丹参中丹参酮类成分及含量测定方法的分析.pdf

提要目的: 本研究旨在建立丹参中丹参酮类成分的快速分离方法,并建立测定丹参药材中丹参酮类成分含量的一测多评法,以提高丹参药材质量评价方法的水平。方法: 根据研究目的,首先进行了与丹参有关的文献整理。在此基础上,有针对性地开展了系统的实验研究工作。利用硅胶柱色谱法对丹参脂溶性提取物进行初步分离,再利用高速逆流色谱法进一步分离纯化,对所得单体成分采用 NMR 、 ESI-MS 进行结构鉴定。然后进行了一测多评法测定丹参药材中丹参酮类成分的实验研究。用高效液相色谱法进行了 4种丹参酮类成分的线性范围考察;色谱系统精密度考察;供试品溶液稳定性考察;方法重复性考察;加样回收率考察;丹参酮Ⅱ A 对丹参酮Ⅰ、隐丹参酮和二氢丹参酮的相对校正因子重现性考察;待测成分色谱峰定位参数考察。通过上述方法学研究,建立了以丹参酮Ⅱ A为对照品,同时测定丹参药材中 4 种丹参酮类成分含量的一测多评法。用该法对 10 批丹参药材中 4 种丹参酮类成分进行了含量测定,分别采用一测多评法和外标法计算其中丹参酮Ⅱ A、丹参酮Ⅰ、隐丹参酮和二氢丹参酮的含量,比较外标法测定结果与一测多评法测定结果的差异。结果: 利用硅胶柱色谱法结合高速逆流色谱法从丹参中成功分离获得六种单体成分,分别鉴定为丹参酮 I、二氢丹参酮 I、丹参酮 A Ⅱ、二氢丹参酮、 Trijuganone B 及隐丹参酮。分别采用一测多评法和外标法测定了 10 批丹参药材中丹参酮Ⅱ A 、丹参酮Ⅰ、隐丹参酮和二氢丹参酮的含量,测定结果表明二者无明显差异。结论: 上述研究工作的开展及所取得的各项研究结果,进一步提高了丹参药材质量评价方法的水平,可为完善丹参药材质量标准提供参考。关键词丹参;丹参酮;一测多评法 Studies on the ponents and Dtermination Method of Salvia miltiorrhiza Speciality: Chinese Materia Medica Author: Lan Tian-feng Tut or: Yu Zong-yuan Abstract OBJECTIVE: The present study is to establish the rapid separation ponents tanshinone method,and a measurement to test the content of 4 ki nds of tanshinone in salvia, in order to improve the quality evaluation of Radix Salvia. METHOD: Based on the objective of the present study, we first collect the relevant literature of this basis, we target to start a systematic expe rimental study. Salvia silica gel column chromatography Separation of fat-soluble extract, re-use high-speed counter-current chromatography separation and struct ures of the target compounds were identified by ESI-MS and we adopt a multi-assessment method to measure the quality evaluation of Radi x Salvia together with experimental study. We use high-performance liquid to conduct a seri es of study, including a linear study of the 4 tanshinone, chromatography system precision st udy, stability of the test solution, method precision study, recoveries visits, tanshinone Ⅱ A on tanshinone Ⅰ, tanshinone Cryptotanshinone and the rela tive correction factor dihydro