摘要
目的 建立利胆排石片中游离蒽醌、总蒽醌和结合蒽醌的高效液相色谱测定方法。方法 采用Phenomenex Luna 5u-C18色谱柱（4.6 mm×250 mm,5μm）,以甲醇（A）-0.1%磷酸水溶液（B）为流动相,梯度洗脱,流速1 m L/min,检测波长：254 nm。结果 各待测组分分离度良好;芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚5个成分的进样量在2.408~24.08 ng（r=0.9996）,2.718~27.18 ng（r=0.9999）,3.060~30.60 ng（r=0.9995）,4.298~42.98 ng（r=0.9999）,3.050~30.50 ng（r=0.9998）与峰面积呈良好的线性关系;游离蒽醌中芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚的加样回收率（n=6）分别为：99.1%（RSD=1.3%）,98.6%（RSD=1.1%）,99.0%（RSD=1.4%）,98.5%（RSD=0.8%）,99.7%（RSD=1.0%）;总蒽醌中芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚的加样回收率（n=6）分别为：98.4%（RSD=0.6%）,99.5%（RSD=0.9%）,98.8%（RSD=1.2%）,99.3%（RSD=0.8%）,99.1%（RSD=1.3%）。结论 经方法学验证,本方法简单、快速、灵敏、准确,可用于利胆排石片的质量控制定量分析方法。
Objective To develop an HPLC method for determination of free anthraquinones, total anthraquinones and conjugated anthraquinones in Lidan Paishi Tablets. Methods The chromatographic separation was performed on Phenomenex Luna 5u-C18 （4.6 mm × 250 mm, 5 μm） with mobile phase consisting of methanol （A） -0.1% phosphoric acid solution （B） in a gradient mode at a flow rate of 1 mL/min. The UV detection wavelength was set at 254 nm. Results Excellent chromatographic separation was achieved and the ranges for linear correlation of aloeemodin, rheim emodin, chrysophanol and physcion were 2.408-24.08 ng （r=0.9996）, 2.718-27.18 ng （r=0.9999）, 3.060-30.60 ng （r=0.9995）, 4.298-42.98 ng （r=0.9999）, 3.050-30.50 ng （r=0.9998）, respectively. Of free anthraquinones, the average recoveries （n=6） of aloeemodin, rhein, emodin, chrysophanol and physcion were 99.1% （RSD=1.3 %）, 98.6 % （RSD=1.1%）, 99.0 % （RSD=1.4 %）, 98.5 % （RSD=0.8 %）, 99.7 % （RSD=1.0 %）; of total anthraquinones, the average recoveries （n=6） were 98.4 % （RSD=-0.6 %）, 99.5 % （RSD=0.9 %）, 98.8 % （RSD=1.2 %）, 99.3 % （RSD=0.8 %）, 99.1% （RSD=-1.3 %）, respectively. Conclusion By method validation, this method is proved to be simple, rapid, sensitive and accurate. It＇s an available quantitative analysis method for quality control of Lidan Paishi Tablets.
出处
《食品与药品》
CAS
2015年第6期426-430,共5页
Food and Drug
