HPLC-MS/MS法测定大鼠血浆中黑骨藤的3个指标成分及其药动学研究  

Pharmacokinetics of 3 index components from Periploca forrestii Schltr in rat plasma by HPLC-MS/MS

作　　者：王昌权[1,2] 夏涛 覃小丽 李奎 王爱民 黄勇[1] 李月婷[1] 巩仔鹏[1] 陈思颖[1] 郑林[1] WANG Chang-quan;XIA Tao;QIN Xiao-li;LI Kui;WANG Ai-min;HUANG Yong;LI Yue-ting;GONG Zi-peng;CHEN Si-ying;ZHENG Lin(Guizhou Medical University Guizhou Provincial Key Laboratory of Pharmaceutics/State Key Laboratory of Functions and Applications of Medicinal Plants,Guiyang 550004,China;Guizhou Medical University Engineering Research Center for the Development and Application of Ethnic Medicine and TCM,Ministry of Education,Guiyang 550004,China;Guizhou Medical University School of Pharmacy,Guiyang 550004,China)

机构地区：[1]贵州医科大学贵州省药物制剂重点实验室/药用植物功效与利用国家重点实验室,贵阳550004 [2]贵州医科大学药学院,贵阳550004 [3]贵州医科大学民族药与中药开发应用教育部工程研究中心,贵阳550004

出　　处：《中国新药杂志》2020年第17期2021-2026,共6页Chinese Journal of New Drugs

基　　金：国家自然科学基金资助项目(81660691,U1812403);贵州省科技计划项目(黔科合平台人才[2019]5660,[2017]5601);中央引导地方科技专项项目(黔科中引地[2018]4006);贵阳市科研创新团队项目(筑科合同[2017]30-29号);贵州省大学生创新创业训练计划项目(2018520335)。

摘　　要：目的:建立高效液相色谱-串联质谱(HPLC-MS/MS)法测定大鼠灌胃黑骨藤提取物后血浆中活性成分3-O-咖啡酰基奎宁酸、4-O-咖啡酰基奎宁酸和5-O-咖啡酰基奎宁酸的分析方法,并用该方法研究3-O-咖啡酰基奎宁酸等3个指标成分的药动学特征。方法:血浆样品处理选择酸化后甲醇沉淀蛋白,ACE C18-PFP(150 mm×4.6 mm,3μm),流速:0.6 mL·min^-1,柱温:40℃,进样器温度:15℃,流动相:0.1%甲酸乙腈(B)-0.1%甲酸水(A)梯度洗脱,进样体积:1μL,采用电喷雾电离源(ESI-),扫描方式为选择二级离子监测。结果:3个指标成分分别在1.09~1114.00,1.00~1086.00,0.98~1024.00 ng·mL^-1呈良好线性关系,提取回收率、精密度、准确度和稳定性均良好达到测定要求。3-O-咖啡酰基奎宁酸、4-O-咖啡酰基奎宁酸和5-O-咖啡酰基奎宁酸3个指标成分的Tmax分别为(1.22±0.55),(0.93±0.45)和(0.81±0.56)h,Cmax分别为(151.01±28.75),(83.84±14.71和(78.686±3.27)ng·mL^-1。结论:建立的HPLC-MS/MS检测方法具有特异、快速、准确和灵敏的特点,能够同时测定生物样品中3-O-咖啡酰基奎宁酸等3个指标成分的血药浓度,并成功应用于黑骨藤在正常大鼠体内这3个指标成分的药动学研究。Objective:To establish a HPLC-MS/MS method for determining 3-O-caffeoyl-quinic acid,4-O-caffeoylquinic acid and 5-O-caffeoylquinic acid and to investigate the pharmacokinetics profile of the 3 index components from the extract of Periploca forrestii Schltr in rat plasma.Methods:The analysis was achieved by an ACE C18-PFP column(150 mm×4.6 mm,3μm)with a mobile phase composed of 0.1%formic acid using step gradient elution at a flow rate of 0.6 mL·min^-1,column temperature of 40℃,sample injector temperature of 15℃,and sample volume of 1μL.A tandem mass spectrometry equipped with electrospray ionization source in selected ion recording mode was used as the detector.Results:In the selected linear range,calibration curves of the 3 marker components showed good linearity.Extraction recovery rate,precision,accuracy and stability reached the determination request.The parameters of Tmax of the three index components were(1.22±0.55),(0.93±0.45)and(0.81±0.56)h,respectively,and Cmax were(151.01±28.75),(83.84±14.71)and(78.686±3.27)ng·mL^-1,respectively.Conclusion:The fully validated HPLC-MS/MS method has been successfully applied to the pharmacokinetic study of the 3 index components from Periploca forrestii Schltr in rat plasma.

关 键 词：黑骨藤 高效液相色谱-串联质谱法 3-O-咖啡酰基奎宁酸 4-O-咖啡酰基奎宁酸 5-O-咖啡酰基奎宁酸 

分 类 号：R965[医药卫生—药理学]