金匮肾气丸中马钱苷、京尼平苷酸、23-乙酰泽泻醇B和β-蜕皮甾酮含量测定方法的建立  

Establishment of a method for the determination of loganin,geniposide,23-acetylalisol B andβ-ecdysterone in Jinkui Shenqi Pills

作　　者：王开裕[1] 林天东[2] 吴振宁 许海丹 WANG Kaiyu;LIN Tiandong;WU Zhenning;XU Haidan(Department of Pharmacy,Hainan Provincial Hospital of Traditional Chinese Medicine,Hhaikou 570203,China;Chinese Medicine Master Workshop,Hainan Provincial Hospital of Traditional Chinese Medicine,Haikou 570203,China)

机构地区：[1]海南省中医院药学部,海口570203 [2]海南省中医院国医大师工作室,海口570203

出　　处：《西北药学杂志》2023年第5期48-52,共5页Northwest Pharmaceutical Journal

摘　　要：目的建立高效液相色谱法(high performance liquid chromatography,HPLC)测定金匮肾气丸中马钱苷、京尼平苷酸、23-乙酰泽泻醇B和β-蜕皮甾酮的含量。方法将金匮肾气丸样品研细、甲醇超声提取后,用Capcell Pak UG C_(18)色谱柱分离,柱温为28℃,京尼平苷酸、β-蜕皮甾酮、马钱苷和23-乙酰泽泻醇B检测波长分别设定为254、250、240、254 nm,进样体积为10μL,流速为1.0 mL·min^(-1),以乙腈为流动相A、3 mL·L^(-1)磷酸溶液为流动相B,梯度洗脱,外标法定量检测。结果京尼平苷酸、β-蜕皮甾酮、马钱苷和23-乙酰泽泻醇B质量浓度分别在0.0495~4.95、0.0981~9.81、0.0197~1.97、0.0983~9.83μg·mL^(-1)范围内具有良好的线性关系;重复性RSD值(n=6)分别为1.62%、1.31%、1.76%、1.24%;平均加样回收率分别为100.05%、98.33%、99.97%、99.42%。结论该方法具有前处理简单、分析时间短、检测结果准确等优点,适用于金匮肾气丸的质量控制。Objective To develop an analytical method for the determination of loganin,geniposide acid,23-acetylalisol B andβ-ecdysterone in Jinkui Shenqi Pills by high performance liquid chromatography(HPLC).Methods The sample of Jinkui Shenqi Pills was porphyrized and extracted by methanol ultrasound,and then separated by Capcell Pak UG C_(18)chromatographic column.The column temperature was set at 28℃.The detection wavelengths of geniposide acid,β-ecdysterone,loganin and 23-acetylalisol B were set at 254,250,240 and 254 nm,respectively,and the injection volume was 10μL.The flow rate was 1.0 mL·min^(-1),acetonitrile as mobile phase A,and 3 mL·L^(-1)phosphoric acid solution as mobile phase B,in a gradient elution mode.External standard method was used for quantitation.Results Geniposide acid,β-ecdysterone,loganin and 23-acetylalisol B showed good linear relationships in the ranges of 0.0495-4.95,0.0981-9.81,0.0197-1.97 and 0.0983-9.83μg·mL^(-1),respectively.The repeatability RSDs(n=6)were 1.62%,1.31%,1.76%and 1.24%,respectively.The average recoveries were 100.05%,98.33%,99.97%and 99.42%respectively.Conclusion This method has the advantages of simple pretreatment,short analysis time and accurate detection results,and is suitable for the quality control of Jinkui Shenqi Pills.

关 键 词：高效液相色谱法 金匮肾气丸 马钱苷 京尼平苷酸 β-蜕皮甾酮 

分 类 号：R927.2[医药卫生—药学]