木香挥发油超声辅助提取工艺优化及其化学成分分析

Optimization of Ultrasonic Assisted Extraction of Volatile Oil from Aucklandia odorifera and Its Chemical Components Analysis

本文研究响应面法优化超声辅助法提取木香挥发油的工艺,同时并对木香挥发油成分进行研究。在单因素试验的基础上,采用Box-Behnken响应面法设计试验,运用3因素3水平,以木香挥发油的得率为响应指标,考察液料比、提取温度、超声时间对木香挥发油得率的影响;并对最佳提取工艺下超声提取的挥发油进行GC-MS分析,采用峰面积归一化法,确定各成分的相对含量并进行鉴定。结果表明最佳工艺为:料液比1:21、提取温度50℃、超声时间36 min,经验证此条件下的挥发油得率为5.60%,与理论值5.70%相比差别不大,表明此法较为准确;采用GC-MS分析所得到的挥发油成分中,共鉴定出35种化合物,占总挥发油组分的92.03%。其中相对含量较高的成分为石竹素、(-)-异芳香烃-(V)、1-甲基环庚烯、1,4-环丁二烯、4-(1-甲基戊基)-1-环己烯-1-羧醛、11,11-二甲基螺环[2,9]十二烷-3,7-二烯等,其中含量最高的为1,4-环丁二烯。因此,响应面法优选超声辅助法提取木香挥发油工艺准确、可靠;超声辅助法能应用于木香挥发油的提取。使用GC-MS法能为木香药材的质量鉴别提供较好的依据。

In this work,response surface methodology(RSM)was used to optimize the ultrasonic assisted extraction of volatile oil from Aucklandia odorifera.On the basis of single factor experiment,the box Behnken response surface method was used to design the experiment.The yield of Aucklandia volatile oil was used as the response index and the effects of liquid-solid ratio,extraction temperature and ultrasonic time on the yield of Aucklandia volatile oil were investigated.The volatile oil extracted by ultrasonic under the optimal extraction process was analyzed by GC-MS,and the peak area normalization method was used.Their content was also determined.The results showed that the optimum technical parameters were as follows:the ratio of material to liquid of 1:20,the extraction temperature of 50℃and the ultrasonic time of 36 min.The yield of volatile oil under this condition was 5.60%,which was closeto the theoretical value of 5.70%.The results showed that this method was more accurate.GC-MS analysis indicated that a total of 35 compounds were identified,accounting for 92.03%of the total volatile oil components.The components with high contents were caryophyllin,(-)-isoaromatic hydrocarbon-(V),1-methylcycloheptene,1,4-cyclobutadiene,4-(1-methylamyl)-1-cyclohexene-1-carboxylaldehyde,11,11-dimethyl spirocyclic[2,9]dodecane-3,7-diene.The content of 1,4-cyclobutadiene was highest.Therefore,the technology of ultrasonic assisted extraction of volatile oil from Radix Aucklandiae could beaccurate and reliable,and the ultrasonic assisted method could be applied to the extraction of volatile oil from Radix Aucklandiae.GC-MS method could provide a good basis for the quality identification of Radix Aucklandiae.