HPLC法测定注射用清开灵(冻干)中6种成分  

Determination of six constituents in Qingkailing Freeze-Dried Powder for Injection by HPLC

作　　者：王芳[1,2] 杜鹏[3] 黄红梅 茅向军[2] 许乾丽[2] WANG Fang;DU Peng;HUANG Hong-mei;MAO Xiang-jun;XU Qian-li(Zunyi Medical College,Zunyi 563000,China;Guizhou Provincial Institute for Food and Drug Control,Guiyang 550004,China;Hospital Affiliated to Guizhou Medical University,Guiyang 550004,China;Guiyang College of Traditional Chinese Medicine,Guiyang 550004,China)

机构地区：[1]遵义医学院,贵州遵义563000 [2]贵州省食品药品检验所,贵州贵阳550004 [3]贵州医科大学附属医院,贵州贵阳550004 [4]贵阳中医学院,贵州贵阳550004

出　　处：《中成药》2018年第4期848-852,共5页Chinese Traditional Patent Medicine

基　　金：贵州省中药现代化科技产业研究开发专项项目(黔科合中药字[2013]5026)

摘　　要：目的建立HPLC法测定注射用清开灵(冻干)(胆酸、猪去氧胆酸、水牛角等)中6种成分的含有量。方法腺苷、绿原酸、栀子苷含有量的测定采用XBridge C18色谱柱(4.6 mm×250 mm,5μm);以乙腈-水(含0.1%甲酸)为流动相,梯度洗脱;体积流量1.0 m L/min;柱温30℃;检测波长254 nm。黄芩苷、猪去氧胆酸、胆酸含有量的测定采用XBridge C18色谱柱(4.6 mm×250 mm,5μm);以甲醇-水(含0.1%甲酸)为流动相,梯度洗脱;体积流量1.0 m L/min;柱温35℃。结果 6种成分分别在2.244~56.108、2.658~66.445、4.347~108.682、122.01~1 016.75、131.94~1 099.50、152.22~1 268.50μg/m L范围内线性关系良好(r>0.999 0),平均加样回收率(RSD)分别为101.1%(0.46%)、98.0%(1.74%)、99.7%(0.15%)、100.9%(1.31%)、98.1%(0.18%)、98.2%(1.61%)。结论该方法稳定、重复性好,可用于注射用清开灵(冻干)的质量控制。AIM To establish an HPLC method for the content determination of six constituents in Qingkailing Freeze-Dried Powder for Injection(cholic acid,hyodeoxycholic acid,Bubali Cornu,etc.).METHODS The content determination of adenosine,chlorogenic acid and gardenoside was performed on a 30°C thermostatic XBridge C18 column(4.6 mm x 250 mm,5(xm),with the mobile phase comprising of acetonitrile-water(containing 0.1%formic acid)flowing at 1.0 miymin in a gradient elution manner,and the detection wavelength was set at 254 nm.The content determination of baicalin,hyodeoxycholic acid and cholic acid was performed on a 35°C thermostatic XBridge C18 column(4.6 mm x 250 mm,5(xm),with the mobile phase comprising of methanol-water(containing 0.1%formic acid)flowing at 1.0 mL/min in a gradient elution manner.RESULTS Six constituents showed good linear relationships within the ranges of 2.244-56.108,2.658-66.445,4.347-108.682,122.01-1 016.75,131.94-1 099.50,152.22-1 268.50(xg/mL(r>0.999 0),whose average recoveries(RSDs)were 101.1%(0.46%),98.0%(1.7 4%),99.7%(0?15%),100.9%(1.31%),98.1%(0.18%),98.2%(1.61%),respectively.CONCLUSION This stable and reproducible method can be used for the quality control of Qingkailing Freeze-Dried Powder for Injection.

关 键 词：注射用清开灵(冻干) 腺苷 绿原酸 栀子苷 黄芩苷 猪去氧胆酸 胆酸 HPLC 

分 类 号：R927.2[医药卫生—药学]