目的:采用一测多评,建立味连饮片中非洲防己碱、药根碱、表小檗碱、黄连碱、巴马汀、小檗碱6个生物碱类成分的含量测定方法。方法:采用C18色谱柱(250 mm×4.6 mm,5 μm),以乙腈-水(含0.3%磷酸及0.2%三乙胺)为流动相,梯度洗脱,流速0.7 mL·min-1,柱温20℃,检测波长268 nm,建立小檗碱与非洲防己碱、表小檗碱、巴马汀、黄连碱、药根碱的相对校正因子,并以相对保留时间作为目标峰的定位标准。结果:色谱峰分离度良好,非洲防己碱、药根碱、表小檗碱、黄连碱、巴马汀、小檗碱进样量分别在0.118~1.18、0.176~1.76、0.190~1.90、0.272~2.72、0.198~1.98、0.98~9.80 μg范围内呈良好线性关系,平均加样回收率分别为102.4%、98.1%、100.2%、102.6%、103.6%、103.3%。小檗碱对非洲防己碱、药根碱、表小檗碱、黄连碱、巴马汀的相对校正因子分别为1.351、1.094、1.304、1.361、1.451;12批味连饮片中6个生物碱类成分一测多评法计算值与实测值间均无显著性差异(RE<5%)。结论:采用一测多评法测定味连中生物碱类成分的含量准确、可行。
Objective:To establish the content determination method of 6 alkaloids(columbamine, jatrorrhizine,epiberberine,coptisine,palmatine and berberine) in prepared slides of Coptis chinensis. Methods:C18 chromatographic column(250 mm×4.6 mm,5 μm) was adopted,the mobile phase was acetonitrile-water (containing 0.3% phosphoric acid and triethylamine) at a flow rate of 0.7 mL·min-1. The column temperature was 20℃ and the detection wavelength was 268 nm. The relative correction factors of berberine to columbamine,jatrorrhizine,epiberberine,coptisine and palmatine were determined,and the relative retention time was used for peak identification. Results:The chromatographic peaks were separated well. The linear ranges of columbamine,jatrorrhizine,epiberberine,coptisine,palmatine and berberine were 0.118 to 1.18 μg,0.176 to 1.76 μg,0.190 to 1.90 μg,0.272 to 2.72 μg,0.198 to 1.98 μg,and 0.98 to 9.80 μg,respectively. The average recoveries were 102.4%,98.1%,100.2%,102.6%,103.6% and 103.3%,respectively. The relative correction factors of berberine to columbamine,jatrorrhizine,epiberberine,coptisine,and palmatine were 1.351,1.094,1.304,1.361 and 1.451,respectively. There was no significant difference(RE<5%) between the calculated values and the measured values of 6 alkaloids in 12 batches of prepared slides of Coptis chinensis Franch. Conclusion:The proposed QAMS method for determinantion of alkaloids in Coptis chinensis Franch. is accurate and feasible.