一测多评法测定银黄片中的9种有效成分

Determination of Nine Active Components in Yinhuang Tablets by QAMS Method

以黄芩苷(6)为内参物,建立了一测多评法(QAMS法)同时测定银黄片中的新绿原酸(1)、绿原酸(2)、隐绿原酸(3)、咖啡酸(4)、木犀草苷(5)、黄芩苷(6)、汉黄芩苷(7)、黄芩素(8)和汉黄芩素(9)。采用高效液相色谱法,使用Zorbax SB-C18色谱柱,以甲醇:0.4%磷酸为流动相,线性梯度洗脱,检测波长280 nm(0~35 min,检测1~5),325 nm(35~60 min,检测6~9)。1~9的相对校正因子(RCF)分别为0.65、0.66、0.72、0.43、1.54、1.00、1.13、0.73和0.92,相对保留时间(RRT)分别为0.16、0.27、0.38、0.55、0.86、1.00、1.11、1.16和1.28。1~9分别在1.05~10.50、1.50~15.00、0.28~2.80、0.40~4.00、1.20~12.00、20.00~200.00、7.00~70.00、9.00~90.00和7.30~73.00μg/ml范围内线性关系良好,平均回收率为93.96%~99.28%,RSD为2.14%~3.95%。利用本法与外标法分别测定10批银黄片中的1~9,2种方法测定结果无显著性差异。

A quantitative analysis of multicomponents by single marker（QAMS） was established for multicomponents determination of neochlorogenic acid（1）, chlorogenic acid（2）, cryptochlorogenic acid（3）, caffeic acid（4）, cynaroside（5）, baicalin（6）, wogonoside（7）, baicalein（8） and wogonin（9） in Yinhuang tablets, with baicalin（6） as the internal reference. An HPLC method was applied, and the separation was carried out on a Zorbax SB-C18 column, with the mobile phase of methanol：0.4% phosphoric acid solution, at the detection wavelengths of 280 nm（0-35 min, for detection of 1-5） and 325 nm（35-60 min, for detection of 6-9）. The relative correction factors（RCFs） of 1-9 were 0.65, 0.66, 0.72, 0.43, 1.54, 1.00, 1.13, 0.73 and 0.92, and their relative retention time（RRTs） were 0.16, 0.27, 0.38, 0.55, 0.86, 1.00, 1.11, 1.16 and 1.28, respectively. It was linear for 1-9 in the ranges of 1.05-10.50, 1.50-15.00, 0.28-2.80, 0.40-4.00, 1.20-12.00, 20.00-200.00, 7.00-70.00, 9.00-90.00 and 7.30-73.00 μg/ml. Their average recoveries were 93.96%-99.28%, with RSDs of 2.14%-3.95%. Ten batches of Yinhuang tablets were quantitatively determined both by QAMS method and the external standard method（ESM）. The results showed that there were no significant differences between these two methods.