0.2~70 mg/L范围内线性关系良好(R^(2)=0.9996),氨甲环酸日内、日间精密度为0.55%~5.42%,提取回收率为(83.90±12.6)%~(110.20±3.3)%,氨甲环酸的基质效应在(82.16±15.5)%~(86.47±5.6)%之间。建立的超高效液相色谱-质谱联用方法快速灵敏,重现性好,可用于氨甲环酸在大鼠体内药代动力学研究。A method for the quantitative analysis of tranexamic acid in rat plasma was established based on UPLC-MS/MS technique.The effects of different plasma sample treatments on the method sensitivity and matrix effects were investigated,and the effects of solvent effects on the chromatographic peak patterns were examined.Cis-4-aminoc-yclohexanecarboxylic acid was used as internal standard.The chromatographic column was a Nano ChromcoreHilic-Amide column(150 mm×2.1 mm,3μm)with a mobile phase of 10 mmol/L ammonium formate(pH 3.8)-acetonitrile(95∶5,volume ratio)isocratic elution,and quantitative analysis of tranexamic acid in plasma samples was performed using ESI+ion source and Targeted MS^(2) scanning mode.The results exhibited a good linearity over a range of 0.2-70 mg/L(R^(2)=0.9996).Intra-and inter-day precision was 0.55%-5.42%,the matrix effect of propranolol ranged(82.16±15.5)%-(86.47±5.6)%.The recoveries of TA was(83.90±12.6)%~(110.20±3.3)%.The established ultra-performance liquid chromatography-mass spectrometry method is rapid,sensitive and reproducible,which can be used to study the pharmacokinetics of tranexamic acid in rats.

关 键 词：氨甲环酸 黄褐斑 药代动力学 超高效液相色谱-单四极杆-静电场轨道阱串联质谱 

分 类 号：R917[医药卫生—药物分析学]