当归酚酸类成分提取、富集工艺研究

Extraction and enrichment process of phenolic acids in Danggui (Radix Angelicae Sinensis)

目的优选当归中酚酸类成分提取、富集工艺。方法以当归酚酸类成分中阿魏酸为指标物质,按照L9(34)正交设计表的条件进行试验,考察乙醇浓度、溶剂倍量、提取时间和提取次数对提取效果的影响,优选提取工艺。再通过考察大孔树脂的种类、树脂径高比、上样液性质、洗脱流速等参数,优选富集工艺。结果最终优选的当归中酚酸类成分的提取、富集工艺为:70%乙醇,8倍量,回流提取2次,每次1 h,将提取液合并浓缩至0.5 g/mL,4 500 r/min,离心30 min,取下清液,上HPD-400型大孔吸附树脂,上样量为4.5 g/mL树脂,吸附流速0.5 mL/min,径高比为1∶7,蒸馏水3倍柱体积(BV)、20%乙醇2 BV除杂,除杂流速1 mL/min,50%乙醇6 BV进行洗脱,洗脱流速2mL/min。结论采用本文优选的提取、富集工艺,得到的富集物中阿魏酸含量为151.8 mg/g,相较于当归药材、当归粗提物,有较大幅度的提高,且工艺稳定、可行。

Objective To optimize the extraction and enrichment process of phenolic acids in Danggui （Radix Angelieae Sinensis）. Methods The experiment was carried out taken ferulic acid as indicator according to the condition in L9 （34） orthogonal design table for investigating the influences of ethanol concentration, solvent amount and duration and frequency of extraction on extraction results and optimizing extraction process. The enrichment process was optimized through investigating the types of macroporous resins, ratio of diameter to height, pH and concentration of sample solution, maximum volume of sample, washed volume, ethanol concentration and volume for eduleoration and elution and flow velocity. Results The final preferred extraction and enrichment process of phenolic acids in Danggui was as follows ： 8 times amount of 70% ethanol, reflux extracting for 2 times, 1 hour each time, combining and concentrating extracts to 0.5 g/mL, eentrifugating for 30 min （4 500 r/min）, supernatant putting in HPD-400 macroporous resins, sample amount being 4.5 g/mL, adsorption flow velocity being 0.5 mL/min, ratio of diameter to height being 1：7, distilled water （3 BV） and 20% ethanol （2 BV） for edulcoration, flow velocity of edulcoration being 1 mL/min, 50% ethamol （6 BV） for elution, and flow velocity of elution being 2 mL/min. Conclusion The content of ferulic acid is 151.8 mg/g in concen- trates after enriched with the extraction and enrichment process optimized in the paper, and the process is stable and viable.