HPLC-一测多评法测定参葛补肾胶囊中总黄酮醇苷的含量  

Simultaneous Determination of Total Flavonol Glycosides in Shenge Bushen Capsule by HPLC-QAMS

作　　者：李成功 胡时先 任宾 潘树球 徐海燕 王涵斌 郝娟 LI Cheng-gong;HU Shi-xian;REN Bin;XU Hai-yan;PAN Shu-qiu;WANG Han-bin;HAO Juan(Xinjiang Huachun Biopharmaceutical Co.,Ltd.,Xinjiang Urumqi 830000,China;Sinopharm Dezhong(Foshan)Pharmaceutical Co.,Ltd.,Guangdong Foshan 528000,China)

机构地区：[1]新疆华春生物药业股份有限公司,新疆乌鲁木齐830000 [2]国药集团德众(佛山)药业有限公司,广东佛山528000

出　　处：《中国药物评价》2024年第3期198-203,共6页Chinese Journal of Drug Evaluation

基　　金：国家重大新药创制科技重大专项资助(2018ZX09731020)。

摘　　要：目的:建立参葛补肾胶囊中淫羊藿苷、朝藿定A、朝藿定B、朝藿定C含量的HPLC测定方法。方法:采用高效液相色谱法,色谱柱为Waters ACQUITY UPLC HSS T3 C 18(2.1×100 mm,1.8μm),流动相为乙腈-0.05%磷酸水溶液体系,梯度洗脱,流速为0.3 mL·min^(-1),检测波长为320 nm,柱温为30℃,进样量为2μL。以淫羊藿苷为内参物,采用斜率校正法计算其他3个成分的相对校正因子,比较外标法和一测多评法(QAMS)测定结果,验证一测多评法的可行性及准确性。结果:淫羊藿苷、朝藿定A、朝藿定B、朝藿定C分别在7.130~713.38μg·mL^(-1)、1.284~128.4μg·mL^(-1)、5.108~510.8μg·mL^(-1)、4.360~435.67μg·mL^(-1)质量浓度范围内存在良好的线性关系,线性系数R 2均大于0.99,平均加样回收率分别为104.5%、99.69%、100%、98.59%,RSD分别为1.4%、2.7%、1.2%、2.8%。朝藿定A、朝藿定B、朝藿定C的相对校正因子为1.31、1.19、1.17。一测多评法和外标法测定结果比较,其差异无统计学意义(P>0.05)。结论:该方法准确、简便、重复性好,可作为参葛补肾胶囊中淫羊藿总黄酮醇苷的质量控制研究。Objective:To develop a HPLC method for determination of icariin,epimedin A,epimedin B,epimedin C in Shenge Bushen capsule.Methods:The chromatographic was performed on a Waters ACQUITY UPLC HSS T3 C 18 column(2.1×100 mm,1.8μm),with acetonitrile(A)-0.05%phosphoric acid solution at the flow rate of 0.3 mL·min^(-1).Detection wavelength was set at 320 nm,the column temperature was maintained at 30℃,and the injection volume was 2μL.The relative correction factors(f s/k)of the other three components was calculated by slope correction method with icariin as internal reference substance.Results:The linear range of icariin,epimedin A,epimedin B and epimedin were 7.13~713.38μg·mL^(-1)(r=0.9999),1.28~128.40μg·mL^(-1)(r=0.9999),5.11~510.80μg·mL^(-1)(r=0.9999),4.36~435.67μg·mL(r=0.9999),respectively.The average recoveries were 104.56%,99.69%,100.00%,98.59%,and the RSDs were 1.4%,2.7%,1.2%,2.8%,respectively.By slope correction method,f s/k of epimedin A,epimedin B and epimedin C were 1.31,1.19,1.17.There were no significance difference in content determination results between two correction methods of QAMS and external standard(P>0.05).Conclusion:The method is simple,accurate and sensitive,and can be used for the quality control study of total Flavonol Glycosides in Shenge Bushen Capsule.

关 键 词：参葛补肾胶囊 总黄酮醇苷 高效液相色谱 一测多评法 

分 类 号：R284.2[医药卫生—中药学]