山茱萸酒发酵及中试工艺的研究
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摘要
山茱萸是我国珍贵的药材资源,多用于中医及其临床医学的研究。果肉中含有24种矿物元素,17种氨基酸,人体所需要的8种必须氨基酸全部具备,还含有VA、VC、VE和VB2等对人有益的成分。本论文以湖北郧县产山茱萸干果肉为原料酿造酒,主要对发酵工艺、陶瓷膜过滤工艺、两种功能性成分马钱素和熊果酸的测定以及风味物质的定性进行了研究。
通过单因素实验,分别研究了酵母品种、温度、酵母接种量、SO2添加量、果胶酶添加量、糖度对酒精发酵的影响,实验结果表明,温度、酵母接种量、SO2添加量、糖度四个因素对发酵影响较大,为关键影响因子。在此基础上进行四因素三水平正交试验,以功能性成分马钱素和熊果酸的含量作为检测标准,对发酵工艺进行优化,确定山茱萸发酵的最佳工艺条件为:料液比为1:10,温度24℃,酵母接种量0.2%,SO2添加量50mg/l,糖度为18%。根据优化工艺得出的结果进行中试,经无机陶瓷膜微滤,最终山茱萸发酵酒的酒度为10°,酸度为0.984%,功能性成分马钱素和熊果酸的含量分别为0.078 mg/mL和4.846μg/mL。
根据试验最佳优化工艺结合实际生产的可实施性,进行中试,采用自动气流式搅拌发酵罐扩大发酵,使整个发酵过程没有杂菌污染,保证了酒精发酵的质量保留了酒的风味物质。
将自然沉降的山茱萸酒液用0.2μm无机陶瓷膜在24℃和0.1~0.15MPa左右进行微滤。结果表明:山茱萸酒液的澄清度有了明显的提高,细菌和大肠杆菌数量达到国家标准规定范围,稳定性提高,功能性物质马钱素和熊果酸的变化不大,主要风味物质影响不大。
采用高效液相色谱法对山茱萸及其发酵酒中的马钱素和熊果酸进行分析。测得本试验所用原料山茱萸干果肉中马钱素的含量为0.23%,熊果酸含量为0.33%,发酵酒中的马钱素和熊果酸在陶瓷膜过滤前后的含量分别为0.086mg/mL,0.078 mg/mL;5.462μg/mL,4.846μg/mL。
山茱萸发酵原酒通过GC-MS共检出36种香气成分,醇类化合物的种类为14种,酯类化合物的种类为9种,羧酸类化合物的种类为4种,杂环类和烷烃类化合物为9种。过滤后共检出28种香气成分。香气的主要组分为醇类和酯类,其中醇类主要有苯乙醇、10-甲基二环十一烷基-10-醇、植醇酯类主要有3-甲基丁酸乙酯、2-辛炔酸甲酯、三甲基乙酸环己酯。
Cornus officinatis Sieb. et Zucc. is one of our country's precious medical material resources. The fruit pulp contains 24 kinds of mineral elements, 16 kinds of amino acids. It possesses 8 kinds of must amino acids that are needed in human. It also includes VA, VC, VE, VB2 and so on which are beneficial to people. The wine was fermented by dry fruit pulp of Fructus corni from xian in Anhui province. The processing of fermentation, the technics of ceramic membrane filter, the determination of two functional ingredients (the loganin and the ursolic acid) and the qualitative of the flavor were mainly studied.
Through the single factor experiment, factors that had influenced on the alcoholic fermentation were mainly considered, including yeast breed, temperature, inoculation amount of yeast, the SO2 amount, the pectase amount and sugar concentrations. The results indicated that four factors had more influence on fermentation. They were temperature, inoculation amount of yeast , the SO2 amount and sugar concentrations. On the basis of the experiments, the four factors and three levels orthogonal experiment was used to search the optimum fermentation parameters taken two functional ingredients (the loganin and the ursolic acid) as the inspection standard, the optimum conditions were: the ratio of material to water was 1:10, the temperature was 24℃, the inoculation amoun of yeast was 0.2%, , the addition of SO2 was 50mg/L, the sugar concentrations was 18%. Then a pilot was did and the alcohol of the product was 10°, the degree of acid was 0.984%. The content of the loganin was 0.078 mg/mL and the ursolic acid was 4.846μg/mL.
According to the optimum conditions of extraction in laboratory as well as the realizable of mass-produce, it was fermented in automatic air current type agitation fermentation pot. The entire process wasn’t contaminated by harmful bacterium. The quality of the alcoholic fermentation was ensured and the flavor of wine was preserved.
0.2μm ceramic membrane was used to micro-filtrate the fructus corni wine which was subsided spontaneously under the condition of 24℃and 0.1~0.15MPa. The results indicated that: the clarification of the wine was improved obviously, the number of bacteria and colibacillus decreased to the GB, the stability increased, the amount of the loganin and the ursolic acid changed unconspicuously so did the main flavor.
The method of high-performance liquid chromatography was utilized to analysis the loganin and the ursolic acid in the fructus corni and wine. The results of the content of the loganin were: 0.23% in raw materials, 0.086mg/mL in the wine and 0,078 mg/mL in the filtrated wine. The results of the content of the ursolic acid were: 0.33% in raw materials, 5.462μg/mL in the wine and 4.846μg/mL in the filtrated wine.
36 kinds of aromatic components were identified in the original fructus corni wine through the method of GC-MS, including 14 kinds of alcohols, 9 kinds of esters, 4 kinds of carboxylic acids, 9 kinds of heterocycle and alkane. 28 kinds of aromatic components were identified in the wine which was filtrated from ceramic membrane. The great components of aroma were alcohols and esters. The main of alcohols were phenylethyl alcohol, 10-methylbicyclo[4,3,1,1(2,5)] undecan-10-ol and phytol. The main of esters were butanoic acid,3-methyl-,ethyl ester, 2-octynoic acid,methyl ester and butanoic acid,3-methyl-,ethyl ester.
通过单因素实验,分别研究了酵母品种、温度、酵母接种量、SO2添加量、果胶酶添加量、糖度对酒精发酵的影响,实验结果表明,温度、酵母接种量、SO2添加量、糖度四个因素对发酵影响较大,为关键影响因子。在此基础上进行四因素三水平正交试验,以功能性成分马钱素和熊果酸的含量作为检测标准,对发酵工艺进行优化,确定山茱萸发酵的最佳工艺条件为:料液比为1:10,温度24℃,酵母接种量0.2%,SO2添加量50mg/l,糖度为18%。根据优化工艺得出的结果进行中试,经无机陶瓷膜微滤,最终山茱萸发酵酒的酒度为10°,酸度为0.984%,功能性成分马钱素和熊果酸的含量分别为0.078 mg/mL和4.846μg/mL。
根据试验最佳优化工艺结合实际生产的可实施性,进行中试,采用自动气流式搅拌发酵罐扩大发酵,使整个发酵过程没有杂菌污染,保证了酒精发酵的质量保留了酒的风味物质。
将自然沉降的山茱萸酒液用0.2μm无机陶瓷膜在24℃和0.1~0.15MPa左右进行微滤。结果表明:山茱萸酒液的澄清度有了明显的提高,细菌和大肠杆菌数量达到国家标准规定范围,稳定性提高,功能性物质马钱素和熊果酸的变化不大,主要风味物质影响不大。
采用高效液相色谱法对山茱萸及其发酵酒中的马钱素和熊果酸进行分析。测得本试验所用原料山茱萸干果肉中马钱素的含量为0.23%,熊果酸含量为0.33%,发酵酒中的马钱素和熊果酸在陶瓷膜过滤前后的含量分别为0.086mg/mL,0.078 mg/mL;5.462μg/mL,4.846μg/mL。
山茱萸发酵原酒通过GC-MS共检出36种香气成分,醇类化合物的种类为14种,酯类化合物的种类为9种,羧酸类化合物的种类为4种,杂环类和烷烃类化合物为9种。过滤后共检出28种香气成分。香气的主要组分为醇类和酯类,其中醇类主要有苯乙醇、10-甲基二环十一烷基-10-醇、植醇酯类主要有3-甲基丁酸乙酯、2-辛炔酸甲酯、三甲基乙酸环己酯。
Cornus officinatis Sieb. et Zucc. is one of our country's precious medical material resources. The fruit pulp contains 24 kinds of mineral elements, 16 kinds of amino acids. It possesses 8 kinds of must amino acids that are needed in human. It also includes VA, VC, VE, VB2 and so on which are beneficial to people. The wine was fermented by dry fruit pulp of Fructus corni from xian in Anhui province. The processing of fermentation, the technics of ceramic membrane filter, the determination of two functional ingredients (the loganin and the ursolic acid) and the qualitative of the flavor were mainly studied.
Through the single factor experiment, factors that had influenced on the alcoholic fermentation were mainly considered, including yeast breed, temperature, inoculation amount of yeast, the SO2 amount, the pectase amount and sugar concentrations. The results indicated that four factors had more influence on fermentation. They were temperature, inoculation amount of yeast , the SO2 amount and sugar concentrations. On the basis of the experiments, the four factors and three levels orthogonal experiment was used to search the optimum fermentation parameters taken two functional ingredients (the loganin and the ursolic acid) as the inspection standard, the optimum conditions were: the ratio of material to water was 1:10, the temperature was 24℃, the inoculation amoun of yeast was 0.2%, , the addition of SO2 was 50mg/L, the sugar concentrations was 18%. Then a pilot was did and the alcohol of the product was 10°, the degree of acid was 0.984%. The content of the loganin was 0.078 mg/mL and the ursolic acid was 4.846μg/mL.
According to the optimum conditions of extraction in laboratory as well as the realizable of mass-produce, it was fermented in automatic air current type agitation fermentation pot. The entire process wasn’t contaminated by harmful bacterium. The quality of the alcoholic fermentation was ensured and the flavor of wine was preserved.
0.2μm ceramic membrane was used to micro-filtrate the fructus corni wine which was subsided spontaneously under the condition of 24℃and 0.1~0.15MPa. The results indicated that: the clarification of the wine was improved obviously, the number of bacteria and colibacillus decreased to the GB, the stability increased, the amount of the loganin and the ursolic acid changed unconspicuously so did the main flavor.
The method of high-performance liquid chromatography was utilized to analysis the loganin and the ursolic acid in the fructus corni and wine. The results of the content of the loganin were: 0.23% in raw materials, 0.086mg/mL in the wine and 0,078 mg/mL in the filtrated wine. The results of the content of the ursolic acid were: 0.33% in raw materials, 5.462μg/mL in the wine and 4.846μg/mL in the filtrated wine.
36 kinds of aromatic components were identified in the original fructus corni wine through the method of GC-MS, including 14 kinds of alcohols, 9 kinds of esters, 4 kinds of carboxylic acids, 9 kinds of heterocycle and alkane. 28 kinds of aromatic components were identified in the wine which was filtrated from ceramic membrane. The great components of aroma were alcohols and esters. The main of alcohols were phenylethyl alcohol, 10-methylbicyclo[4,3,1,1(2,5)] undecan-10-ol and phytol. The main of esters were butanoic acid,3-methyl-,ethyl ester, 2-octynoic acid,methyl ester and butanoic acid,3-methyl-,ethyl ester.
引文
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