基于正交设计优化新鲜川芎中挥发油提取工艺  

Extraction process optimization of volatile oil from freshLigusticum chuanxiong based on orthogonal design

作　　者：李超 刘云华[1] 秦登云 黄志芳[1] 刘玉红[1] 陈燕[1] 易进海[1,2] LI Chao;LIU Yun-hua;QIN Deng-yun;HUANG Zhi-fang;LIU Yu-hong;CHEN Yan;YI Jin-hai(Sichuan Provincial Key Laboratory of Quality and Innovation Research of Chinese Materia Medica,Sichuan Academy of Chinese Medicine Sciences,Chengdu 610041,China;School of Pharmacy of Southwest Medical University,Luzhou 646000,China)

机构地区：[1]四川省中医药科学院中药材品质及创新中药研究四川省重点实验室,成都610041 [2]西南医科大学药学院,泸州646000

出　　处：《天然产物研究与开发》2024年第5期771-778,共8页Natural Product Research and Development

基　　金：国家中医管理局-中央财政转移支付地方项目(A-2023N-8);四川省科技厅重点实验室中药材品质及创新中药研究项目(A-2022N-47);科研院所科技成果转化项目(24YSZH0021)。

摘　　要：为优化川芎挥发油提取工艺,建立以新鲜川芎为原料提取制备挥发油的新方法,采用正交试验设计对乙醇回流提取工艺条件进行优化,并进一步考察优选回收浓缩、油水分离等关键工艺参数。以藁本内酯和洋川芎内酯A作为指标成分,应用HPLC一测多评法进行含量测定。以提取量、油收率、油含量为评价指标,最终确定川芎挥发油提取制备新方法为:鲜川芎切片,加8倍量70%乙醇回流提取2次(以干药材计,第一次需测定鲜川芎水分,调节乙醇浓度为70%),每次1.5 h,滤液回收浓缩至2.0~3.0 g生药/mL,静置过夜,弃去水层,上层乳化层加热至60℃离心,分取油层,余下乳化层再加氯化钠至饱和并加热至60℃离心,合并油层,即得川芎挥发油。新方法所得川芎挥发油收率约为3%,藁本内酯和洋川芎内酯A含量达70%。该研究所建立的新方法生产设备要求低、操作简便易行,可实现川芎挥发油的高效制备,且含量高、品质优,为川芎挥发油的工业化生产提供了新思路和新方法。In order to optimize the extraction process of Ligusticum chuanxiong volatile oil,this study established a new method to extract volatile oil from fresh L.chuanxiong which used orthogonal experimental design to optimize the extraction process conditions of ethanol reflux,and further investigated the key process parameters such as recovery concentration and oil-water separation.With the ligustilide and senkyunolide A as index components,the content was determined by quantitative analysis of multi-components by single-marker(QAMS).and the extraction amount,oil yield and oil content were evaluated as evaluation indexes.Finally,the new extraction and preparation method of L.chuanxiong volatile oil was determined as follows:Slice fresh L.chuanxiong,add 8 times the amount of 70%ethanol to extract it by reflux twice(calculated with reference to the dried drug,the moisture of fresh L.chuanxiong should be measured for the first time,and the ethanol concentration should be adjusted to 70%)for 1.5 hour each time,then recover and concentrate the filtrate to 2.0-3.0 g crude medicine/mL,left for overnight.Discarded the water layer,heat the upper emulsified layer to 60℃,centrifuge,and then separate the oil layer.Add sodium chloride to the remaining emulsified layer to saturation,then heat to 60℃and centrifuge.L.chuanxiong volatile oil is obtained by combining two centrifugal oil layers.The yield of L.chuanxiong volatile oil was about 3%,and the total amount of ligustilide and senkyunolide A was 70%.This research established a new method which has low production equipment requirements,simple operation,and can realize the efficient preparation of the L.chuanxiong volatile oil with high content and excellent quality.Therefore,it provides a new idea and a new method for the industrial production of L.chuanxiong volatile oil.

关 键 词：新鲜川芎 挥发油 乙醇提取 正交试验 制备工艺 

分 类 号：R932[医药卫生—生药学]