HPLC波长切换技术同时测定复方黄连素片中6个成分的含量

Simultaneous determination of the content of 6 components in Fufang Huangliansu tablets by HPLC wavelength switching technology

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.