HPLC法测定消渴平片中5种成分

Simultaneous determination of five compoents in Xiaokeping Tablets by HPLC

目的通过色谱条件的优化,建立了一种同时测定消渴平片中丹参素、原儿茶醛、丹酚酸B、葛根素和盐酸小檗碱的多指标分析方法。方法采用Agilent Zorbax Eclipse XDB-C18（150 mm×4.6 mm,5μm）色谱分离柱,流动相为乙腈（A）-甲醇（B）-0.5%H3PO4水溶液（C）,采用梯度洗脱（0 min：4%A,96%C;7 min：4%A,1%B,95%C;20 min：10%A,3%B,87%C;30 min：15%A,3%B,82%C;45 min：25%A,10%B,65%C;60 min：30%A,10%B,60%C）,体积流量1.0 m L/min,柱温30℃,进样量10μL,波长280 nm（丹参素、原儿茶醛、丹酚酸B）、250 nm（葛根素）、265 nm（小檗碱）。结果丹参素、原儿茶醛、丹酚酸B、葛根素和盐酸小檗碱分别在33.02~528.41、1.44~22.46、374.51~5 992.20、84.86~1 357.82、312.50~5 000.00μg/m L线性关系良好,平均回收率分别为98.24%（RSD 0.26%）、98.37%（RSD 1.01%）、98.86%（RSD 0.50%）、98.93%（RSD 0.68%）、99.04%（RSD 0.29%）。结论此方法分离效果好、操作简单、方便,能达到较好地控制产品质量的目的。

Objective By optimizing the chromatographic conditions, to establish a method of multi-target content analysis, the components of danshensu, protocatechuic aldehyde, salvianolic acid B, puerarin, and berberine hydrochloride in Xiaokeping Tablets were simultaneously determined. Methods Agilent Zorbax Eclipse XDB-C18（150 mm × 4.6 mm, 5 μm） chromatographic separation column was used, mobile phase was composed of acetonitrile（A）, methanol（B）, and 0.5% H3PO4 aqueous solution（C） in a linear gradient elution mode（0 min： A 4%, C 96%; 7 min： A 4%, B 1%, C 95%; 20 min： A 10%, B 3%, C 87%; 30 min： A 15%, B 3%, C 82%; 45 min： A 25%, B 10%, C 65%; and 60 min： A 30%, B 10%, C 60%）. The flow rate was 1.0 m L/min, the column temperature was set at 30 ℃, and injection volume was 10 μL. The detection wavelength was set at 280 nm for danshensu, protocatechuic aldehyde, and salvianolic acid B, 250 nm for puerarin, and 265 nm for berberine hydrochloride. Results There was a good linear relationship over a rang of 33.02 — 528.41 μg/m L for danshensu, 1.44 — 22.46 μg/m L for protocatechuic aldehyde, 374.51— 5 992.20 μg/m L for salvianolic acid B, 84.86—1 357.82 μg/m L for puerarin, and 312.50—5 000.00 μg/m L for berberine hydrochloride, respectively. The average recovery rates were 98.24%（RSD = 0.26%）, 98.37%（RSD = 1.01%）, 98.86%（RSD = 0.50%）, 98.93%（RSD = 0.68%）, 99.04%（RSD = 0.29%）, respectively. Conclusion The separation effect is good, the operation is simple and convenient, so as to achieve the better quality control of the products by this method.