高效液相色谱串联电喷雾检测器一测多评法同时测定当归丸中5种皂苷类成分  

Simultaneous determination of 5 saponins in Danggui Pills with quantitative analysis of multi-component by single marker by high performance liquid chromatography coupled with charged aerosol detector

作　　者：郭润芳 李瑞燕[2] 李建伟[2] Guo Runfang;Li Ruiyan;Li Jianwei(Changzhi City Luzhou District Maternal and Child Health Planning Service Center,Changzhi Shanxi 046011;Department ofPharmacy,Changzhi Medical College,Changzhi Shanxi 046013)

机构地区：[1]长治市潞州区妇幼保健计划生育服务中心,山西长治046011 [2]长治医学院药学系,山西长治046013

出　　处：《山西中医药大学学报》2023年第6期631-635,共5页Journal of Shanxi University of Chinese Medicine

基　　金：山西省重点实验室项目(202104010910002)。

摘　　要：目的:建立高效液相色谱串联电喷雾检测器一测多评法(HPLC-CAD-QAMS),同时测定当归丸中5种成分黄芪皂苷Ⅱ、黄芪皂苷IV、异黄芪皂苷Ⅱ、黄芪皂苷Ⅰ、异黄芪皂苷Ⅰ的含量。方法:采用电雾式检测器(CAD),将漂移管的温度调节至50℃,并将气体的流速调节至50 psi;Agilent SB-C18(150 mm×4.6 mm,3.5μm)色谱柱,将A相和B相分别设置为0.1%的甲酸和乙腈,并将流速调节至1.5 ml/min,同时将进样量调节至20μl,最后将柱温调节至40℃。建立黄芪皂苷Ⅱ与黄芪皂苷IV、异黄芪皂苷Ⅱ等4个皂苷成分的相对校正因子(RCF),用RCF计算各指标成分含量,并验证一测多评法(QAMS)的准确度和重复性。结果:色谱峰分离度良好,黄芪皂苷Ⅱ、黄芪皂苷IV、异黄芪皂苷Ⅱ、黄芪皂苷Ⅰ、异黄芪皂苷Ⅰ的线性范围分别为7.5~150μg/ml、8.2~164μg/ml、8.3~16.6μg/ml、7.8~156μg/ml、9.8~245μg/ml,平均加样回收率分别为98.1%、98.7%、99.3%、98.6%、99.2%,RSD分别为1.13%、1.66%、0.97%、1.03%、1.01%。黄芪皂苷Ⅱ设定为内参物,对黄芪皂苷IV、异黄芪皂苷Ⅱ、黄芪皂苷Ⅰ、异黄芪皂苷Ⅰ的相对校正因子分别为0.822、0.549、0.287、0.786,建立的一测多评法检测方法、结果可靠。结论:建立的HPLC-CAD-QAMS法简便、准确,同时测定当归丸中5个指标成分,可用于当归丸的多指标成分质量控制,为当归丸的质量标准研究提供参考。Objective:To establish quantitative analysis of multi-component by single marker by high performance liquid chromatography coupled with charged aerosol detector(HPLC-CAD-QAMS) for the simultaneous determination of astragaloside II,astragaloside IV,isoastragaloside II,astragaloside I and isoastragaloside I in Danggui Pills.Methods:The charged aerosol detector(CAD) was used to adjust the temperature of the drift tube to 50℃ and the gas flow rate to 50 psi.Agilent SBC18(150 mm×4.6 mm,3.5 μm) column was used to set the A phase and B phase to 0.1% formic acid and acetonitrile,respectively.The flow rate was adjusted to 1.5 ml/min,and the sample size was adjusted to 20 μl.Finally,the column temperature was adjusted to 40℃.Relative correction factors(RCF) for four saponins including astragaloside II,astragaloside IV,and isoastragaloside II were established.RCF was used to calculate the content of each index component,and the accuracy and repeatability of QAMS were verified.Results:Chromatographic peak separation was good.The linearity ranges of astragaloside II,astragaloside IV,isoastragaloside II,astragaloside I and isoastragaloside I were 7.5-150 μg/ml,8.2-164 μg/ml,8.3-16.6μg/ml,7.8-156 μg/ml,and 9.8-245 μg/ml,respectively.The average sample recoveries were 98.1%,98.7%,99.3%,98.6%,and 99.2%,and RSD were 1.13%,1.66%,0.97%,1.03%,and 1.01%,respectively.When astragaloside II was set as the internal reference,the RCFs for astragaloside IV,isoastragaloside II,astragaloside I and isoastragaloside I were 0.822,0.549,0.287,and 0.786,respectively.The results of QAMS were simple and reliable.Conclusion:The established HPLC-CAD-QAMS method is simple and accurate.The simultaneous determination of 5 index components in Danggui Pills can be used for quality control of multi-index components of Danggui Pills,and provide reference for quality standard research of Danggui Pills.

关 键 词：当归丸 黄芪皂苷Ⅱ 黄芪皂苷IV 异黄芪皂苷Ⅱ 黄芪皂苷Ⅰ 异黄芪皂苷Ⅰ 一测多评 HPLC-CAD 

分 类 号：R286[医药卫生—中药学] O657.2[医药卫生—中医学]