有机试剂法制备羟基红花黄色素A

Preparation of HSYA by Organic Reagent Method

目的初探有机试剂法制备HSYA的最优工艺。方法本文采用高效液相法,以HSYA含量为指标,比较冷提、热提、超声提取的提取效果,采用正交试验优选最佳提取工艺,考察沉淀试剂及用量,并考察不同除杂方式的效果。结果最佳制备工艺为:14倍量DMSO常温避光搅拌30min除杂,抽滤;滤渣加入14倍量DMSO浸泡1h,在80℃下,密闭热提50min,抽滤,滤渣加入12倍量DMSO,在80℃下,密闭热提50min,抽滤,合并滤液;滤液加入3倍量乙酸丁酯,离心,沉淀用适量乙醇洗涤,干燥,最终沉淀物纯度为14.56%。结论本实验首次以非水溶媒为提取溶剂制备HSYA。该工艺具有操作简单、经济、环保等优点,且为热敏性物质提供了常温浓缩的方法,为HSYA的工业化生产和新药开发提供了实验依据。

OBJECTIVE In this study,we aimed to preliminaryly study on the extraction and purification method of SY by organic reagent method. METHODS The content of HSYA was determined by HPLC,with the content of HSYA as the index. The optimum extraction of HSYA was determined by comparing the extraction effects of cold extraction,heating extraction and ultrasonic extraction and using orthogonal test. The precipitation reagent,dosage and the effect of impurity removal were investigated. RESULTS The optimum preparation of HSYA was as follows：Stirred 14 times the amount of DMSO at room temperature to avoid light for 30 min,impurity removal,filtered. The filter residue added 14 times the amount of DMSO to soaking for an hour,heating extraction in seal conditon at 80℃ for50 min,filtered. Then the filter residue again added 12 times the amount of DMSO,heating extraction in seal conditon at 80℃ for 50 min. Filtered and combined the filtrate. The filtrate added 3 times of the amount of butyl acetate,centrifuged. Washed the precipitate with ethanol,dried. The purity of precipitate was 14. 56%. CONCLUSION In this study,the first use of organic reagents prepared HSYA. This method is simple,economical and environment-friendly,etc…and provides a method for concentration of heat-sensitive substances at room temperature. And the thermal stability of HSYA was improved. It provides an experiment evidence for the industrial production and the new medicament research of HSYA.