绿色低共熔溶剂提取互叶白千层精油及成分分析

Extraction and component analysis of essential oil of Melaleuca alternifolia by green deep eutectic solvents

关键词:  互叶白千层, 精油, 低共熔溶剂, 提取, 成分分析

Key words:  Melaleuca alterniflora, essential oil, deep eutectic solvents(DESs), extract, component analysis

摘要:

为探究绿色低共熔溶剂提取互叶白千层精油的最佳工艺,该研究采用四种提取工艺作对比,并在单因素实验的基础上结合响应面进行了工艺优化,利用气相色谱-质谱法(GC-MS)对四种工艺提取到的互叶白千层精油进行了比较分析。结果表明:(1)互叶白千层精油最佳提取工艺为干燥原料低共熔溶剂蒸馏,最优提取条件为氯化胆碱与1,3-丁二醇摩尔比1:3、含水量52 mol、原料干燥时间9 h、料液比1:5 g·mL^-1、蒸馏时间60 min,在此条件下所得提取率为4.06%,实验值与响应面模型的预测值有较好的拟合性,证实模型有效,提取率比新鲜原料水蒸气蒸馏、干燥原料水蒸气蒸馏和冻融原料水蒸气蒸馏分别提高了383.33%、290.38%和497.06%。(2)经四种工艺提取所得精油主要成分大致相同,但含量差距很大,主要有醇类和烯烃类物质。(3)干燥原料低共熔溶剂蒸馏的精油提取率和特征组分含量都高于其他工艺,包括醇类8种,烯烃类9种,其他化合物3种; 主要成分为γ-松油烯、松油烯、α-蒎烯、α-松油醇、香树烯,其中烯烃类化合物相对含量最大,为45.31%; 特征组分松油烯-4-醇含量为30.58%,桉叶油醇为0.12%。该研究为互叶白千层的资源开发和天然产物的绿色提取提供了数据支撑。

Abstract:

In order to explore the best extraction process of essential oil of Melaleuca alternifolia by green deep eutectic solvents, four different extraction processes were compared including fresh-steam distillation extraction, dry-steam distillation extraction, freeze thawing-steam distillation extraction and deep eutectic solvents-distillation extraction. The effects of liquid-material ratio, distillation time, molar ratio of deep eutectic solvents, raw material drying time, water content on extraction rate of essential oil of M. alternifolia were investigated by single factor test. Based on single-factor tests, the quadratic regression parasitism model was established through the response surface methodology. The essential oil of M. alternifolia was determined by gas chromatography-mass spectrometry(GC-MS). The results were as follows:(1)Deep eutectic solvents-distillation extraction was the best extraction processes. The optimal extraction conditions were determined to be molar ratio of choline chlorid to 1,3-Butanediol 1:3(mol:mol), water content 52 mol, drying time of raw materials 9 h, material-liquid ratio 1:5 g·mL^-1, distillation time 60 min, and the maximum extraction rate of essential oil of M. alternifolia reached 4.06%, which was 383.33%, 290.38% and 497.06% higher than that of fresh-steam distillation extraction, dry-steam distillation extraction and freeze thawing-steam distillation extraction, respectively. Response surface methodology was proved to be applicable for extraction of essential oil from M. alternifolia, the experimental results were in good agreement with the predicted values of the response surface model.(2)The main components of essential oil of M. alternifolia extracted by four different extraction processes were proved to be almost same, while the contents were signifcanthy different.(3)Alcohols and alkenes were confirmed to be the main components in the essential oil of M. alternifolia. The extraction yield and characteristic component content of essential oil of M. alternifolia extracted by deep eutectic solvents-distillation were indicated much higher than those by other three processes,which including eight alcohols, nine alkenes and three other compounds, with the main components of γ-Terpinene,α-Terpinene,α-Pinene,α-Terpineol and alloaromadendrene, and the relative content of alkenes was 45.31%, the content of Terpinen-4-ol and eucalyptol was 30.58% and 0.12%. This study provides the data supporte for the further utilization of M. alternifolia and green extraction of natural products.