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.
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)
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)。
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
Shenge Bushen capsules
Total flavonol glycosides
High performance liquid chromatography(HPLC)
Quantitative analysis of multi-components by single marker(QAMS)
