【摘要】：由于中藥化學(xué)對(duì)照品多數(shù)來(lái)源于動(dòng)植物藥材,很容易混有結(jié)構(gòu)類似物,故有機(jī)雜質(zhì)測(cè)定是可能影響其化學(xué)對(duì)照品賦值準(zhǔn)確性的關(guān)鍵風(fēng)險(xiǎn)因素。中藥化學(xué)對(duì)照品的有機(jī)雜質(zhì)測(cè)定通常采用藥典收載或文獻(xiàn)報(bào)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(wú)適宜色譜柱的品牌信息,或者實(shí)驗(yàn)室無(wú)文獻(xiàn)所用的色譜柱品牌,而目前市場(chǎng)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(cè)定結(jié)果不準(zhǔn)確的風(fēng)險(xiǎn)。該文采用國(guó)外色譜柱分類數(shù)據(jù)庫(kù)指導(dǎo)對(duì)照品純度考察時(shí)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(zhǔn)確的風(fēng)險(xiǎn)。首先,用數(shù)據(jù)庫(kù)挑選2根選擇性差異顯著的色譜柱(選擇性因子F≥6)進(jìn)行平行實(shí)驗(yàn),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(cè)定結(jié)果無(wú)顯著性差異,則可以交叉驗(yàn)證該對(duì)照品純度測(cè)定的準(zhǔn)確性。否則需要從數(shù)據(jù)庫(kù)中選擇另外1根與之前試驗(yàn)中分離效果更好、選擇性相似的色譜柱進(jìn)行純度結(jié)果驗(yàn)證。在N-反式-p-對(duì)香豆酰基酪胺和表兒茶素沒(méi)食子酸酯首批對(duì)照品的純度考察中,使用了上述策略并驗(yàn)證了其有效性和科學(xué)性,計(jì)劃推廣應(yīng)用至更多的中藥化學(xué)對(duì)照品,特別當(dāng)其可能含堿性或弱酸性化合物時(shí),更應(yīng)該嘗試采用本文推薦的色譜柱選擇策略交叉驗(yàn)證其純度測(cè)定結(jié)果的準(zhǔn)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(hào)：2220043