芪连降糖片的质量标准研究  

Study on Quality Standard of Qilian Jiangtang Tablets

作　　者：张蕾 杨春静 黄明月 ZHANG Lei;YANG Chun-jing;HUANG Ming-yue(Department of Pharmacy,Beijing Shijitan Hospital Affiliated to Capital Medical University,Beijing 100038,China;Beijing Key Laboratory of Bio-characteristic Profiling for Evaluation of Rational Drug Use,Beijing 100038,China)

机构地区：[1]首都医科大学附属北京世纪坛医院药学部,北京100038 [2]临床合理用药生物特征谱学评价北京市重点实验室,北京100038

出　　处：《食品与药品》2023年第3期193-200,共8页Food and Drug

基　　金：国家“重大新药创制”科技重大专项(编号:2017ZX09301040);首都医科大学附属北京世纪坛医院院基金(编号:2022-C03)。

摘　　要：目的建立芪连降糖片的质量标准。方法采用薄层色谱法(TLC)定性鉴别芪连降糖片中的黄芪、黄连(味连)。采用高效液相色谱-蒸发光散射检测法(HPLC-ELSD)测定芪连降糖片中黄芪甲苷的含量,色谱柱为Phenomenex Luna C_(18)色谱柱(250 mm×4.6 mm,5μm),流动相为乙腈-水(33:67),流速为1.0 ml/min。采用HPLC法同时测定芪连降糖片中表小檗碱、盐酸黄连碱、盐酸巴马汀和盐酸小檗碱的含量,色谱柱同黄芪甲苷含量测定,流动相为乙腈-0.05 mol/L磷酸二氢钾溶液(48:52)(每100 ml中加十二烷基硫酸钠0.4 g,再以磷酸调节pH值为4.0),流速为1.0 ml/min,检测波长为345 nm。结果黄芪、黄连(味连)薄层色谱斑点清晰,阴性对照无干扰。黄芪甲苷、表小檗碱、盐酸黄连碱、盐酸巴马汀和盐酸小檗碱分别在30.28~969.00,0.97~30.91,3.71~1_(18).88,0.95~30.50,16.26~520.20μg/ml范围内线性关系良好;平均加样回收率分别为98.8%,97.8%,101.2%,98.9%和97.3%,RSD分别为2.25%,1.89%,1.35%,2.40%和1.25%。结论此法简便可靠,专属性强,重现性好,适用于芪连降糖片的质量控制。Objective To establish the quality standard for Qilian Jiangtang Tablets.Methods Astragali Radix and Coptidis Rhizoma were identified by TLC.Astragaloside IV was determined by HPLC equipped with an ELSD and a phenomenex Luna C_(18) column(250 mm×4.6 mm,5μm).The mobile phase was a mixture of acetonitrile and water(33:67,V/V)and the flow rate was 1.0 ml/min.Epiberberine,coptisine hydrochloride,palmatine hydrochloride and berberine hydrochloride were determined by HPLC equipped with a DAD(345 nm)and the column was the same as above.The mobile phase was a mixture of acetonitrile and 0.05 mol/L KH2PO4(48:52,V/V)(added 0.4 g sodium dodecyl sulfate into every 100 ml solution,then adjusted the pH value to 4.0 with H3PO4)and the flow rate was 1.0 ml/min.Results The TLC spots of Astragali Radix and Coptidis Rhizoma were clear and without interference from negative controls.The good linear ranges of astragaloside IV,epiberberine,coptisine hydrochloride,palmatine hydrochloride and berberine hydrochloride were 30.28-969.00μg/ml(r=0.9989),0.97-30.91μg/ml(r=1.0000),3.71-118.88μg/ml(r=1.0000),0.95-30.50μg/ml(r=1.0000)and 16.26-520.20μg/ml(r=1.0000),respectively.The average recoveries were 98.8%,97.8%,101.2%,98.9%and 97.3%,with RSDs of 2.25%,1.89%,1.35%,2.40%and 1.25%,respectively.Conclusion The methods are simple,reliable,specific and repeatable,which can be used to control the quality of Qilian Jiangtang Tablets.

关 键 词：芪连降糖片 薄层色谱法 高效液相色谱法 黄芪甲苷 表小檗碱 盐酸黄连碱 盐酸巴马汀 盐酸小檗碱 

分 类 号：R927.2[医药卫生—药学]