[关键词]
[摘要]
目的 建立参芪消渴颗粒中尿囊素、24-乙酰泽泻醇A、23-乙酰泽泻醇B、茯苓酸和毛蕊异黄酮葡萄糖苷同时测定的方法。方法 采用高效液相色谱法,使用依利特Hypersil ODS 2色谱柱(250 mm×4.6 mm,5 μm);流动相:乙腈–0.1%磷酸溶液,梯度洗脱;测定波长:0~14 min在224 nm波长下尿囊,14~20 min在208 nm波长下检测24-乙酰泽泻醇A、23-乙酰泽泻醇B,20~26 min在210 nm波长下检测茯苓酸,26~36 min在260 nm波长下检测毛蕊异黄酮葡萄糖苷;体积流量:0.9 mL/min;柱温:30 ℃;进样量:10 μL。结果 5个成分的线性范围分别为9.43~188.60 μg/mL(r=0.999 4),3.75~75.00 μg/mL(r=0.999 7),4.06~81.20 μg/mL(r =0.999 9),4.82~96.40 μg/mL(r=0.999 5),3.79~75.80 μg/mL(r=0.999 8)。平均回收率分别为97.99%、99.34%、98.20%、96.57%、98.98%,RSD值分别为0.62%、1.14%、1.28%、0.79%、0.93%。结论 所建方法简便、可靠、准确度高,可有效地控制参芪消渴颗粒的质量。
[Key word]
[Abstract]
Objective To develop a method for simultaneous determination of allantoin, 24-acetate alisol A, 23-acetate alisol B, pachymic acid, and calycosin 7-O-β-D-glucopyranoside in Shenqi Xiaoke Granules. Method An HPLC method was adopted for the analysis on Hypersil ODS 2 column (250 mm × 4.6 mm, 5 μm). The mobile phase consisted of acetonitril-0.1% phosphoric acid solution with gradient elution. The detection wavelengths were set at 224 nm in 0-14 min (determination of allantoin), 208 nm in 14-20 min (determination of 24-acetate alisol A and 23-acetate alisol B), 210 nm in 20-26 min (determination of pachymic acid), and 260 nm in 26-36 min (determination of calycosin 7-O-β-D-glucopyranoside). The flow rate was 0.9 mL/min, temperature of column was set at 30 ℃, and volume of injection was 10 μL. Results The linear range of allantoin, 24-acetate alisol A, 23-acetate alisol B, pachymic acid, and calycosin7-O-β-D-glucopyranoside were 9.43-188.60 μg/mL (r=0.999 4), 3.75-75.00 μg/mL (r=0.999 7), 4.06-81.20 μg/mL (r=0.999 9), 4.82-96.40 μg/mL (r=0.999 5), and 3.79-75.80 μg/mL (r=0.999 8), respectively. The average recoveries were 97.99%, 99.34%, 98.20%, 96.57%, and 98.98% with RSD 0.62%, 1.14%, 1.28%, 0.79%, and 0.93%, respectively. Conclusion The method is simple, reliable, and accurate, and can effectively control the quality of Shenqi Xiaoke Granules.
[中图分类号]
[基金项目]