HPLC内标法同时测定芪麝丸中9种成分

目的建立芪麝丸(黄芪、川芎、青风藤、粉防己等)中9种成分,毛蕊异黄酮、毛蕊异黄酮葡萄糖苷、芒柄花素、芒柄花素苷、洋川芎内酯I、洋川芎内酯A、粉防己碱、防己诺林碱、青藤碱的定量分析方法。方法采用HPLC内标法,选用异补骨脂素为内标物,样品经过甲醇提取,采用Kromasil C18柱,甲醇-0.2%甲酸水溶液为流动相,梯度洗脱,紫外检测波长262 nm。结果毛蕊异黄酮、毛蕊异黄酮葡萄糖苷、芒柄花素、芒柄花素苷、洋川芎内酯I、洋川芎内酯A、粉防己碱、防己诺林碱、青藤碱分别在13.8～440μg/mL、25.9～830μg/mL、9.7～310μg/mL、6.6～212μg/mL、6.3～200μg/mL、6.3～200μg/mL、14.1～450μg/mL、11.3～360μg/mL、50.9～1 630μg/mL范围内呈良好线性关系,内标法与标准曲线法测定结果一致。结论该方法准确可靠,可用于芪麝丸的质量控制。

Simultaneous determination of nine constituents in Qishe Pill by HPLC internal standard method

AIM To establish a quantitative analysis method for determining nine constituents(calycosin,calycosin-7-glucoside,formononetin,ononin,senkyunolide I,senkyunolide A,tetrandrine,fangchinoline and sinomenine) in Qishe Pill(Astragali Radix,Chuanxiong Rhizoma,Sinomenii Caulis,Stephaniae tetrandrae Radix,etc.).METHODS Nine constituents in Qishe Pill with the internal standard isopsoralen were separated on a Kromasil C18 column.The mobile phase consisted of methanol-0.2%methanoic acid(gradient elution) and detection wavelength was set at 262 nm.The contents of nine constituents were calculated by internal standard method.RESULTS The linear ranges of calycosin,calycosin-7-glucoside,formononetin,ononin,senkyunolide I,senkyunolide A,tetrandrine,fangchinoline,and sinomenine were 13.8-440 μg/mL,25.9-830 μg/mL,9.7-310 μg/mL,6.6-212 μg/mL,6.3-200 μg/mL,6.3-200 μg/mL,14.1-450 μg/mL,11.3-360 μg/mL,50.9-1 630 μg/mL,respectively.The result of the standard curve method agreed with that of internal standard method.CONCLUSION The method is sensitive,stable,practical and suitable for the quality control of Qishe Pill.