色谱柱分类数据库用于指导天然药物化学对照品色谱纯度测定时色谱柱理性选择（英文）  

Rational column selection approach for purity determination of chemical reference standards of natural products based on a column characterization database

作　　者：王明娟[1] 戴忠[1] 马双成[1] 金红宇[1] HOOGMARTENS Jos ADAMS Erwin 

机构地区：[1]中国食品药品检定研究院中药民族药检定所,北京100050 [2]鲁汶大学药物分析实验室

出　　处：《色谱》2017年第2期196-202,共7页Chinese Journal of Chromatography

基　　金：National Science and Technology Major Projects for "Major New Drugs Innovation and Development"(No.2014ZX09304307-002)

摘　　要：由于中药化学对照品多数来源于动植物药材,很容易混有结构类似物,故有机杂质测定是可能影响其化学对照品赋值准确性的关键风险因素。中药化学对照品的有机杂质测定通常采用药典收载或文献报道的高效液相色谱法,这些方法通常仅规定"以十八烷基硅烷键合硅胶为填充剂",无适宜色谱柱的品牌信息,或者实验室无文献所用的色谱柱品牌,而目前市场上已有800多种品牌的C18柱,生产工艺的不同导致不同品牌C18柱的选择性有差异,甚至差异显著。这很容易出现由于色谱柱选择不适宜而导致测定结果不准确的风险。该文采用国外色谱柱分类数据库指导对照品纯度考察时色谱柱的理性选择,尽可能减少色谱柱盲选可能导致的纯度结果不准确的风险。首先,用数据库挑选2根选择性差异显著的色谱柱(选择性因子F≥6)进行平行实验,以尽可能反映采用不同品牌色谱柱可能出现的分离效果差异。如果这2根色谱柱的分离效果及纯度测定结果无显著性差异,则可以交叉验证该对照品纯度测定的准确性。否则需要从数据库中选择另外1根与之前试验中分离效果更好、选择性相似的色谱柱进行纯度结果验证。在N-反式-p-对香豆酰基酪胺和表儿茶素没食子酸酯首批对照品的纯度考察中,使用了上述策略并验证了其有效性和科学性,计划推广应用至更多的中药化学对照品,特别当其可能含碱性或弱酸性化合物时,更应该尝试采用本文推荐的色谱柱选择策略交叉验证其纯度测定结果的准确性。Organic impurity determination is a critical aspect since it has a great impact on the assigned content of chemical reference standards (CRS). This is especially the case for CRS of natural products (CRSNPs) which are mostly obtained from medicinal plants or animals. Total amount of organic impurities of CRSNPs is generally determined by high performance liquid chromatography based on official or reported methods. Since the brand of column is not always prescribed or when the brand prescribed is not available in the laboratory, this can cause serious consequences, especially when the sample contains a basic or weak acid compound with pK(a) values ranged from 3 to 6. In this paper, columns were originally selected based on a peer. reviewed column characterization database. Firstly two columns with orthogonal selectivity (selectivity factor F >= 6) were selected from the database to determine the purity of the respective CRSNPs. The selection was performed to minimize the risk to obtain different values caused by use of various brands of columns. If there is no significant difference between their results, then the purity result is cross. validated. Otherwise, a third column has to be selected from the database and its selectivity should be similar to the above one which give better separation (F <= 2). The approach has been illustrated by the purity determinations of N-trans-p-coumaroyltyramine and (-)-epicatechin-3-O-gallate CRSNPs, and it is most likely to be applied in more CRSNPs, especially those of basic or weak acid ones.

关 键 词：中药化学对照品 色谱纯度 色谱柱理性选择策略 色谱柱分类数据库 N-反式-P-对香豆酰基酪胺 表儿茶素没食子酸酯 

分 类 号：O658[理学—分析化学]