HPLC-MS/MS法测定人血浆中人参皂苷Rh_2的浓度  

Determination of ginsenoside-Rh_2 in human plasma by HPLC-MS/MS

作　　者：岳娇 王振磊 李艳玲 夏伯姗 南峰[2] 向瑾[2] 钱广生[1] 秦永平[2] YUE Jiao;WANG Zhen-lei;LI Yan-ling;XIA Bo-shan;NAN Feng;XIANG Jin;QIAN Guang-sheng;QIN Yong-ping(Key Laboratory of Drug-Targeting and Drug Delivery System of the Education Ministry,Sichuan Engineering Laboratory for Plant-Sourced Drug and Sichuan Research Center for Drug Precision Industrial Technology,West China School of Pharmacy,Sichuan University,Chengdu 610041,China;GCP Center/Institute of Drug Clinical Trials,West China Hospital,Chengdu 610041,China;Pharmacy School of Chengdu University of TCM,Chengdu 610075 ,China)

机构地区：[1]靶向药物与释药系统教育部重点实验室(四川大学)四川省植物来源工程实验室和四川省小分子药物精准化工程技术研究中心四川大学华西药学院,成都610041 [2]四川大学华西医院临床药理研究室,成都610041 [3]成都中医药大学药学院,成都610075

出　　处：《中国新药杂志》2019年第10期1214-1220,共7页Chinese Journal of New Drugs

摘　　要：目的:建立了HPLC-MS/MS法测定人体血浆中人参皂苷Rh_2的浓度,并用于人参次苷H滴丸的药动学研究。方法:采用Welch Materials Column XB-C_(18)色谱柱(100 mm×4.6 mm,5μm),以甲醇-水为流动相,流速为0.4 m L·min^(-1),柱温40℃。以阿立哌唑为内标,血浆样本碱化后,以二氯甲烷和乙醚(3∶2,v∶v)萃取,40℃水浴挥干后用流动相复溶进样。采用多反应离子监测,正离子模式扫描,电喷雾离子源。结果:建立的HPLC-MS/MS法在0.5～200 ng·m L^(-1)范围内人参皂苷Rh_2色谱响应与浓度相关性良好,定量下限为0.5 ng·m L^(-1);人参皂苷Rh_2及内标的保留时间分别为14.10和6.61 min;准确度、精密度、回收率和经内标校准后的基质效应均合格;稳定性各项数据均符合相关要求。结论:该法灵敏、专属性强、准确性好,适用于人血浆中人参皂苷Rh_2的浓度测定。Objective:To develop HPLC-MS/MS method for determination of ginsenoside-Rh2 in human plasma to study pharmacokinetics of Ginsenoside H drop pill in human.Methods:The analysis was carried on the reverse column Welch Material XB-C18(100 mm×4.6 mm,5μm).The mobile phase consisting of a mixture of methanol:water was delivered at a flow rate of 0.4 mL·min-1with the column temperature maintained at 40℃.Aripiprazole was chosen as the internal standard.Plasma samples were extracted by a mixture of dichloromethane:diethyl ether(3∶2,v∶v)after alkalinized.The extraction solution was evaporated to dryness under a gentle stream of water at 40℃.The residue was resolved in mobile phase before injection.An electron spray ionization(ESI)was applied and operated in the positive multiple reaction monitoring(MRM)mode.Positive ion mode was scanned.Results:The established HPLC-MS/MS method showed a good correlation between the chromatographic response of ginsenoside-Rh2 and its concentration in the range of 0.5~200 ng·m L^-1,the low limit of quantification was 0.5 ng·m L^-1.The retention time of ginsenoside-Rh2 and its internal standard in plasma were 14.10 and 6.61 min.The accuracy,precision,pretreatment recovery and matrix effect calibrated by internal standard were qualified.The results of stability test all meet the relevant requirements.Conclusion:This method is sensitive,specific and accurate for the determination of ginsenoside-Rh2 in human plasma.

关 键 词：液相色谱-质谱/质谱法 人参次苷H滴丸 人参皂苷RH2 药动学 

分 类 号：R927.2[医药卫生—药学]