[關(guān)鍵詞]
[摘要]
目的 建立了HPLC-DAD波長切換法測定通絡(luò)開痹片中5-O-甲基維斯阿米醇苷、士的寧、馬錢子堿和杯莧甾酮的分析方法。方法 Purospher ODS C18色譜柱(250mm×4.6mm,5μm);以乙腈–0.5%磷酸溶液為流動相,梯度洗脫;測定波長:260nm(士的寧和馬錢子堿)、243nm(杯莧甾酮)、254nm(5-O-甲基維斯阿米醇苷);體積流量:1.0mL/min;柱溫:30℃;進樣體積:10μL。結(jié)果 杯莧甾酮、馬錢子堿、士的寧和5-O-甲基維斯阿米醇苷分別在0.0584~5.8400、0.1180~11.8000、0.0949~9.9000、0.0238~2.3800μg/mL具有良好的線性,平均回收率分別為100.51%、99.59%、98.75%、100.38%,RSD值分別為1.6%、1.1%、1.7%、1.6%。結(jié)論 本法具有前處理簡單、分析時間短、檢測結(jié)果準確等優(yōu)點,適用于通絡(luò)開痹片的質(zhì)量控制。
[Key word]
[Abstract]
Objective To establish an HPLC-DAD wavelength switching method for determination of 5-O-methylvisamitol glycoside, strychnine, brucine, and cyasterone in Tongluo Kaibi Tablets. Methods Purospher ODS C18 column (250 mm×4.6 mm, 5 μm) was used. The mobile phase was consisted of acetonitrile-0.5% phosphoric acid solution with gradient elution. The detection wavelengths were set at 260 nm for strychnine and brucine, 243 nm for cyasterone, and 254 nm for 5-O-methylvisamitol glycoside. The column temperature was 30℃, volume flow was 1.0 mL/min, and the injection volume was 10 μL. Results Cyasterone, brucine, strychnine, and 5-O-methylvisamitol glycoside showed good linear relationships in concentration range of 0.0584-5.8400, 0.1180-11.8000, 0.0949-9.9000, and 0.0238-2.3800 μg/mL. The average recoveries were 100.51%, 99.59%, 98.75%, and 100.38% with RSD values of 1.6%, 1.1%, 1.7%, and 1.6%, respectively. Conclusion The method has the advantages of simple pretreatment, short analysis time, and accurate detection result, which is suitable for quality control of Tongluo Kaibi Tablets.
[中圖分類號]
R286.02
[基金項目]