超声波与半仿生提取艾叶挥发油及成分分析
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摘要
艾叶(Folium Aretm isiae Argyi)是多年生菊科草本植物艾(Aretem isia argyi levt et Vant)的干燥叶,具有浓烈的香气,其挥发油不仅具有抑菌抗炎、抗病毒、平喘、镇咳、祛痰、止血等功能,而且是香料工业、食品工业及化学工业的重要原料。对于挥发油的提取,已研究报道了以活性离子水浸提-乙醚为吸收剂的水蒸气蒸馏法、超临界CO_2萃取法、微波萃取、以乙酸乙酯或二氯甲烷为吸收剂的水蒸气蒸馏法、直接水蒸气蒸馏法、溶剂萃取法等方法,在挥发油的提取率和有效组分数量上取得了一定的进展,但研究有效的提取方法或工艺,提高产率和提取速度,减低能耗等方面,还有较大的研究潜力。
本文通过采用半仿生法(Semi-bionic Extraction method,简称SBE法)浸提-水蒸气蒸馏和经超声波破壁后选取异丙醇抽提-水蒸气蒸馏提取方法对艾叶挥发油的提取进行研究,采用气相色谱-质谱联用仪结合标准图谱和文献分析其化学组分。
实验结果表明:半仿生法浸提和超声波破壁后经异丙醇抽提-水蒸气蒸馏提取两种方法提取的挥发油有22种成分相同,为邻苯二甲酸酐-1,3-异丙呋喃二酮、2-甲基-5(1-甲基乙基)-2-环己醇、双环[2,2,1]-2-庚醇、二环大根香叶烯、蛇床烷-6-烯-4-醇、β-筚澄茄烯、β-石竹烯、邻苯二甲酸、3-胆甾烷酮、2-(亚胡椒基氨)安替比林、δ-杜松烯、α-巴草烯、3-(苯甲酰巯)-2-甲酸丙酯、β-木香醇等。
采用SBE法浸提-水蒸气蒸馏产油率为1.05%,较直接蒸馏水蒸馏提高0.3%。半仿生法浸提的挥发油共检出33个成分,其中11个成分是直接水蒸气蒸馏获得的样品中所没有的组分,为桉树脑、薄荷酮、(-)-乙酸龙脑酯、1,3-(2-氢)-二酮-2-氨基-1氢-1-吲哚、邻苯二甲酸单乙酯、菊槐酮、顺-异丁子香酚、α-紫穗槐烯、石竹烯醇、11,15-二甲基三十五烷。文献中α-侧柏烯、β-蒎烯、1-辛烯-3-醇、β-芹子烯等萜烯类却未检出。
采用超声波破壁后经异丙醇萃取结合水蒸气蒸馏技术提取艾叶的挥发性成分较直接水蒸气蒸馏技术提取的成分多,能获得高提取率的组分邻苯二甲酸单乙酯、1-氢-茚-1,2,3-三酮、3,4-二甲基环己醇,这些组分是以前研究工作没有报道过。但对一些较低挥发性成分的提取效率不高,要更好地提取艾叶的挥发性成分,采用SBE法浸提-水蒸气蒸馏提取技术能提高对较低挥发性成分的提取效率。
Folium Aretm isiae Argyi,with given other names including Artemisia lavandulaefolia,Artemisiasantolina Schrenk and Argy Wormwood Leaf,is a kind of dried leaves.It smells strong aromatic and the volatile oil extracted can not only function as anti-inflammatory, anti-virus,Antitussive,expectorant,antiasthmatic,and haemostats,but also play important roles in the spice industry,food industry and chemical industry.Taking account of high Pharmacology value on its volatile oil application,the researches into ways to extract volatile oil from it have been paid increasing interest.Some kinds of extraction methods have been reported on how to get its volatile oil to some extend.Summarily, the extraction methods introduced include steam distillation based on activated ion-water as extractant and ether as absorbent,extraction based on supercritical fluidic carbon dioxide,extraction under microwave at appropriate wavelength,steam distillation directly,steam distillation based on acetic ester or dichloroethane as absorbents,solvent extraction. It could be concluded that some progresses have been made on the extraction yield and the number of components.However,it is worth to develop new way regarding the higher extraction yield,extraction rate and energy saving.
Semi-Bionic Extraction technique(briefly,termed as SBE)is a new kind of technique for extraction useful components from Chinese medicine(herb).The thesis carried out studies on both the SBE-coupling steam distillation and isopropyl extraction-coupling steam distillation to extract volatile oil.The analysis of components in extracted oil has been taken on GC-MS.
The experiment result shows that there are 22 chemical components similar in extraction oil obtained by either SBE-coupling steam distillation or isopropyl extraction-coupling steam distillation after ultrasonic treatment.These components are phthalic anhydride -1,3-asopropyl furandione、2-methyl-5(1-methylethyl)-2-cyclohexanol、 bicyclo[2,2,1]-2-heptanol、bicyclogermacrene、selinane-6-ene-4-ol、β-cubebene、β-caryophyllene、o-phthalic acid、cholestan-3-one、2-(piperonilidene amino)antipyrine、δ-cadinene、α-humulene、3-(benzothioylthio)-2-formic acetate、β-costol,et al.
The resulting yield of the so-extraction was measured as 1.05%, which is about 0.3%higher than that by applying the steam distillation directly.The GC-MS analysis shows that 43 chemical were given from so-extracted volatile oil and 11 of them were absent from the volatile oil,extracted by the steam distillation directly,such as eucalyptole, piperitone,(-)-bornyl acetate,1,3-(2-H)-dimone-2-amino-1H-1-indole; phthalic acid monoethy ester,chrysanthenone,cis-isoeugenol,α-amorphene,caryophyllenol,11,15-dimethyl 35ane.Some chemical components such asα-thujone、β-pinene、1-octen-3-ol、β-selinene,et al didn't be checked.
It is concluded from our studies that the number of components obtained from isopropyl-extraction coupling- steam distillation are more than that obtained by steam distillation.The components with high extraction yield such as phthalic acid monoethy ester、1H-indene-1,2,3-trione、3,4-dimethyl cyclohexan-ol have been present in the extraction oil by isopropyl-extraction coupling- steam distillation, which were absent in extraction oil by extraction methods reported previously.However,the isopropyl-extraction coupling- steam distillation was not good regarding extraction yield of the high volatile components. For high volatile component extraction,SBE-coupling steam distillation would be applied to improve the extraction yield of these high volatile components.
本文通过采用半仿生法(Semi-bionic Extraction method,简称SBE法)浸提-水蒸气蒸馏和经超声波破壁后选取异丙醇抽提-水蒸气蒸馏提取方法对艾叶挥发油的提取进行研究,采用气相色谱-质谱联用仪结合标准图谱和文献分析其化学组分。
实验结果表明:半仿生法浸提和超声波破壁后经异丙醇抽提-水蒸气蒸馏提取两种方法提取的挥发油有22种成分相同,为邻苯二甲酸酐-1,3-异丙呋喃二酮、2-甲基-5(1-甲基乙基)-2-环己醇、双环[2,2,1]-2-庚醇、二环大根香叶烯、蛇床烷-6-烯-4-醇、β-筚澄茄烯、β-石竹烯、邻苯二甲酸、3-胆甾烷酮、2-(亚胡椒基氨)安替比林、δ-杜松烯、α-巴草烯、3-(苯甲酰巯)-2-甲酸丙酯、β-木香醇等。
采用SBE法浸提-水蒸气蒸馏产油率为1.05%,较直接蒸馏水蒸馏提高0.3%。半仿生法浸提的挥发油共检出33个成分,其中11个成分是直接水蒸气蒸馏获得的样品中所没有的组分,为桉树脑、薄荷酮、(-)-乙酸龙脑酯、1,3-(2-氢)-二酮-2-氨基-1氢-1-吲哚、邻苯二甲酸单乙酯、菊槐酮、顺-异丁子香酚、α-紫穗槐烯、石竹烯醇、11,15-二甲基三十五烷。文献中α-侧柏烯、β-蒎烯、1-辛烯-3-醇、β-芹子烯等萜烯类却未检出。
采用超声波破壁后经异丙醇萃取结合水蒸气蒸馏技术提取艾叶的挥发性成分较直接水蒸气蒸馏技术提取的成分多,能获得高提取率的组分邻苯二甲酸单乙酯、1-氢-茚-1,2,3-三酮、3,4-二甲基环己醇,这些组分是以前研究工作没有报道过。但对一些较低挥发性成分的提取效率不高,要更好地提取艾叶的挥发性成分,采用SBE法浸提-水蒸气蒸馏提取技术能提高对较低挥发性成分的提取效率。
Folium Aretm isiae Argyi,with given other names including Artemisia lavandulaefolia,Artemisiasantolina Schrenk and Argy Wormwood Leaf,is a kind of dried leaves.It smells strong aromatic and the volatile oil extracted can not only function as anti-inflammatory, anti-virus,Antitussive,expectorant,antiasthmatic,and haemostats,but also play important roles in the spice industry,food industry and chemical industry.Taking account of high Pharmacology value on its volatile oil application,the researches into ways to extract volatile oil from it have been paid increasing interest.Some kinds of extraction methods have been reported on how to get its volatile oil to some extend.Summarily, the extraction methods introduced include steam distillation based on activated ion-water as extractant and ether as absorbent,extraction based on supercritical fluidic carbon dioxide,extraction under microwave at appropriate wavelength,steam distillation directly,steam distillation based on acetic ester or dichloroethane as absorbents,solvent extraction. It could be concluded that some progresses have been made on the extraction yield and the number of components.However,it is worth to develop new way regarding the higher extraction yield,extraction rate and energy saving.
Semi-Bionic Extraction technique(briefly,termed as SBE)is a new kind of technique for extraction useful components from Chinese medicine(herb).The thesis carried out studies on both the SBE-coupling steam distillation and isopropyl extraction-coupling steam distillation to extract volatile oil.The analysis of components in extracted oil has been taken on GC-MS.
The experiment result shows that there are 22 chemical components similar in extraction oil obtained by either SBE-coupling steam distillation or isopropyl extraction-coupling steam distillation after ultrasonic treatment.These components are phthalic anhydride -1,3-asopropyl furandione、2-methyl-5(1-methylethyl)-2-cyclohexanol、 bicyclo[2,2,1]-2-heptanol、bicyclogermacrene、selinane-6-ene-4-ol、β-cubebene、β-caryophyllene、o-phthalic acid、cholestan-3-one、2-(piperonilidene amino)antipyrine、δ-cadinene、α-humulene、3-(benzothioylthio)-2-formic acetate、β-costol,et al.
The resulting yield of the so-extraction was measured as 1.05%, which is about 0.3%higher than that by applying the steam distillation directly.The GC-MS analysis shows that 43 chemical were given from so-extracted volatile oil and 11 of them were absent from the volatile oil,extracted by the steam distillation directly,such as eucalyptole, piperitone,(-)-bornyl acetate,1,3-(2-H)-dimone-2-amino-1H-1-indole; phthalic acid monoethy ester,chrysanthenone,cis-isoeugenol,α-amorphene,caryophyllenol,11,15-dimethyl 35ane.Some chemical components such asα-thujone、β-pinene、1-octen-3-ol、β-selinene,et al didn't be checked.
It is concluded from our studies that the number of components obtained from isopropyl-extraction coupling- steam distillation are more than that obtained by steam distillation.The components with high extraction yield such as phthalic acid monoethy ester、1H-indene-1,2,3-trione、3,4-dimethyl cyclohexan-ol have been present in the extraction oil by isopropyl-extraction coupling- steam distillation, which were absent in extraction oil by extraction methods reported previously.However,the isopropyl-extraction coupling- steam distillation was not good regarding extraction yield of the high volatile components. For high volatile component extraction,SBE-coupling steam distillation would be applied to improve the extraction yield of these high volatile components.
引文
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