氯化胆碱基低共熔萃取剂在大黄5种游离蒽醌类成分测定中的应用

HPLC Analysis of Five Free Anthraquinones Species of Rhubarbin Samples Based on the Choline Chloride-Based Deep Eutectic Extraction Solvent

以大黄药材中的主要化学组分5种蒽醌类化合物为研究对象,制备了4种氯化胆碱类低共熔性溶剂,用涡旋方法筛选出最佳的低共熔性溶剂来提取游离态蒽醌类化合物。考察了低共熔溶剂的种类、摩尔比、含水量及涡旋时间等因素对游离态蒽醌类化合物萃取量的影响。确定最佳的提取参数为氯化胆碱/三乙二醇(摩尔比1:1)作为提取溶剂,提取时间9 min,含水量为12.5%。在此条件下,芦荟大黄素、大黄素、大黄酸、大黄酚、大黄素甲醚的平均萃取量分别达到2.53±0.16 mg/g,4.67±0.23 mg/g,2.34±0.15 mg/g,5.91±0.28 mg/g和2.79±0.16 mg/g。与药典方法测定相比,提取效率更优。采用已经优化的提取条件对大黄10个批次的样品分析,5种游离蒽醌类化合物能实现基线分离,且分离度良好。

This study focused on five major anthraquinone compounds found in rhubarb medicinal herbs.Four choline chloride-based low-melting-point solvents were prepared for the extraction of free anthraquinone compounds.The optimal low-melting-point solvent was selected using a vortex method.The effects of different eutectic solvents,liquid to solid ratio,extraction time and alcohol content on the extraction efficiency of anthraquinones were studied by using a single factor test and a multi-factor and multi-level experimental design method.The results showed that lactic acid:choline chloride(molar ratio 1:1)was the best extraction solvent,the water content was 12.5%,and the extraction time was 9 minutes.Under these conditions,the average extraction rates of Aloe-emodin,Rhein,Emodin,Chrysophanol and Physcion reached 2.53±0.16 mg/g,4.67±0.23 mg/g,2.34±0.15 mg/g,5.91±0.28 mg/g and 2.79±0.16 mg/g,respectively.Compared with Chinese pharmacopoeia,this method has better extraction efficiency.The optimized extraction conditions were used to analyze 10 batches of rhubarb samples,five anthraquinones in rhubarb can be separated from each other at baseline with good resolution.