分子蒸馏纯化薰衣草精油主要成分的HS-SPME-GC分析
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摘要
目的:采用分子蒸馏法纯化薰衣草精油(LO)的挥发性成分,HS-SPME-GC法分析其化学成分。方法:在单因素的基础上,通过星点设计效应面法的设计原理,以提取物质的色谱图总峰面积为考察指标,对顶空固相微萃取的萃取温度、平衡时间、萃取时间和解吸时间进行4因素3水平响应面分析;通过正交实验,以薰衣草精油中主要组分的纯度为考察指标,对分子蒸馏的蒸馏温度、蒸馏压力和刮膜转速进行3因素3水平分析。结果:顶空固相微萃取的最佳萃取条件为萃取温度70℃、萃取时间41 min、平衡时间10 min、解吸时间6 min,在最优条件下的峰面积平均值为7750;分子蒸馏的最佳条件为蒸馏温度55℃,蒸馏压力0.6 k Pa,刮膜转速320 r·min~(-1),在最优条件下薰衣草精油中乙酸芳樟酯、芳樟醇、乙酸薰衣草酯的纯度分别为45.11%、25.52%、14.27%。结论:HS-SPME技术和分子蒸馏技术适用于薰衣草精油挥发性成分的富集纯化。
Objective: The main components of lavender essential oil( LO) of molecular distillation purification by headspace solid phase microextraction and gas chromatography( HS-SPME-GC) was studied. Methods: Based on single factor,the total peak areas of chromatogram extraction were the indexes by central composite design response surface method to analyze 4 factors and 3 levels of response surface analysis of the extraction temperature,equilibrium time,extraction time and analysis time of the headspace solid phase micro extraction. By the orthogonal experiment,the purity of main components of lavender essential oil was indicator to analyze molecular distillation of distillation temperature,distillation pressure and film speed by 3 factors and 3 levels analysis. Results: The optimum extraction conditions of headspace solid phase micro extraction were extraction temperature 70 ℃,extraction time 41 min,equilibrium time 10 min,analysis time 6 min and the average of peak area was 7750 in the optimized condition. The optimized conditions of molecular distillation were the distillation temperature of55 ℃,distillation pressure of 0.6 k Pa,film speed of 320 r·min~(-1) and the purities oflinalyl acetate,linalool,Lavandayl acetate in lavender essential oil were 45.11%,25.52%,14.27% in the optimized condition. Conclusion: HS-SPME and molecular distillation technology were applied to the enrichment and purification of volatile components of lavender essential oil.
Objective: The main components of lavender essential oil( LO) of molecular distillation purification by headspace solid phase microextraction and gas chromatography( HS-SPME-GC) was studied. Methods: Based on single factor,the total peak areas of chromatogram extraction were the indexes by central composite design response surface method to analyze 4 factors and 3 levels of response surface analysis of the extraction temperature,equilibrium time,extraction time and analysis time of the headspace solid phase micro extraction. By the orthogonal experiment,the purity of main components of lavender essential oil was indicator to analyze molecular distillation of distillation temperature,distillation pressure and film speed by 3 factors and 3 levels analysis. Results: The optimum extraction conditions of headspace solid phase micro extraction were extraction temperature 70 ℃,extraction time 41 min,equilibrium time 10 min,analysis time 6 min and the average of peak area was 7750 in the optimized condition. The optimized conditions of molecular distillation were the distillation temperature of55 ℃,distillation pressure of 0.6 k Pa,film speed of 320 r·min~(-1) and the purities oflinalyl acetate,linalool,Lavandayl acetate in lavender essential oil were 45.11%,25.52%,14.27% in the optimized condition. Conclusion: HS-SPME and molecular distillation technology were applied to the enrichment and purification of volatile components of lavender essential oil.
引文
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[13]胡震,于海莲.分子蒸馏技术精制洋葱精油及其工艺影响因素的考察[J].食品工业科技,2009(1):239-240,243.
[14]刘克海,陈秋林,谢晶,等.分子蒸馏法富集甜橙油特征香气成分[J].食品科学,2012(10):200-203.
[2]中华人民共和国卫生部药典委员会编.中华人民共和国卫生部药品标准维吾尔药分册[M].乌鲁木齐:新疆科技卫生出版社,1998:112.
[3]周广亮,宋晓琳,王志伟,等.薰衣草精油对Hep G2细胞的抗增殖作用研究[J].食品工业科技,2013(8):158-160.
[4]杨少馀,冯丽娇,罗志刚.薰衣草精油的提取及成分鉴定[J].广东化工,2007,34(9):109-112.
[5]陆宗鲁.薰衣草与香味整理[A].中国纺织工程学会、广东纺织助剂行业协会,第一届广东纺织助剂行业年会论文集[C].中国纺织工程学会、广东纺织助剂行业协会,2009:9.
[6]Hyun-Hee Lim,Ho-Sang Shin.Simple determination of4-methylimidazole in soft drinks by headspace SPME GC-MS[J].Chromatographia,2013,76:97-101.
[7]刘晓慧,张丽霞,王日为,等.顶空固相微萃取-气相色谱-质谱联用法分析黄茶香气成分[J].食品科学,2010(16):239-243.
[8]张伟,张娟娟,尹震花,等.HS-SPME-GC-MS法快速检测积雪草挥发性成分[J].中国药房,2016(33):4710-4711.
[9]Asadollahi-Baboli M,Aghakhani A,Bikdeloo V.Application of polyamide nanofibers,SPME/GC-MS,and chemometrics for comprehensive analysis of volatiles in Thymus vulgaris L.and Thymus serpyllum L.[J].Food Analytical Methods,2016,9(2):528-536.
[10]赵欣欣,张明成,陈倩,等.分子蒸馏技术在甘油二酯纯化中的应用[J].食品工业,2016(12):217-220.
[11]郭亮.超临界CO2-分子蒸馏分离纯化大蒜素的研究[D].泰安:山东农业大学,2011.
[12]李雄,吕庆银,李岑,等.分子蒸馏法纯化宽叶缬草挥发油中的乙酸龙脑酯[J].食品工业科技,2017(5):274-278.
[13]胡震,于海莲.分子蒸馏技术精制洋葱精油及其工艺影响因素的考察[J].食品工业科技,2009(1):239-240,243.
[14]刘克海,陈秋林,谢晶,等.分子蒸馏法富集甜橙油特征香气成分[J].食品科学,2012(10):200-203.