参芪益气固本片中皂苷类成分的UPLC-MS测定  

Quantitative Determination of Six Active Ingredients in Shenqi Yiqi Guben Tablet by UPLC-MS

作　　者：安军永[1] 王世华[1] 李云鹏[1] 周梦夏[1] 刘翠[1] 张晓风[1] 李向军[1] 

机构地区：[1]石家庄以岭药业股份有限公司,石家庄050035

出　　处：《中国实验方剂学杂志》2015年第2期99-102,共4页Chinese Journal of Experimental Traditional Medical Formulae

摘　　要：目的：建立了参芪益气固本片中6种有效成分的UPLC-MS定量方法.方法：采用C18色谱柱,以乙腈-0.1％甲酸水为流动相梯度洗脱,流速0.5 mL· min^-1,采用负离子模式检测,源喷雾电压（IS）-5 000 V,辅助加热气温度450℃,雾化气50 psi,辅助气40 psi,气帘气30 psi,解簇电压-55 V,采集方法TOF-MS/MS.结果：6种成分芍药苷,人参皂苷Re,人参皂苷Rg1,连翘苷,人参皂苷Rb1,黄芪甲苷在检测的范围内线性良好,r均大于0.999,方法回收率为98％～102％,RSD均小于4.5％.结论：采用本方法测定参芪益气固本中的6种成分方法准确度高、仪器精密度良好,可以用于该制剂的质量控制方法,同时本文使用了UPLC-MS方法,与传统的HPLC-MS比较,具有提高分离度、降低药品的生产成本,可以为其他含有该成分的中成药制剂制定标准提供参考.Objective：To established an UPLC-MS method for quantitative determination of six active ingredients in Shenqi Yiqi Guben tablet.Method：The UPLC separation was carried out with an Acquility UPLC BEH C18 （2.1 mm × 100 mm,1.7 μm） using gradient elution with a mobile phase consisting of acetonitrile-water （included 0.1% formic acid） at a constant flow rate of 0.5 mL ·min ^-1 The MS detector set as follows：negative ion mode detection,source spray voltage （IS）-5 000 V,auxiliary heating gas temperature 450 ℃,atomization gas 50 psi,auxiliary gas 40 psi,curtain gas 30 psi,deaggregation voltage-55 V,collection methods TOF-MS/ MS.Result：Six components：paeoniflorin,ginsenoside Re,ginsenoside Rg1,forsythin,ginsenosides Rb1,and astragaloside were in a good linearity,r greater than 0.999,recoveries were 98%-102%,RSD were less than 4.5%.Conclusion：The established method for the determination of the six components of Shenqi Yiqi Guben tablet is accuracy and precision that can be used for quality control of the preparation.The UPLC-MS method can increased resolution,lower production costs of drugs compared with HPLC-MS.It provides a reference to set standards for other Chinese medicine formulations containing these ingredients.

关 键 词：超高液相色谱-质谱联用 参芪益气固本片 芍药苷 人参皂苷RE 人参皂苷Rg1 连翘苷 人参皂苷Rb1 黄芪甲苷 

分 类 号：R284.1[医药卫生—中药学]