牛蒡子亚临界萃取后药渣中总木脂素的富集工艺优选

Optimization of Enrichment Process for Total Lignans from Arctii Fructus Residue After Subcritical Extraction

摘要:

目的: 优选经亚临界萃取后牛蒡子药渣中总木脂素的富集工艺,为该药材资料的开发与利用提供参考. 方法: 以牛蒡子油得率、药渣中总木脂素含量为指标,通过单因素试验考察牛蒡子亚临界萃取溶媒.采用醇提水沉法富集牛蒡子药渣中木脂素类成分,通过单因素试验优选工艺条件.采用HPLC测定牛蒡子苷和牛蒡子苷元的含量,流动相乙腈(A)-0.1%磷酸水溶液(B)梯度洗脱(0~5 min,30%~35%A;5~13 min,35%~45%A;13~15 min,45%~48%A;15~20 min,48%~53%A;20~29 min,53%~80%A;29~40 min,80%~100%A),检测波长280 nm. 结果: 选择丁烷为萃取溶媒脱脂.最佳富集工艺为加8倍量70%乙醇回流提取3次,每次1 h,滤液减压回收至0.5 g·mL^-1,按药渣量加12倍量水沉淀,煮沸回流60 min;总木脂素纯度>50%,转移率>80%. 结论: 醇提水沉法适用于牛蒡子中总木脂素部位的富集纯化,优选的工艺稳定可行.

Abstract:

Objective: To optimize enrichment technology of total lignans from Arctii Fructus residue after subcritical extraction. Method: Taking yield of Arctii Fructus oil and the content of total lignans in residue as indexes,subcritical extraction solvent of Arctii Fructus was investigated by single factor test.Total lignans in residue was enriched by alcohol extraction and water precipitation method,process parameters was optimized by single factor tests.HPLC was employed to determine contents of arctiin and arctigenin with mobile phase of acetonitrile(A)-0.1% phosphoric acid solution(B) for gradient elution(0-5 min,30%-35%A;5-13 min,35%-45%A;13-15 min,45%-48%A;15-20 min,48%-53%A;20-29 min,53%-80%A;29-40 min,80%-100%A) and detection wavelength at 280 nm. Result: Butane was selected as extraction solvent for degreasing.Optimum enrichment process was as follows:reflux extracted thrice with 8 times the amount of 70% ethanol for 1 h each time,filtrate pressure recoveried to 0.5 g·mL^-1,precipitation with 12 time the amount of water according to quantity of dregs,reflux boiling time of 60 minutes;purity of total lignans was more than 50%,transfer rate reached more than 80%. Conclusion: Alcohol extraction and water precipitation method is suitable for enrichment and purification of total lignans in Arctii Fructus,this optimized process is stable and feasible.