芪葵颗粒定性定量方法研究

目的:建立芪葵颗粒的定性定量方法。方法:用薄层色谱法对该颗粒中的黄芪、黄蜀葵花、制何首乌进行定性鉴别。采用HPLC-ELSD法测定制剂中黄芪甲苷,使用Hedera ODS-2(4.6 mm×250 mm,5 μm)色谱柱,以乙腈-水(32:68)为流动相,流速1.0 mL·min^-1,柱温30℃,Alltech 2000ES蒸发光散射检测器(漂移管温度102℃,载气流量2.8 L·min^-1);采用HPLC法测定制剂中金丝桃苷、2,3,5,4'-四羟基二苯乙烯-2-O-β-D-葡萄糖苷(简称二苯乙烯苷)的含量,使用Hedera ODS-2(4.6 mm×250 mm,5 μm)色谱柱,以乙腈-0.1%磷酸水溶液为流动相进行梯度洗脱,流速1.0 mL·min^-1,检测波长320 nm,柱温30℃。结果:在薄层色谱中均能检出黄芪、黄蜀葵花、制何首乌。黄芪甲苷、金丝桃苷、二苯乙烯苷线性范围分别为1.59~21.3 μg(r=0.9997),0.048~0.567 μg(r=0.9999),0.054~0.625 μg(r=1.000);平均回收率 (n=6)分别为95.0%(RSD=2.2%),104.0%(RSD=1.3%),101.5%(RSD=1.4%)。结论:所建方法简便、准确,重复性好,可作为复方芪葵颗粒的定性定量方法。

Objective:To establish a qualitative and quantitative method for Qikui granules determination. Methods:TLC was used to identify Radix Astragali, Abelmoschi Corolla, and Polygoni Multiflori Radix Praeparata in Qikui granules. Astragloside in preparation was determination by HPLC-ELSD on Hedera ODS-2(4.6 mm×250 mm,5 μm) chromatographic column, the mobile phase was acetonitrile-water(32:68) at a flow rate of 1.0 mL·min^-1, and column temperature was 30℃;The flow rate of N₂ in ELSD was 2.8 L·min^-1, and the temperature of drift tube was 102℃. The contents of hyperin and stilbene glucoside were determined by HPLC on Hedera ODS-2(4.6 mm×250 mm,5 μm) column, the mobile phase was acetonitrile-0.1% phosphoric acid solution with gradient elution at a flow rate of 1.0 mL·min^-1;the detection wavelength was 320 nm and column temperature was 30℃. Results:Radix Astragali, Abelmoschi Corolla, and Polygoni Multiflori Radix Praeparata could be identified by TLC;The calibration curves of astragaloside, hyperin, and stilbene glucoside were linear in the ranges of 1.59-21.3 μg(r=0.9997),0.048-0.567 μg(r=0.9999),and 0.054-0.625 μg(r=1.000), respectively. The average recoveries(n=6) were 95.0%(RSD=2.2%), 104.0%(RSD=1.3%), and 101.5%(RSD=1.4%), respectively. Conclusions:The method established is simple, accurate and reproducible, which can be used for the quality and quantity study of Qikui granules.