高效液相色谱法检测七味都气丸中活性成分五味子醇甲、马钱苷和23-乙酰泽泻醇B的含量  

Determination of contents of active ingredients of schisandrin,loganin and 23-acetyl alisol B in Qiweiduqi pills by HPLC

作　　者：张宪[1] ZHANG Xian(Beijing Institute for Drug Control,Beijing Key Laboratory of Analysis and Evaluation on Chinese Medicine,Beijing 102206,China)

机构地区：[1]北京市药品检验所中药成分分析与生物评价北京市重点实验室,北京102206

出　　处：《安徽医药》2022年第10期1933-1936,共4页Anhui Medical and Pharmaceutical Journal

摘　　要：目的研究建立采用高效液相色谱法检测七味都气丸中活性成分五味子醇甲、马钱苷和23-乙酰泽泻醇B含量的分析方法。方法研究起止时间为2019年3月至2022年5月。七味都气丸样品经粉碎,90%甲醇水溶液超声提取后,采用Waters X-bridge C_(18)色谱柱分离,柱温27℃,检测波长228 nm,进样体积25µL,流动包括流动相A(乙腈),流动相B(0.3%磷酸水溶液),梯度洗脱,洗脱程序为0~7 min 8%A,7~18 min 8%~60%A,18~28 min 60%~91%A,28~30 min 91%~8%A,30~35min 8%A,外标法定量检测。结果马钱苷、五味子醇甲和23-乙酰泽泻醇B在质量浓度0.1~20.0 mg/L范围内具有良好的线性关系,相关系数(r)均大于0.995;重复性RSD(n=6)分别为2.7%、3.1%和3.4%;加样回收率分别为99.67%、100.11%和100.49%。结论该方法具有简便、快速、准确度好等优点,适用于七味都气丸品种的质量控制。Objective To develop an analytical method for determinating contents of active ingredients of schisandrin,loganin and 23-acetyl alisol B in Qiweiduqi pills by high performance liquidchromatography(HPLC).Method The study starts and ends from March 2019 to may 2022.After Qiweiduqi pill samples were crushed and ultrasonic extracted with 90%methanol solution,Waters Xbridge C_(18) column was selected for separation,with column temperature of 27℃.Detection wavelength was set at 228 nm,injection volume was 25µL.Mobile phase,acetonitrile(A)and 0.3%phosphoric acid solution(B).Gradient elution procedure was as follows,0-7 min 8%A,7-18 min 8%-60%A,18-28 min 60%-91%A,28-30 min 91%-8%A,30-35min 8%A.Quantitative analysis was performed by external standard.Result Schisandrin,loganin and 23-acetyl alisol B showed good linear relationships in the concentration range of 0.1 to 20.0 mg/L,the correlation coefficients(r)were all greater than 0.995.Relative standard deviation(RSD)of repeatability was 2.7%、3.1%and 3.4%,respectively.Average recoveries of 3 active components were 101.26%,101.12%and 99.55%.Conclusions This method has the characteristics of simple pretreatment,high efficiency and accurate results and can be used for the quality control of Qiweiduqi pills.

关 键 词：主成分分析 色谱法 高压液相 七味都气丸 五味子醇甲 马钱苷 23-乙酰泽泻醇B 

分 类 号：R286.0[医药卫生—中药学] O657.72[医药卫生—中医学]