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出 处:《西部中医药》2014年第11期25-28,共4页Western Journal of Traditional Chinese Medicine
基 金:国家中医药管理局新药开发专项基金(编号DLX-016A)
摘 要:目的:采用不同纯化方式和优化色谱条件建立湿疹康喷剂中苦参碱与氧化苦参碱的测定方法。方法:分别采用浓氨水碱化后三氯甲烷萃取方法、AB-8大孔树脂方法、中性氧化铝吸附方法纯化样品,通过HPLC进行含量测定,确定最佳纯化工艺;采用氨基硅烷键合硅胶柱(4.6 mm×150 mm,5μm),流动相分别为乙腈-无水乙醇-3%磷酸溶液(80∶10∶10)、乙腈-无水乙醇-3%磷酸溶液(80∶12∶8);检测波长为220 nm。结果:苦参碱的线性范围为Y=646567X+8332.1(r=0.999 9);氧化苦参碱的线性范围为Y=501 596X-414 182(r=0.9994)。结论:三种不同纯化方式中,浓氨水碱化后三氯甲烷萃取方法中苦参碱与氧化苦参碱测定含量最好,流动相为乙腈-无水乙醇-3%磷酸溶液(80∶10∶10)时苦参碱与氧化苦参碱峰形最佳,保留时间合适。Objective: To establish the determination methods of matrine and oxymatrine in Shi Zhen Kang spray by adopting different purification ways and optimizing chromatographic conditions. Methods: Chloroform extraction after alkalifying by strong ammonia water, AB-8 macroporous resin method and neutral alumina absorption were adopted to purifying the sample, the contents were determined by HPLC to find out the optimal purification technology. Amino chemically bonded silica column(4.6 mm×150 mm, 5 μm) was adopted, and mobile phases were acetonitrile-absolute ethyl alcohol-3% phosphoric acid solution(80 ∶10∶10), acetonitrile-absolute ethyl alcohol-3% phosphoric acid solution(80∶12∶8) respectively. Detection wavelength was 220 nm. Results: Linear range of matrine was Y=646 567X+ 8 332.1(r=0.999 9); linear range of oxymatrine was Y=501 596X-414 182(r=0.999 4).Conclusion: Among three difference purification methods, chloroform extraction after alkalifying by strong ammonia water is used to extract matrine and oxymatrine in high contents, matrine and oxymatrine show the best peaks with suitable retention time when mobile phase is acetonitrile-absolute ethyl alcohol-3% phosphoric acid solution(80∶10∶10).
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