双山颗粒剂质量标准提高实验研究.pdf

目 录 中文摘要 ···················································1 英文摘要 ···················································3 引 言 ·······················································5 正 文 ······················································7 第一部分 双山颗粒定性分析方法的研究 1 薄层色谱鉴别条件研究与优化 ·································7 1.1 材料、实验仪器与试剂 ······································7 1.2 原标准中双山颗粒薄层鉴别条件 ·····························7 1.3 薄层鉴别条件的优化 ·······································8 1.4 薄层鉴别条件优化的结果 ···································9 1.5 小结与讨论 ··············································11 2 制剂通则检查 ·············································12 2.1 材料、实验仪器与试剂·····································12 2.2 制剂通则检查 ············································12 第二部分 双山颗粒定量分析方法的研究 1 总黄酮含量测定方法的设计 ·································16 1.1 材料、实验仪器与试剂 ·····································16 1.2 单因素考察 ··············································16 1.3 实验方法学考察〃〃········································18 1.4 测定结果 ················································22 1.5 小结与讨论 ··············································22 2 高效液相色谱含量测定的研究与条件优化 ·····················23 2. 1 材料、实验仪器与试剂 ·····································23 2.2 原标准中双山颗粒绿原酸含量测定条件 ······················23 2.3 色谱条件优化············································24 2.4 供试品制备方法的考察 ····································27 2.5 分析测定方法学研究 ······································28 2.6 中间体含量测定结果······································39 2.7 样品含量测定结果 ········································40 2.8 小结与讨论 ··············································43 第三部分 双山颗粒指纹图谱分析方法的研究 1 双山颗粒指纹图谱分析方法的研究 ···························44 1.1 材料、实验仪器与试剂 ·····································44 1.2 色谱及检测条件的选择····································44 1.3 分析测定的方法学考察研究 ································50 1.4 指纹图谱的建立及技术参数 ································55 1.5 双山颗粒相似度评价 ···················