HPLC-PAD-ELSD法同时测定牛黄降压丸中6个成分的含量  

Simultaneous Determination of 6 Components in Niuhuang Jiangya Pills by HPLC-PAD-ELSD

作　　者：张松达 李积杰 辛晓恩 李卫鸿 程国栋 Zhang Songda;Li Jijie;Xin Xiaoen;Li Weihong;Cheng Guodong(The Fourth People’s Hospital of Qinghai Province,Xining 810000,China)

机构地区：[1]青海省第四人民医院,西宁810000

出　　处：《中国药师》2021年第5期972-976,共5页China Pharmacist

摘　　要：目的:建立高效液相色谱-二极管阵列检测-蒸发光散射检测(HPLC-PAD-ELSD)法同时测定牛黄降压丸中芍药苷、阿魏酸、毛蕊异黄酮葡萄糖苷、黄芩苷、胆酸、黄芪甲苷含量的方法。方法:以L9(34)正交试验优化提取条件。采用Waters Sunfire C18色谱柱(250 mm×4.6 mm,5μm),以乙腈-0.2%甲酸溶液为流动相,梯度洗脱;流速为1.0 ml·min^(-1)。芍药苷、阿魏酸、毛蕊异黄酮葡萄糖苷、黄芩苷检测波长为278 nm;胆酸、黄芪甲苷使用ELSD检测器,漂移管温度为100℃,氮气流速为3.0 L·min^(-1)。结果:芍药苷、阿魏酸、毛蕊异黄酮葡萄糖苷、黄芩苷、胆酸、黄芪甲苷进样浓度分别在6.14~98.21μg·ml-1(r=0.9994)、10.84~173.50μg·ml-1(r=0.9998)、1.13~18.06μg·ml-1(r=0.9996)、301.98~4831.73μg·ml-1(r=0.9997)、3.44~55.02μg·ml-1(r=0.9991)、2.38~38.02μg·ml-1(r=0.9999)范围内与峰面积呈现良好的线性关系;平均加样回收率分别为103.0%,100.4%,101.5%,99.0%,102.4%,101.0%,RSD分别为0.6%,0.4%,1.0%,0.6%,0.7%,1.1%(n=9)。牛黄降压丸最佳提取方法为:采用50 ml 70%乙醇30℃超声提取30 min。结论:所建立的方法准确、灵敏度高、重复性好,可用于牛黄降压丸的质量控制。Objective:To establish an HPLC-PAD-ELSD method for the simultaneous determination of paeoniflorin,ferulic acid,calycosin7-O-β-D-glucopyranoside,baicalin,cholic acid and astragalosideⅣin Niuhuang Jiangya pills.Methods:L9(34)orthogonal design was carried out in order to optimize the extraction method.HPLC assay was performed on a Waters Sunfire C18 column(250 mm×4.6 mm,5μm)with a mixture of acetonitrile and 0.2%formic acid as the mobile phase with gradient elution at a flow rate of1.0 ml·min^(-1).The detection wavelength for paeoniflorin,ferulic acid,calycosin7-O-β-D-glucopyranoside and baicalin was set at278 nm,and ELSD was used for the detection of cholic acid and astragalosideⅣ.The temperature of drift tube was maintained at 100℃and the flow rate of nebulizing gas was 3.0 L·min^(-1).Results:The linear range of paeoniflorin,ferulic acid,calycosin7-O-β-Dglucopyranoside,baicalin,cholic acid and astragalosideⅣwas 6.14-98.21μg·ml-1(r=0.9994),10.84-173.50μg·ml-1(r=0.9998),1.13-18.06μg·ml-1(r=0.9996),301.98-4831.73μg·ml-1(r=0.9997),3.44-55.02μg·ml-1(r=0.9991)and 2.38-38.02μg·ml-1(r=0.9999),and the average recovery was 103.0%,100.4%,101.5%,99.0%,102.4%and101.0%with the RSDs of 0.6%,0.4%,1.0%,0.6%,0.7%and 1.1%(n=9),respectively.The optimal extraction method of Niuhuang Jiangya pills was using 50 ml 70%ethanol at 30℃by ultrasonic extraction for 30 min.Conclusion:The established method is accurate,highly sensitive and repeatable,which can be used for the quality control of Niuhuang Jiangya pills.

关 键 词：牛黄降压丸 高效液相色谱-二极管阵列检测-蒸发光散射检测 芍药苷 阿魏酸 毛蕊异黄酮葡萄糖苷 黄芩苷 胆酸 黄芪甲苷 

分 类 号：R927.2[医药卫生—药学]