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青花椒香气成分的提取、分析及抑菌性研究

Study on Extraction、Analyses and Bacteriostatic Action of Aroma Composition of Zanthoxulum spp.

【作者】 高逢敬

【导师】 蒲彪; 叶萌;

【作者基本信息】 四川农业大学 , 农产品加工及贮藏工程, 2007, 硕士

【摘要】 本试验以四川洪雅、金阳两地青花椒为原料,主要对花椒香气成分的提取方法进行筛选,并对两地所产的青花椒果皮、种籽和叶子进行香气成分的提取及分析,最后对不同方法提取的两种青花椒果皮香气成分的抑菌性进行了初步探索,为花椒的精深加工及全面利用提供依据。1.采用水提法、有机溶剂萃取法和超临界CO2萃取法对花椒香气成分进行提取,对三种方法的工艺参数进行摸索和优化,并采用GC-MS法对各种方法提取的香气成分进行分析,结果表明:原料在70℃下烘箱干燥3h挥发性成分损失最少,水提法得率最低(8.42ml/100g),但成本也最低。有机溶剂萃取中选用乙醚作为萃取剂,各因素对提取率的影响次序为:水浴温度>提取时间>料液比,最佳工艺条件为:原料粒度20-40目,水浴温度40℃,萃取时间2h,料液比为1:30,得率为9.81%,由于溶剂可循环利用,此法成本较低,得率较高。由于存在溶剂残留问题,可用于食品以外的其它工业化生产。超临界CO2萃取中各因素对提取结果的影响次序为:温度>压力>时间>流量,最佳工艺条件为:温度55℃、压力40 MPa、提取时间2.5 h、CO2流量20 kg/h,理论得率为11.2%,实际得率为10.89%,加入萃取釜体积3%的浓度为95%的乙醇作为夹带剂,可以使提取率达到13.2%,超临界萃取法成本最高,但操作方便,效率高,得率也最高,不存在溶剂残留。2.采用GC-MS法对不同方法提取的青花椒香气成分进行鉴定,水提法共鉴定出24种化学成分,主要是花椒的香味成分,包括:芳樟醇、柠檬烯、顺式-β-罗勒烯、β-水芹烯、4-萜品醇等;有机溶剂萃取共鉴定出39种化学成分,包括:芳樟醇、柠檬烯、β-水芹烯、大根香叶烯、香桃木烯醇等;超临界CO2萃取共鉴定出54种化学成分,除上述几种外,还有Z-11-十一碳烯酸、酞酸丁酯、Z-11-透明质酸。就提取的花椒风味物质的种类而言,超临界CO2萃取是最好的提取方法3.用GC-MS法对四川洪雅、金阳两地青花椒不同部位(果皮、种籽、叶子)的无水乙醚萃取物进行分析、对比,结果表明:金阳青花椒各部位香气成分含量均高于洪雅青花椒。两种果皮中含有芳樟醇、香桃木烯醇、大根香叶烯等共有香气成分21种,分别占总检出量的78%和74.87%;种籽中含有棕榈酸甲酯、亚油酸、肉豆蔻酸等共有香气成分12种,分别占总检出量的94.5%和94.22;叶子中含有的共有成分为30种,但所占比例较小,分别为69.86%和46.52%。在洪雅青花椒各部位中含量较高的柠檬烯在金阳青花椒中含量较少。4.不同方法提取的两种花椒香气成分除对绿色木霉无抑制作用以外,对大肠杆菌、金黄色葡萄球菌、热带假丝酵母、产朊假丝酵母、白地霉、烟曲霉、黑曲霉等均有不同程度的抑制作用。水提法得到的香气成分抑菌效果最好,另外两种方法得到的产品抑菌效果相差不大。洪雅青花椒对热带假丝酵母、产朊假丝酵母、烟曲霉的抑制效果优于金阳青花椒,对大肠杆菌、金黄色葡萄球菌、白地霉、黑曲霉的抑制效果比后者要差。

【Abstract】 The material of this experiment is Zanthoxulum spp.from Hongya and Jinyang of Sichuan.The experiment mainly filters the extracting methods of the aroma composition of Zanthoxulum spp.,then extracts the aroma composition of peek seeds and leaves of two kinds of Zanthoxulum spp. from Hongya and Jinyang of.At last,researches the bacteriostatic action of the peels aroma composition extracting by different methods.The experiment provides bases for deep processing and overall utilization of Zanthoxulum spp..1.Using distillation、solvent extraction and SCFE to extract the aroma composition of Zanthoxulum spp., the experiment gropes and optimizes the technology parameter of the three methods, then analyses the aroma composition extracted by different methods by gas chromatography-mas spectrometry.The result indicates:The loss of evaporability composition is least when the material dried 3 hours under 70℃.The yield of distillation is lowest(8.42 ml/100g),but the cost is lowest too.Selecting aether as the solvent,the infection order of every factor of solvent extraction to the extracting rate is: waterbath temperature>time>ratio of dosage liquor.The best extracting condition is:grade size 20-40 screen mesh, waterbath temperature 40℃,time 2h, ratio of dosage liquor 1:30,the yield is 9.81%.Because the solvent can be used circularly,the cost of this method is lower and the yield is higher.Because of the remanet of solvent,this method can be used in the industrialization production except food industry.The infection order of every factor of SCFE to the extracting rate is: temperature>pressure>time>fluence.The best extracting condition of SCFE is:temperature 55℃>pressure 40 MPa、time 2.5h、fluence of CO2 20 kg/h, the academic yield is 11.2% and the actual yield is 10.89%.When putting in ethanol that the volume is 3% of the extacting kettle and concentration 95%,the yield reaches 13.2%.The cost of this method is highest but it is convenient and efficient,and the yield is highest.And there isn’t remanet of solvent in this method.2. Uses GC-MS to identify the aroma compositions extracting by different methods.There are 24 kinds of compositions in distillation,mainly the fragrance element including Linalool、Limonene、cis-beta-Ocimene、beta-Phellandrene、4-Terpineol and so on; there are 39 kinds of compositions in solvent extraction, including Linalool、Limonene、beta-Phellandrene、Germacrene、Myrtenol and so on; there are 54 kinds of compositions in SCFE.Excepting the kinds previously tells, there are Undecylenic acid、Dibutyl phthalate、Z-11-Hexadecenoic acid and so on.Acording to c the sort of the aroma substance,SCFE is the best method.3.Using GC-MS,the paper analyseses and contrasts the products extracted from different parts(peel、seeds、leaves) of the two kinds of Zanthoxulum spp.extracting by aether. The result indicates:every parts of the Zanthoxulum spp. of Jinyang contain more aroma compositions than the breed of Hongya. The two kinds of peels contain 21 kinds of identical composition such as LinalooK Myrtenol、Germacrene and so on,which account 78% and 74.87% of the total detection; The two kinds of seeds contain 12 kinds of identical composition such as Hexadecanoic acid, methyl ester、9,12-Octadecadienoic acids Myristicid and so on, which account 94.5% and 94.22% of the total detection; There’re 30 kinds of identical composition in the two kinds of leaves,but the ratio of them is lower,it is 69.86% and 46.52%. Content of Limonene is high in every part of Zanthoxulum spp. of Hongya while it is low in the breed of Jinyang.4. Aroma composition extracted by different methods have distinct extent bacteriostatic action to Escherichia coli、Staphylococcus aureus、Candida tropicalis、Candida utilis、Geotrichum candidum、A. fumigatus and A spergillus niger,but have no action to Trichoderma varide Pers.ex Fr.The depressant effect of the aroma composition extracted by distillation is best,and the other two are alike.The bacteriostatic effect of Hongya Zanthoxulum spp. on Candida tropicalis、Candida utilis and A. fumigatus is better than that of Jinyang,but infirmer on Escherichia col、Staphylococcus aureus、Geotrichum candidum、A spergillus niger.

  • 【分类号】TS255
  • 【被引频次】22
  • 【下载频次】1225
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