利胆排石片中游离蒽醌、总蒽醌和结合蒽醌的含量测定  

Determination of Free Anthraquinones, Total Anthraquinones and Conjugated Anthraquinones in Lidan Paishi Tablets

作　　者：郭琪[1] 张辉 李桂本[1] 李海燕[1] 

机构地区：[1]河南省食品药品检验所,河南郑州450003 [2]山东省药学科学院,山东济南250101

出　　处：《食品与药品》2015年第6期426-430,共5页Food and Drug

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.

关 键 词：利胆排石片 蒽醌 芦荟大黄素 大黄酸 高效液相色谱 

分 类 号：R927.2[医药卫生—药学]