目的 建立高效液相色譜法同時測定痛風(fēng)定膠囊中龍膽苦苷、馬錢苷酸、獐牙菜苦苷、獐牙菜苷、杯莧甾酮、澤瀉醇F、澤瀉醇A、24-乙酰澤瀉醇A和23-乙酰澤瀉醇B。方法 采用HPLC法，Waters Symmetry C₁₈色譜柱（250 mm×4.6 mm，5 μm）；流動相：乙腈-0.1%磷酸水溶液，梯度洗脫；檢測波長：240 nm（0~27 min檢測龍膽苦苷、馬錢苷酸、獐牙菜苦苷、獐牙菜苷和杯莧甾酮）和208 nm（27~55 min檢測澤瀉醇F、澤瀉醇A、24-乙酰澤瀉醇A、23-乙酰澤瀉醇B）；體積流量：1.0 mL/min；柱溫：30℃；進(jìn)樣量：10 μL。結(jié)果 龍膽苦苷、馬錢苷酸、獐牙菜苦苷、獐牙菜苷、杯莧甾酮、澤瀉醇F、澤瀉醇A、24-乙酰澤瀉醇A、23-乙酰澤瀉醇B分別在45.84~1 146.00、9.02~225.50、12.86~321.50、4.69~117.25、0.88~22.00、0.59~14.75、0.77~19.25、0.66~16.50、3.37~84.25 μg/mL與峰面積線性關(guān)系良好（r ≥ 0.999 1），平均加樣回收率分別為100.03%、99.55%、99.78%、98.56%、97.98%、96.95%、98.21%、97.75%、100.06%，RSD值分別為0.61%、0.95%、0.71%、1.17%、1.63%、1.09%、1.73%、1.20%、0.84%。結(jié)論 所建立的方法結(jié)果準(zhǔn)確，操作便捷，重復(fù)性好，為全面評價痛風(fēng)定膠囊的整體質(zhì)量提供了參考依據(jù)。

Objective To establish an HPLC method for simultaneous determination of gentiopicrin, loganic acid, swertiamain, sweroside, cyasterone, alisol F, alisol A, 24-acetate alisol A, and 23-acetate alisol B in Tongfengding Capsules. Methods The separation by HPLC was performed on Waters Symmetry C₁₈ column (250 mm×4.6 mm, 5 μm) with mobile phase of acetonitrile-0.1% phosphoric acid in gradient elution. The detection wavelength were set at 240 nm (for gentiopicrin, loganic acid, swertiamain, sweroside, and cyasterone) and 208 nm (for alisol F, alisol A, 24-acetate alisol A, and 23-acetate alisol B). The flow rate was 1.0 mL/min, the column temperature was 30℃, and the volume of injection was 10 μL. Results Gentiopicrin, loganic acid, swertiamain, sweroside, cyasterone, alisol F,alisol A, 24-acetate alisol A, and 23-acetate alisol B had good linear relationships in the ranges of 45.84-1 146.00, 9.02-225.50, 12.86-321.50, 4.69-117.25, 0.88-22.00, 0.59-14.75, 0.77-19.25, 0.66-16.50, and 3.37-84.25 μg/mL (r ≥ 0.999 1). The average recoveries were 100.03%, 99.55%,99.78%, 98.56%,97.98%, 96.95%, 98.21%, 97.75%, and 100.06% with the RSD values of 0.61%, 0.95%, 0.71%, 1.17%, 1.63%, 1.09%, 1.73%, 1.20%, and 0.84%. Conclusion The established method is accurate, convenient, and reproducible, which provides a reference for the comprehensive evaluation of the overall quality of Tongfengding Capsules.

R284.1

河南省中醫(yī)藥科學(xué)研究專項(xiàng)課題（2017ZY2027）