在线固相萃取净化-高效液相色谱法测定人血浆中的霉酚酸  

Determination of Mycophenolic Acid in Human Plasma by High Performance Liquid Chromatography with Online Solid Phase Extraction Purification

作　　者：许泽君[1] 景霞[1] 孙芳[1] 吉超 杨新磊[2] XU Ze-jun;JING Xia;SUN Fang;JI Chao;YANG Xin-lei(Children's Hospital of Nanjing Medical University,Nanjing 210008,China;Agilent Technologies(China)Co.,Ltd,Shanghai 200080,China)

机构地区：[1]南京医科大学附属儿童医院,江苏南京210008 [2]安捷伦科技(中国)有限公司,上海200080

出　　处：《分析测试学报》2020年第1期162-166,共5页Journal of Instrumental Analysis

基　　金：江苏省药学会-奥赛康医院药学基金科研项目(A201810);南京市药学会-常州四药医院药学科研基金(2019YX003).

摘　　要：建立了在线固相萃取净化-高效液相色谱法联用(Online SPE-HPLC)测定人血浆中霉酚酸浓度的分析方法。联用系统以Capcell PAK MF Ph-1为净化柱,Poroshell 120?EC-C18为分析柱,血浆样品经甲醇沉淀蛋白后,直接进样分析。结果表明,霉酚酸在0.20~50.00μg/mL范围内线性关系良好,相关系数(r)为0.9998,检出限和定量下限分别为0.07、0.20μg/mL。在0.39、25.00、50.00μg/mL 3个质量浓度下的平均回收率为96.2%~105%,日内和日间相对标准偏差(RSD)分别为2.6%~3.1%和2.9%~3.3%。该法操作简便、快速,可用于人血浆中霉酚酸浓度的分析。An online solid phase extraction-high performance liquid chromatographic(Online SPE-HPLC)method was developed for the determination of mycophenolic acid in human plasma.Plasma samples were directly injected into the online SPE-HPLC system after simple protein precipitation.Capcell PAK MF Ph-1 was employed as an online SPE column and Poroshell 120?EC-C18 was employed as an analysis column.Results showed that there was a good linear relationship for mycophenolic acid in the concentration range of 0.20-50.00μg/mL,with a correlation coefficient(r)of 0.9998.The limit of detection(LOD)and limit of quantitation(LOQ)were of 0.07μg/mL and 0.20μg/mL,respectively.The spiked recoveries for mycophenolic acid in human plasma at three spiked levels of 0.39,25.00 and 50.00μg/mL ranged from 96.2%to 105%,with intra-assay relative standard deviations(intra-RSD)of 2.6%-3.1%and inter-assay relative standard deriation(inter-RSD)of 2.9%-3.3%.The method was rapid and simple,and was suitable for the determination of mycophenolic acid concentrations in human plasma.

关 键 词：霉酚酸 血浆 在线固相萃取-高效液相色谱法(Online SPE-HPLC) 

分 类 号：O657.63[理学—分析化学] TQ460.72[理学—化学]