薰衣草油提取工艺的研究
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摘要
薰衣草(Lavender)是唇型科薰衣草属植物,为多年生亚灌木。主要产于法国,意大利,英国,澳大利亚等国家。我国的新疆,陕西等地有广泛栽培。本研究以新疆伊犁地区的薰衣草为试验材料,采用超声波辅助溶剂萃取,微波辅助溶剂萃取以及超临界CO_2流体萃取技术提取薰衣草油,并对其提取率进行比较,确定最佳工艺条件,主要结果如下:
在单因素试验的基础上,选择物料粒度,溶剂用量,超声时间三个因素,以提取率和油脂的清亮度为评价指标,进行超声波萃取薰衣草油工艺的正交试验。试验结果显示,超声波辅助溶剂萃取的最佳工艺参数为:物料粒度60目,料液比1:12,超声时间30min,提取率为1.09%±0.02%。
在单因素试验的基础上,选择辐射时间,微波功率,溶剂用量,萃取温度四个因素,以提取率和油脂的清亮度为评价指标,进行微波萃取薰衣草油工艺的正交试验。试验结果显示,微波辅助溶剂萃取的最佳工艺参数:辐射温度40℃,料液比1:10,微波功率700W,辐射时间350s;提取率为2.06%±0.02%。
在单因素试验的基础上,选择萃取压力,萃取温度,萃取时间,CO_2流量四个因素,以提取率和油脂的清亮度为评价指标,进行超临界CO_2流体萃取薰衣草工艺的正交试验,试验结果显示,超临界CO_2流体萃取的最佳工艺参数:萃取压力20MPa,萃取温度45℃,CO_2流量15L/h,萃取时间160min,提取率为4.497%±0.02%。
通过提取率以及提出油的质量比较,发现超临界流体萃取具有工艺流程简单,萃取效率高,产品纯净,无污染等特点,为萃取薰衣草油的最佳工艺,并对其最佳工艺进行放大试验研究,结果与小试实验结果基本一致,反映了小试实验数据和工艺参数的可靠性和稳定性,并采用气相色谱-质谱联用仪(GC-MS)对超临界CO_2流体萃取的薰衣草油的成分进行分析,为萃取工艺直接在工业化上的应用提供依据并起到一定的指导作用。
Lavender is one piece of labiate Lavender genus plant, which can be found in France, Italia, England, Australia and so on. And in China it is broadly planted in Xin jiang, Shan xi and so on. In this paper, Lavender from Yi li of Xin jiang has been taken as the experiment material. Oil was extracted from Lavender by ultrasonic, microwave and supercritical carbon dioxide and composition of oil was determined. The main results are listed as follow:
The influence of mess of particle size, rate of material and liquid, time of ultrasonic on the oil′s yield and oil transparency was studied by orthogonal layout. The optimal extract process of ultrasonic were achieved when the mess of particle size was 60 mesh, the rate of material and liquid was 1:12 ,the time of ultrasonic was 30min, the rate of extraction was 1.09%±0.02%.
The influence of temperature of radiation, rare of material and liquid, power of microwave, time of radiation on the oil′s yield and oil transparency was studied by orthogonal layout. The optimal extract process of microwave were achieved when temperature of radiation was 40℃, the rare of material and liquid was 1:10, power of microwave was 700w, time of radiation was 350s, the rate of extraction is 2.60%±0.02%.
The influence of extraction pressure, the extraction temperature, CO_2 flowing rate, extraction time on the oil′s yield and oil transparency was studied by orthogonal layout. The optimal extract process of supercritical carbon dioxide were achieved when the extraction pressure was 20mpa,the extraction temperature was 45℃, CO_2 flowing rate was 15L/h,the extraction time was 160min , the rate of extraction is 4.497%±0.02%.
Through the comparison of the rate of extraction and the quality of oil, I found Supercritical carbon dioxide extraction has many characteristic: simple process, high purity and high efficiency. So it was the optimal extracting process. And the optimal extract process in laboratory-scale was blow up to pilot scale successfully and results were accord with laboratory-scale. And gas chromatography-mass spectrometry (GC/MS) was used for the determined of the composition of the oil. It is proved that the extract process in laboratory-scale was reliable and stable.
在单因素试验的基础上,选择物料粒度,溶剂用量,超声时间三个因素,以提取率和油脂的清亮度为评价指标,进行超声波萃取薰衣草油工艺的正交试验。试验结果显示,超声波辅助溶剂萃取的最佳工艺参数为:物料粒度60目,料液比1:12,超声时间30min,提取率为1.09%±0.02%。
在单因素试验的基础上,选择辐射时间,微波功率,溶剂用量,萃取温度四个因素,以提取率和油脂的清亮度为评价指标,进行微波萃取薰衣草油工艺的正交试验。试验结果显示,微波辅助溶剂萃取的最佳工艺参数:辐射温度40℃,料液比1:10,微波功率700W,辐射时间350s;提取率为2.06%±0.02%。
在单因素试验的基础上,选择萃取压力,萃取温度,萃取时间,CO_2流量四个因素,以提取率和油脂的清亮度为评价指标,进行超临界CO_2流体萃取薰衣草工艺的正交试验,试验结果显示,超临界CO_2流体萃取的最佳工艺参数:萃取压力20MPa,萃取温度45℃,CO_2流量15L/h,萃取时间160min,提取率为4.497%±0.02%。
通过提取率以及提出油的质量比较,发现超临界流体萃取具有工艺流程简单,萃取效率高,产品纯净,无污染等特点,为萃取薰衣草油的最佳工艺,并对其最佳工艺进行放大试验研究,结果与小试实验结果基本一致,反映了小试实验数据和工艺参数的可靠性和稳定性,并采用气相色谱-质谱联用仪(GC-MS)对超临界CO_2流体萃取的薰衣草油的成分进行分析,为萃取工艺直接在工业化上的应用提供依据并起到一定的指导作用。
Lavender is one piece of labiate Lavender genus plant, which can be found in France, Italia, England, Australia and so on. And in China it is broadly planted in Xin jiang, Shan xi and so on. In this paper, Lavender from Yi li of Xin jiang has been taken as the experiment material. Oil was extracted from Lavender by ultrasonic, microwave and supercritical carbon dioxide and composition of oil was determined. The main results are listed as follow:
The influence of mess of particle size, rate of material and liquid, time of ultrasonic on the oil′s yield and oil transparency was studied by orthogonal layout. The optimal extract process of ultrasonic were achieved when the mess of particle size was 60 mesh, the rate of material and liquid was 1:12 ,the time of ultrasonic was 30min, the rate of extraction was 1.09%±0.02%.
The influence of temperature of radiation, rare of material and liquid, power of microwave, time of radiation on the oil′s yield and oil transparency was studied by orthogonal layout. The optimal extract process of microwave were achieved when temperature of radiation was 40℃, the rare of material and liquid was 1:10, power of microwave was 700w, time of radiation was 350s, the rate of extraction is 2.60%±0.02%.
The influence of extraction pressure, the extraction temperature, CO_2 flowing rate, extraction time on the oil′s yield and oil transparency was studied by orthogonal layout. The optimal extract process of supercritical carbon dioxide were achieved when the extraction pressure was 20mpa,the extraction temperature was 45℃, CO_2 flowing rate was 15L/h,the extraction time was 160min , the rate of extraction is 4.497%±0.02%.
Through the comparison of the rate of extraction and the quality of oil, I found Supercritical carbon dioxide extraction has many characteristic: simple process, high purity and high efficiency. So it was the optimal extracting process. And the optimal extract process in laboratory-scale was blow up to pilot scale successfully and results were accord with laboratory-scale. And gas chromatography-mass spectrometry (GC/MS) was used for the determined of the composition of the oil. It is proved that the extract process in laboratory-scale was reliable and stable.
引文
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[3] 麦秋君.桂花油化学成分分析[J].广东工业大学学报,2000,17(1):73-75
[4] 胡文,何静,樊永明等.植物性天然香料及其提取技术[J].精细与专用化妆品,2004,12(6):6一9
[5] 何坚,孙宝国.香料化学与工艺学[M].北京:化学工业出版社,2004(4):30一32
[6] 董丽,邢钧,吴采樱.香精香料的分析进展[J].分析科学学报,2003(4)19(2):188-191
[7] 董丽萍,许松林.天然香料的提取分离技术.天津化工,2006(9)20(5):1-4
[8] 赵华,张金生,李丽华.植物油提取技术的进展.2006(12) 26(4):137-140
[9] 高献礼,李超.植物性香料提取技术的研究进展.中国食品添加剂,2006(9):134,246-249
[10] 陈行烈,翟建军,赵凡智等.新疆薰衣草油化学成分的研究[J].新疆大学学报,,1991:81-84
[11]解成喜等.薰衣草挥发油化学成分的 GC-MS 分析.新疆大学学报(自然科学版),2002(8),19(3):294-296
[12] Liao WC,Landis CA,Lentz MJ,et al.Effect of foot bathing on distal proximal skin temperature gradient in elders[J].International Journal of Nursing Studies,2005,42(7):717-722
[13] Louis M, Kowalski S D. Use of aromatherapy with hospital patients to decrease pain 、anxiety and depression and to promote an increase sense of well-being[J]. Am J Hosp Palliat Care,2002,19(6):381-386
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