三种提取方法对红花椒挥发性成分的影响

Effect of Three Extraction Methods on the Volatile Components of Zanthoxylum bungeanum

为探究不同提取方法以及不同提取参数对花椒提取物挥发性物质组成的影响,以红花椒为原料,通过油浸法浸提、水蒸气蒸馏及超临界CO2萃取获得花椒提取物,采用固相微萃取与气相色谱质谱联用法测定花椒提取物中挥发性物质种类及含量,并通过主成分分析法及相对气味活度值评价提取物品质。对三种提取方法鉴定出的挥发性物质总数进行统计,发现油浸法、水蒸气蒸馏法和超临界CO2萃取法提取物中分别鉴定出挥发性物质65种、100种和82种。超临界CO2萃取法得到花椒提取物中挥发性物质含量最高为13909.90μg/mL、水蒸气蒸馏法次之为1152.61μg/mL、油浸法最低为249.38μg/mL,对香气物质进行主成分分析发现各组得分与香气物质总含量在各单因素条件下的变化趋势相同。其中油浸法在料液比1∶5、浸提时间5 h、浸提温度140℃时,水蒸气蒸馏法在料液比1∶10、浸提时间2 h时,超临界CO2萃取法在乙醇添加量7%、乙醇添加比例85%时挥发性物质总含量及香气物质综合得分最高。相对气味活度值结果表明三种提取方法样品关键香气物质不同,油浸法样品中月桂烯对香气贡献最大,水蒸汽蒸馏法样品中芳樟醇与桉树醇对香气贡献最大,超临界CO2萃取法样品中芳樟醇对香气贡献最大。综上所述,提取方法的差异会导致挥发性物质,特别是关键香气物质种类与含量的显著变化,超临界CO2萃取法提取物中挥发性物质与香气物质含量高于其他两种提取方法。

The experiment was carried out by using Zanthoxylum bungeanum as raw material and extraction of Zanthoxylum bungeanum by oil extraction,steam distillation and supercritical CO 2 extraction.The purpose of this experiment is to explore the effect of different extraction methods and different extraction parameters on volatile components of Zanthoxylum bungeanum extract.In addition,solid phase micro-extraction(SPME)combined with gas chromatography-mass spectrometry(GC-MS)was employed to determine the volatile substances and content in Zanthoxylum bungeanum extract.The quality evaluation of extract were analyzed by principal component analysis(PCA)method and relative odor activity value(ROAV).Under all conditions,65,100 and 82 kinds of volatile substances were identified by oil extraction,steam distillation and supercritical CO 2 extraction respectively.The highest content of volatile substances was obtained by supercritical CO 2 extraction,followed by steam distillation and oil extraction,13909.90,1152.61 and 249.38μg/mL,respectively.The results of principal component analysis showed that the change trend of the scores of each group was the same as that of the total content of aroma substances under each single factor condition.Among them,oil extraction,steam distillation and supercritical CO 2 extraction had the highest total content of volatile matter and the highest comprehensive score of aroma matter when the ratio of material to liquid was 1∶5、the extraction time was 5 h、and the extraction temperature was 140℃,the ratio of material to liquid was 1∶10、the extraction time was 2 hours,and 7%ethanol addition、the ratio of ethanol was 85%,respectively.According to the value of relative odor activity,the key aroma components of the three extraction methods were different.Laurene contributes the most to the aroma in the oil extraction method,linalool and eucalyptus alcohol contribute the most to the aroma in the steam distillation method,and linalool contributes the most to the aroma in the supercritical CO 2 extraction method.In conclusion,the differences of extraction methods lead to significant changes in the types and contents of volatile substances and key aroma components in Zanthoxylum bungeanum extracts.The content of volatile substances and aroma components in supercritical CO 2 extracts are both the highest among the three methods.