目的:建立HPLC法同时测定复方黄连素片中芍药苷、吴茱萸内酯、吴茱萸碱、吴茱萸次碱、木香烃内酯、去氢木香内酯的含量。方法:采用Kromasil C18色谱柱(250 mm×4.6 mm,5 μm),以乙腈(A)-0.033 mol·L-1磷酸二氢钾溶液(B)为流动相,梯度洗脱(0~15 min,9%A;15~55 min,9%A→35%A),柱温和流速分别为35℃和1 mL·min-1,波长切换(0~25 min,在230 nm波长下检测芍药苷;26~50 min,在215 nm波长下检测吴茱萸内酯、吴茱萸碱、吴茱萸次碱、木香烃内酯和去氢木香内酯)。结果:芍药苷、吴茱萸内酯、吴茱萸碱、吴茱萸次碱、木香烃内酯和去氢木香内酯进样量分别在0.1285~1.285、0.2008~2.008、0.1139~1.139、0.1151~1.151、0.1186~1.186和0.1034~1.034 μg范围内与色谱峰峰面积呈良好线性响应;平均回收率(n=6)分别为99.4%、98.6%、98.7%、98.9%、98.9%和98.6%,RSD分别为0.46%、0.64%、0.60%、1.1%、0.61%和0.38%。结论:该方法多种成分同时测定,操作简便、准确,重复性好,可用于复方黄连素片的质量控制。
Objective: To develop an HPLC method for simultaneously determining 6 components in Fufang Huangliansu tablets. Methods: The quantitative analysis was carried out on a column of Kromasil C18(250 mm×4.6 mm,5 μm) by simultaneous HPLC wavelength switching method,using a mobile phase of acetonitrile(A)-0.033 mol·L-1 potassium phosphate monobasic solution(B) by a gradient eluted program(0-15 min,9%A;15-55 min,9%A→35%A) with a flow rate of 1 mL·min-1 at 35℃.The detection wavelength was set at 230 nm for paeoniflorin in the first 25 min,and then changed to 215 nm for evodine,evodiamine,rutaecarpine,costunolide and dehydrocostuslactone between 26 and 50 min. Results: The linear ranges of paeoniflorin,evodine,evodiamine,rutaecarpine,costunolide and dehydrocostuslactone fell within the ranges of 0.1285-1.285 μg,0.2008-2.008 μg,0.1139-1.139 μg,0.1151-1.151 μg,0.1186-1.186 μg,0.1034-1.034 μg,respectively.The recoveries(n=6) of paeoniflorin,evodine,evodiamine,rutaecarpine,costunolide and dehydrocostuslactone were 99.4%,98.6%,98.7%,98.9%,98.9%,and 98.6%,respectively,and the relative standard deviations were 0.46%,0.64%,0.60%,1.1%,0.61%,0.38%,respectively. Conclusion: This method is simple,accurate,reproducible and convenient for the quality control of Fufang Huangliansu tablets.