治带片中苦参碱及氧化苦参碱HPLC法测定.docVIP

治带片中苦参碱及氧化苦参碱HPLC法测定 　【摘要】 目的 建立治带片中苦参碱及氧化苦参碱的高效液相色谱(HPLC)测定方法。方法 色谱柱：LichrospherNH2(4.6mm×250mm，5μm)，C18保护柱；流动相：乙腈无水乙醇0.5mol/L磷酸水溶液(80∶10∶10)；检测波长212nm；流速1.0mL/min；柱温：室温；进样量20μL。结果 苦参碱和氧化苦参碱线性范围均为1.0-10.0μg/mL，回归方程苦参碱为：C=1.201×10-4A+0.161，r=0.9992；氧化苦参碱为：C=1.366×10-4A+0.221，r=0.9996，平均回收率分别为99.9%和99.4%，RSD分别为1.48%和4.33%。结论 本法简便快捷，结果准确，可用于该制剂的质量控制。 【关键词】 治带片；苦参碱；氧化苦参碱；高效液相色谱 　　Determination of Alkaloids in Zhidaipian Tablets　by high performance liquid chromatogram 　　ABSTRACT: Objective To establish a method of high performance liquid chromatogram (HPLC) for measuring matrine and oxymatrine in Zhidaipian Tablets. Methods A LichrospherNH2 column(4.6mm×250mm, 5μm) was used with a mobile phase consisting of acetonitrileethanol0.5mol/L phosphoric acid (80∶10∶10), and in a flow rate of 1.0mL/min. The detective wavelength was 212nm. Column temperature was room temperature and the injection quantity was 20μL. Results The samples were well separated. The linear range was the same for the target (1.0-10.0μg/mL). The linear equations for matrine was C=1.201×10-4A +0.161, the correlation coefficient was 0.9992, and for oxymatrine was C=1.366×10-4A +0.221, while the correlation coefficient was 0.9996, respectively. The mean recovery rate were 99.9% and 99.4%, respectively. RSD was 1.48% and 4.33%, respectively (n=6). Conclusion The method is simple, reliable, accurate and can be used to the quality control of the Zhidaipian Tablets. 　　KEY WORDS: Zhidaipian tablets; matrine; oxymatrine; high performance liquid chromatogram 　　治带片处方由墓头回、苦参、金樱子、知母(盐炒)、苍术(炒)等组成。清利湿热，止带。用于湿热下注，赤带，白带，黄带等症。方中苦参为君药，其有效成分是苦参碱和氧化苦参碱。为有效控制药品质量, 对制剂中的苦参碱和氧化苦参碱采用高效液相色谱(HPLC)法进行含量测定。 　　1 材料与方法 　　1.1 仪器与试药 日本岛津LC10AT高效液相色谱输液泵，SPD10AVP紫外可见检测器，岛津7725i进样器，ANASTAR色谱工作站，DL360超声波清洗器(浙江象山县石浦海天电子仪器厂，功率240W，频率35kHz)，乙腈、无水乙醇为色谱纯，其他试剂为分析纯。苦参碱和氧化苦参碱对照品由中国药品生物制品检定所提供(编号分别为110805200306和0780200004)，供含量测定用。治带片由西安阿房宫制药有限公司提供(批20030613)。 　　1.2 对照品溶液的配制 精密称取苦参碱、氧化苦参碱对照品适量，用乙腈无水乙醇(8∶1)溶解，分别制成0.20mg/mL溶液作为苦参碱