丁香油的超临界CO_2萃取及在果蔬保鲜中的应用研究
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摘要
丁香(Eugenia caryophyllata Thunb.)的干燥花蕾是我国传统的调味品和中草药,近年来又发现丁香油具有较强的杀虫、防腐保鲜作用。丁香油的传统提取方法为水蒸气蒸馏和有机溶剂提取等,近年来新兴的超临界CO_2萃取技术被认为是提取天然植物挥发油的高效洁净工艺。本课题的主要目的是深入研究超临界CO_2萃取丁香油工艺,比较其与传统提取方法的优缺点;同时通过对超临界流体萃取过程中的传质模型与数学模拟,以及测定丁香油中主要成分在超临界CO_2中的溶解度与关联等基础研究,为今后的工程放大提供必要的基础数据和理论指导。本文还首次研究了丁香油对果蔬主要采后病原菌的抑制效果及对青椒等果蔬的防腐保鲜效果与机理,该研究为开发果蔬采后天然防腐保鲜剂提供基础,对其在食品防腐保鲜中的应用具有重要的社会意义和学术价值。
本课题首先以丁香收油率和主要成分丁香酚在萃取物中的含量为目标函数,采用正交试验及延伸试验研究了压力、温度、粒度、时间等因素对萃取效果的影响,从而确定出丁香油的适宜萃取条件。研究表明在萃取温度和压力分别为50℃和10-15MPa的条件下,丁香收油率为17.67%~20.16%。本文还采用GC和GC/MS分析方法,比较了超临界CO_2萃取与传统的水蒸气蒸馏等方法对丁香收油率和油的化学成分等的影响。收油率是水蒸气蒸馏和水中蒸馏的两倍左右。通过GC/MS共鉴定出丁香油中的23种成分,超临界萃取所得丁香油中丁香酚、乙酰丁香酚、β-石竹烯相对含量占90%以上,其中丁香酚和乙酰丁香酚的含量分别为58.8%和19.6%。超临界二氧化碳萃取丁香油没有溶剂残留,萃取时间短,收油率高,较传统方法具有明显的优势。
在对超临界流体萃取过程的研究中,根据质量平衡建立了丁香油萃取过程的集总参数法模型,并结合实验结果对方程进行了合理的简化,利用实验数据拟合出主要参数,模型的计算值和实验值的平均相对误差在6.88～57.78%之间。
利用动态法测定了不同压力(10-30MPa)、温度(313-333K)下丁香酚、乙酰丁香酚、β-石竹烯在SC-CO_2中的溶解度。在实验条件下,丁香酚在SC-CO_2中的溶解度(摩尔分数)为0.0002-0.0580;乙酰丁香酚在SC-CO_2中的溶解度(摩尔分数)为0.00018-0.07030;β-石竹烯在SC-CO_2中的溶解度(摩尔分数)为0.00034-0.07096。而后分别利用ln y_2与压力P的非线性关系方程、Chrastil方程、Chrastil改进方程(Adachi、de Valle)对丁香酚、乙酰丁香酚、β-石竹烯在SC-CO_2中的溶解度进行了关联。关联的AARD平均值在2.91%~5.74%之间,表明上述关联方程对本测量系统的适用性。
本文还利用超临界CO_2萃取丁香油的实验数据求得了丁香油在SC-CO_2中的
Clove oils extracted from Buds of clove ((Eugenia caryophyllata Thunb.) have been used in traditional Chinese medicines and flavoring agent. It is reported that clove oils also have antifungal and insecticidal functions. Traditional extraction methods for clove oil are steam distillation and solvent extraction. Supercritical carbon dioxide extraction (SFE) is considered as a new and green process for the essential oil extraction. The objective of this project is to study the process of extracting clove oil with supercritical CO_2 (SC-CO_2), and to compare the quality of clove oils extracted by SFE with traditional methods. In addition, the basic theoretical research on the mass transport process of SFE and the solubility of clove oils were also studied. At last, the antifungal activity of clove oils and its application in pepper storage were also studied.
Extraction of clove oil with SC-CO_2 was firstly investigated, and the orthogonal array design was used to explore the influences of temperature, pressure and particle size on the yield and the content of main components in the extracted clove oil. The experimental results showed that the yields of clove oil extracted from clove buds were 17.67%~20.16 % at temperature of 50℃and pressures ranging from 10 MPa to 15 MPa. The composition and the quality of the clove oils extracted by different methods, including SFE, hydro distillation, steam distillation and soxhlet extraction, were further compared. The analytical results by GC showed that, the content of eugenol and eugenol acetate in clove oil extracted by SFE is 58.8% and 19.6%, respectively. Twenty three compounds in the clove oils have been identified by GC/MS, and the relative content of eugenol, eugenol acetate andβ-caryophyllene is totally higher than 90%. The oil yield extracted with SC-CO_2 under optimal conditions is about twice as that by hydro distillation or steam distillation. Additionally, the apparent characteristics, such as no solvent residues existed in the extracted oil, shorter extraction time and so on, indicated that SFE could be one of the most clean and highly effective technology for processing essential oil from the plants.
Based on the material balances, a mathematical model was founded by lumped parameter method and then simplified so that it can be employed to simulate the SFE process of clove oil. The simulating results showed that the model fits the experimental data with average relative errors (AARD ) ranging from 6.88～57.78%. The solubility of eugenol, eugenol acetate andβ-caryophyllene in supercritical CO_2 was separately determined with dynamic method at the temperatures ranging from 313 K to 333K and pressures from10 MPa to 30MPa. The experimental results showed that the solubilities of eugenol in SC-CO_2 were between 0.0002 and 0.0580 (mole fraction). The solubilities of eugenol acetate in SC-CO_2 were between
本课题首先以丁香收油率和主要成分丁香酚在萃取物中的含量为目标函数,采用正交试验及延伸试验研究了压力、温度、粒度、时间等因素对萃取效果的影响,从而确定出丁香油的适宜萃取条件。研究表明在萃取温度和压力分别为50℃和10-15MPa的条件下,丁香收油率为17.67%~20.16%。本文还采用GC和GC/MS分析方法,比较了超临界CO_2萃取与传统的水蒸气蒸馏等方法对丁香收油率和油的化学成分等的影响。收油率是水蒸气蒸馏和水中蒸馏的两倍左右。通过GC/MS共鉴定出丁香油中的23种成分,超临界萃取所得丁香油中丁香酚、乙酰丁香酚、β-石竹烯相对含量占90%以上,其中丁香酚和乙酰丁香酚的含量分别为58.8%和19.6%。超临界二氧化碳萃取丁香油没有溶剂残留,萃取时间短,收油率高,较传统方法具有明显的优势。
在对超临界流体萃取过程的研究中,根据质量平衡建立了丁香油萃取过程的集总参数法模型,并结合实验结果对方程进行了合理的简化,利用实验数据拟合出主要参数,模型的计算值和实验值的平均相对误差在6.88～57.78%之间。
利用动态法测定了不同压力(10-30MPa)、温度(313-333K)下丁香酚、乙酰丁香酚、β-石竹烯在SC-CO_2中的溶解度。在实验条件下,丁香酚在SC-CO_2中的溶解度(摩尔分数)为0.0002-0.0580;乙酰丁香酚在SC-CO_2中的溶解度(摩尔分数)为0.00018-0.07030;β-石竹烯在SC-CO_2中的溶解度(摩尔分数)为0.00034-0.07096。而后分别利用ln y_2与压力P的非线性关系方程、Chrastil方程、Chrastil改进方程(Adachi、de Valle)对丁香酚、乙酰丁香酚、β-石竹烯在SC-CO_2中的溶解度进行了关联。关联的AARD平均值在2.91%~5.74%之间,表明上述关联方程对本测量系统的适用性。
本文还利用超临界CO_2萃取丁香油的实验数据求得了丁香油在SC-CO_2中的
Clove oils extracted from Buds of clove ((Eugenia caryophyllata Thunb.) have been used in traditional Chinese medicines and flavoring agent. It is reported that clove oils also have antifungal and insecticidal functions. Traditional extraction methods for clove oil are steam distillation and solvent extraction. Supercritical carbon dioxide extraction (SFE) is considered as a new and green process for the essential oil extraction. The objective of this project is to study the process of extracting clove oil with supercritical CO_2 (SC-CO_2), and to compare the quality of clove oils extracted by SFE with traditional methods. In addition, the basic theoretical research on the mass transport process of SFE and the solubility of clove oils were also studied. At last, the antifungal activity of clove oils and its application in pepper storage were also studied.
Extraction of clove oil with SC-CO_2 was firstly investigated, and the orthogonal array design was used to explore the influences of temperature, pressure and particle size on the yield and the content of main components in the extracted clove oil. The experimental results showed that the yields of clove oil extracted from clove buds were 17.67%~20.16 % at temperature of 50℃and pressures ranging from 10 MPa to 15 MPa. The composition and the quality of the clove oils extracted by different methods, including SFE, hydro distillation, steam distillation and soxhlet extraction, were further compared. The analytical results by GC showed that, the content of eugenol and eugenol acetate in clove oil extracted by SFE is 58.8% and 19.6%, respectively. Twenty three compounds in the clove oils have been identified by GC/MS, and the relative content of eugenol, eugenol acetate andβ-caryophyllene is totally higher than 90%. The oil yield extracted with SC-CO_2 under optimal conditions is about twice as that by hydro distillation or steam distillation. Additionally, the apparent characteristics, such as no solvent residues existed in the extracted oil, shorter extraction time and so on, indicated that SFE could be one of the most clean and highly effective technology for processing essential oil from the plants.
Based on the material balances, a mathematical model was founded by lumped parameter method and then simplified so that it can be employed to simulate the SFE process of clove oil. The simulating results showed that the model fits the experimental data with average relative errors (AARD ) ranging from 6.88～57.78%. The solubility of eugenol, eugenol acetate andβ-caryophyllene in supercritical CO_2 was separately determined with dynamic method at the temperatures ranging from 313 K to 333K and pressures from10 MPa to 30MPa. The experimental results showed that the solubilities of eugenol in SC-CO_2 were between 0.0002 and 0.0580 (mole fraction). The solubilities of eugenol acetate in SC-CO_2 were between
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