【摘要】：由于中藥化學對照品多數(shù)來源于動植物藥材,很容易混有結(jié)構(gòu)類似物,故有機雜質(zhì)測定是可能影響其化學對照品賦值準確性的關(guān)鍵風險因素。中藥化學對照品的有機雜質(zhì)測定通常采用藥典收載或文獻報道的高效液相色譜法,這些方法通常僅規(guī)定"以十八烷基硅烷鍵合硅膠為填充劑",無適宜色譜柱的品牌信息,或者實驗室無文獻所用的色譜柱品牌,而目前市場上已有800多種品牌的C18柱,生產(chǎn)工藝的不同導(dǎo)致不同品牌C18柱的選擇性有差異,甚至差異顯著。這很容易出現(xiàn)由于色譜柱選擇不適宜而導(dǎo)致測定結(jié)果不準確的風險。該文采用國外色譜柱分類數(shù)據(jù)庫指導(dǎo)對照品純度考察時色譜柱的理性選擇,盡可能減少色譜柱盲選可能導(dǎo)致的純度結(jié)果不準確的風險。首先,用數(shù)據(jù)庫挑選2根選擇性差異顯著的色譜柱(選擇性因子F≥6)進行平行實驗,以盡可能反映采用不同品牌色譜柱可能出現(xiàn)的分離效果差異。如果這2根色譜柱的分離效果及純度測定結(jié)果無顯著性差異,則可以交叉驗證該對照品純度測定的準確性。否則需要從數(shù)據(jù)庫中選擇另外1根與之前試驗中分離效果更好、選擇性相似的色譜柱進行純度結(jié)果驗證。在N-反式-p-對香豆�；野泛捅韮翰杷貨]食子酸酯首批對照品的純度考察中,使用了上述策略并驗證了其有效性和科學性,計劃推廣應(yīng)用至更多的中藥化學對照品,特別當其可能含堿性或弱酸性化合物時,更應(yīng)該嘗試采用本文推薦的色譜柱選擇策略交叉驗證其純度測定結(jié)果的準確性。
[Abstract]:Because most of the chemical reference materials of traditional Chinese medicine come from animal and plant herbs, it is easy to mix with structural analogs, so the determination of organic impurities is the key risk factor that may affect the accuracy of assignment of chemical reference materials. The determination of organic impurities in chemical reference substances of traditional Chinese medicine is usually determined by high performance liquid chromatography (HPLC) carried by pharmacopoeia or reported in the literature. These methods usually only stipulate that "octadecyl silane bonded silica gel is used as filler" and there is no brand information suitable for chromatographic columns. There are more than 800 brands of C18 columns in the market, and the different production process leads to the difference of the selectivity of C18 columns of different brands, or even significant difference. This is prone to the risk of inaccurate results due to inappropriate column selection. In this paper, the rational selection of chromatographic column is guided by foreign chromatographic column classification database in order to reduce the risk of inaccuracy of purity result caused by blind selection of chromatographic column as far as possible. Firstly, two chromatographic columns (F 鈮，

本文編號：2220043