泸州老窖大曲的质量、微生物与香气成分关系
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摘要
利用大曲酿造白酒是我国白酒酿造的关键和区别于世界上其它知名蒸馏酒的重要技术特征。大曲是以小麦为主的谷物原料通过生料发酵而得到,大曲是白酒酿造过程中重要的微生物、酶类、香气物质和香气物质前体物质的主要来源。大曲的质量直接关系到白酒的出酒率和品质。本文选取泸州老窖生产的中、高温大曲为研究对象,对其中的香气成分、理化指标和酶进行了分析鉴定;并从大曲中筛选能够产生香气的微生物;研究了泸州老窖中、高温大曲发酵过程中微生物种群变化与相应香气形成的关系;同时初步研究了大曲在发酵过程中的安全性问题,主要的研究内容如下:
使用一种简便、快速、灵敏的顶空固相微萃取-气相色谱-质谱联用法(GC-MS)测定曲样中的挥发性化合物,并配合电子鼻(EN)技术,比较了仪器分析与感官判别大曲质量的关系。顶空固相微萃取-气相色谱-质谱联用法(GC-MS)能将大曲样品中的醇类、吡嗪、醛类、酮类和酯类等挥发性物质较好地萃取出来,对大曲样品中具有代表性的挥发性成分如酯类、醇类和吡嗪类等测定的结果重复性良好,同时具有较高的加标回收率。利用GC-MS对不同的大曲样品进行分析,共检测出挥发性化合物75种,包括的挥发性风味物质分别有:醇类物质、酸类物质、酯类物质、醛类物质、酮类物质、芳香族化合物、酚类物质、呋喃类物质和含氮类化合物;采用主成分分析方法分析10种大曲中的挥发性化合物,十种大曲能够被区分为三大类,发酵温度不高于60℃的中温大曲的优级大曲和普级大曲在主成分分析图上距离较为接近,而高温大曲的优级大曲和普级大曲能够明显分成两类;采用电子鼻(EN)技术分析大曲样品,不同大曲样品对电子鼻有一定的响应,从雷达图可以发现,中温优级大曲、中温普级大曲和高温普级大曲的雷达图趋势较为相似,而高温优级大曲与上述三种大曲趋势较为不同,与其它三种大曲的气味存在较大的差异;依据气相-嗅闻法(GC-O)的频率检测法(DF)和香气提取稀释分析法(AEDA)两种方法考察了中温优级大曲和高温优级大曲,依据DF值和FD值的大小判断香气物质对大曲香气的贡献程度,结果表明:中温优级大曲中的特征香气成分可能主要是由己醛、未知化合物(no.u2)、苯乙醛和4-乙基愈创木酚等化合物组成;高温优级大曲中的特征香气可能主要是由己醛、2,6-二甲基吡嗪、壬醛、1-辛烯-3-醇、苯乙醛、4-乙基愈创木酚和未知化合物(no.u2、u3、u5和u7)组成;其它挥发性化合物可能作为背景香气物质。
从感官特征的角度,分析了不同等级的大曲在微生物组成、酶、理化成分等方面的区别,并分析了风味物质形成的外部条件。结果表明,优级大曲的“穿衣”情况要比普级大曲好且均匀,其微生物数量多,尤其是霉菌数量更为明显;优级大曲中主要酶的活力均高于普级大曲,优级大曲的酯化力高于普级大曲,而酯分解率低于普级大曲,有利于促进风味物质的形成,优级大曲的发酵力和游离氨基酸总量均高于普级大曲。对大曲在发酵期间的各项指标,包括微生物数量、理化指标、酶、风味变化和感官变化进行跟踪测定发现:随着发酵时间的延长,中、高温大曲中的水分含量和水活度都呈现下降的趋势;温度表现为先升后降;大曲中微生物的数量和种类与曲醅的温度、水分含量、水活度和pH等多种因素息息相关,中温大曲的微生物数量在发酵起始均有小幅度增加,但是随温度的增加和水活度的降低,大曲中的一些不耐热的微生物大量死亡;而高温大曲由于其特殊的工艺条件,大曲维持在一个高温高湿的环境,耐热的芽孢杆菌能够正常生长代谢;两类大曲在发酵过程中均出现一个产酸高峰期,随着微生物数量的递减,酸度也减低。使用顶空固相微萃取-质谱联用技术考察了中温大曲在发酵和贮存培菌期间的风味物质的变化,共检测出46种化合物,在大曲发酵的第5天多数风味物质含量达到最大值,而在大曲发酵的第9天含氮类化合物含量才达到最大,在大曲发酵30天时挥发性风味物质含量趋于稳定,这为优化大曲生产工艺提供了理论依据。对大曲在发酵期间的香气物质进行定量描述和分析,大曲的果香、花香和辛香等香气物质在发酵的前5天快速增加,随着发酵的进行这些香气物质在第5天后开始下降,香气变化的规律与利用气质联用方法检测到的化合物含量变化规律较为相似。
对大曲发酵和贮存各个时期的微生物进行了分离、纯化、筛选和鉴定,对产香微生物模拟发酵产生香气成分的机理进行了探索。利用多种培养基进行微生物分离,得到霉菌93株,酵母菌112株,嗜热芽孢杆菌45株。通过初筛和复筛从中温大曲和高温大曲中分别筛选到能产香的酵母菌ZY-1和GY-3和产香芽孢杆菌ZL-1和GL-4;利用分子生物学和生理生化鉴定方法确定,ZY-1属于东方伊萨酵母,GY-3属于假丝酵母属的一种,ZL-1是枯草芽孢杆菌,GL-4是地衣芽孢杆菌。对ZL-1和GL-4菌株产香条件进行优化,考察了美拉德模式反应,ZL-1和GL-4均能促进培养基褐变物质的生成,采用小麦浸出液在37℃~55℃(37℃、45℃和55℃各2天)发酵的第6天褐变程度最高;对发酵液在发酵过程中蛋白酶活力、游离氨基酸和还原糖含量进行了跟踪测定,考察了除菌灭酶对发酵液香气的影响。利用气质联用技术测定ZL-1和GL-4发酵液,发现2,3-丁二酮、三甲基吡嗪、四甲基吡嗪和愈创木酚可能与大曲香气成分的形成有一定的关系。利用小麦浸出液培养ZY-1和GY-3两种酵母,酵母在发酵过程中主要生成一些酯类、醇类和酮类等挥发性风味物质,可见产香酵母是大曲中风味物质形成的重要原因。
进行了大曲单独酿酒实验和大曲安全性研究,发现大曲质量与白酒产量、品质和风味有密切联系。两种温度类型大曲的优级大曲发酵产酒、总酸和总酯量均高于普级大曲,所酿白酒的品质在很大程度由大曲质量决定,四类大曲发酵所产白酒中的固形物及总醛含量差异较小,但酒精的含量却差异显著,同时在氨基酸总量也不同,高温优级大曲酒的挥发性化合物总量明显高于中温优级大曲酒,但是挥发性风味物质的总量上相差不是太大,这与检测出的高温优级大曲和中温优级大曲中的挥发性风味成分数量上的趋势一致,安琪高活性酿酒酵母组挥发性风味组分的总量与大曲酒相差不大,但是在挥发性化合物数目上相差较多,这也从一个侧面反映出,大曲在提高大曲酒风味成分上的作用。利用HPLC方法测定了大曲中4种具有代表性的真菌毒素,该方法具有很好的精密度和回收率,大曲中检测到的4种真菌毒素含量均未超过国家或国际上通用的限量标准。由于白酒酿造的后续工艺,大曲中毒素被最终带入到白酒成品的可能性极小。
In China, using Daqu to initiate the solid fermentations for the production of Chinese liquor is the key technology which is a major difference from the other famous distilled spirits in the world. Daqu is a type of grain Qu, which is mainly made from raw wheat and by natural inoculation. Daqu is the major source of microorganisms, enzymes, flavour compounds and their precursors in Chinese liquor process. Its quality is directly related to the yield and the quality of Chinese liquor. Medium and high temperature Daqu which were produced by Luzhou Laojiao Company located in Luzhou China was studied here. Characteristic flavours, physicochemical indexes and enzymes of medium and high temperature Daqu were analyzed. Aroma-producing microorganisms were screened from Daqu and the relationship between the changes of microbial population and the aroma formation was studied. This article also preliminary study the safety problems of Daqu. The main research contents are as follows:
Volatile compounds in Daqu samples were extracted by headspace solid phase microextraction and analyzed by gas chromatography-mass spectrum (GC-MS). Comparing volatiles with the quality of Daqu by sensory analysis, electronic noses (EN) method was adopted to analyse Daqu with GC-MS. The method is quick, simple and less sample consumption. Most volatiles of Daqu can be extracted by this method, and the repeatability and recovery of some compounds were satisfactory. A total of 75 volatile compounds were characterized by GC-MS, including alcohols, esters, acids, aromatic compounds, phenols, furans, nitrogen-containing compounds, aldehydes and ketones. By a principal component analysis (PCA), the ten Daqu samples could be classified into three groups according to their origins, and in particular, the production technologies. In this case, Daqu samples fermented by middle temperature procedure formed a clear group; Daqu samples fermented by high temperature procedure formed two different groups. Daqu also be analyzed by electronic noses (EN) method, different samples of daqu has certain response to electronic nose. As can be seen from the radar map, the trend of common and high quality of medium temperature Daqu and common quality of high temperature Daqu were similar, but the trend of high quality of high temperature Daqu was different. Odorants of Daqu extracted by solvent-assisted flavour evaporation (SAFE) were investigated by gas chromatography-olfactometry (GC-O) system with two olfactometric methods: detection frequency (DF) method and aroma extract dilution analysis (AEDA). Based on the results of the two olfactometric method (FD and DF), the aroma of medium temperature Daqu could be primarily attributed to hexanal, unknown (no.u2), phenylacetaldehyde and 4-ethyl guaiacol; the aroma of high temperature Daqu could be primarily attributed to hexanal, 2,6-dimethylpyrazine, nonanal, 1-octene-3-ol, phenylacetaldehyde, 4-ethyl guaiacol and unknown (no.u2, u3, u5 and u7).
Based on sensory properties, the relationship of microorganisms, physicochemical indexes and enzymes of different quality of Daqu were analyzed. The results show that the numbers of microorganisms in good clothing Daqu were more than the numbers of microorganisms in poor clothing Daqu, especially the number of moulds. The activities of most enzymes and esterifying capability in commom quality Daqu were lower than those in high quality Daqu, but the esterifying power of breaking was lower in high quality Daqu than commom quality Daqu, which would be good for producing volatile compounds. Besides, fermentation ability and total free amino acids of high quality Daqu was higher than that of commom quality Daqu too. The changes of microorganisms, physicochemical indexes, enzymes, volatile compounds and sensory during Daqu fermentation and storage were studied. The water content and humidity decreased gradually during fermentation and then remained stable during storage and the temperature rose rapidly as fermentation progressed during the first 3 days and peaked on the seventh day. The evolutions of physicochemical indexes, enzymes, flavour and sensory was related to microbial growth. The total microbial population including bacillus, yeast and mould proliferated rapidly at the preliminary stage of fermentation. With the rising of temperature and declining of water content and humidity, the environment was no longer suitable for the growth of microorganisms in medium temperature Daqu. Bacillus species have a better ability than other microorganism to survive under high water content and high temperature in high temperature Daqu. There were two peak hours of producing acidity in Daqu, and the acidity decreased as the the numbers of microorganisms decreased. A total of 46 volatile compounds were identified and measured in the Daqu samples using HS-SPME-GC-MS. The sum of the nitrogen-containing compounds showed a slowly increase from the first day to the third day and followed by a sharp increase from the third day to the ninth day of fermentation, and then decreased gradually. The evolution of each group of volatile compounds during fermentation and storage of Daqu had a relationship with the change of physical index and microflora and determined the aroma intensity of Daqu. This made it possible to optimize the productive technology of Daqu on the basis of the contents of volatile compounds. The aroma intensity of fruity, flowery and clove increased on the first five days and then decreased gradually. The result was in line with the change of aroma content and showed that fermentation period had significant impacts on the aroma score.
A total of 93 moulds, 112 yeasts and 45 bacilli were screened and identified using different culture during during Daqu fermentation and storage. After primary screening and secondary screening, ZY-1 and GY-3 were identified as Issatchenkia orientalis and Candida xylopsoci through ITS sequence analysis, ZL-1 and GL-4 were identified as Bacillus subtilis and Bacillus licheniformis through 16SrDNA sequence analysis. The aroma-producing conditions of ZL-1 and GL-4 were optimized. ZL-1 and GL-4 have a great influence in promoting brown of medium through model Maillard reaction, and the brown reached a maximum on 6th day. The changes of total free amino acid, the activity of proteases and reducing sugar during fermentation were studied. Compared with the fermentation products after sterilization and inactivation of enzyme by high temperature, the fermentation products after sterilization by membrane filtration smelled stronger sauce aroma. The volatile compounds of ZL-1 and GL-4 fermentation product were analyzed by GC-MS. 2,3-butanedione, 2,3,5-trimethyl pyrazine, 2,3,5,6-Tetramethylpyrazine and guaiacol could have a relationship with characteristic flavour of Daqu. The volatile compounds of ZY-1 and GY-3 fermentation product were esters, alcohols and ketones which could have a relationship with aroma-producing of Daqu.
Brewing experiment was carried out using different quality of Daqu. The results indicated that the total content of esters, free amino acids and acids in liquor produced by high quality Daqu were better than those in liquor produced by common quality Daqu. The total aldehydes and solid content had little difference in the different quality Daqu, but the alcohol content had features obviously difference from each other. The volatile compounds of high quality Daqu was higher than those of common quality Daqu. Numbers of the volatile compounds producing by angel yeast were less than those producing by Daqu, which reflects the importance of Daqu in producing aroma during liquor production. Four typical toxin producing by moulds were tested by HPLC which had a satisfactory repeatability and recovery. The content of four typical toxin producing by moulds did not exceed national or international standard. Because of the complexity of the special traditional techniques of Chinese liquor, there is little chance to bring toxin producing by moulds to Chinese liquor.
使用一种简便、快速、灵敏的顶空固相微萃取-气相色谱-质谱联用法(GC-MS)测定曲样中的挥发性化合物,并配合电子鼻(EN)技术,比较了仪器分析与感官判别大曲质量的关系。顶空固相微萃取-气相色谱-质谱联用法(GC-MS)能将大曲样品中的醇类、吡嗪、醛类、酮类和酯类等挥发性物质较好地萃取出来,对大曲样品中具有代表性的挥发性成分如酯类、醇类和吡嗪类等测定的结果重复性良好,同时具有较高的加标回收率。利用GC-MS对不同的大曲样品进行分析,共检测出挥发性化合物75种,包括的挥发性风味物质分别有:醇类物质、酸类物质、酯类物质、醛类物质、酮类物质、芳香族化合物、酚类物质、呋喃类物质和含氮类化合物;采用主成分分析方法分析10种大曲中的挥发性化合物,十种大曲能够被区分为三大类,发酵温度不高于60℃的中温大曲的优级大曲和普级大曲在主成分分析图上距离较为接近,而高温大曲的优级大曲和普级大曲能够明显分成两类;采用电子鼻(EN)技术分析大曲样品,不同大曲样品对电子鼻有一定的响应,从雷达图可以发现,中温优级大曲、中温普级大曲和高温普级大曲的雷达图趋势较为相似,而高温优级大曲与上述三种大曲趋势较为不同,与其它三种大曲的气味存在较大的差异;依据气相-嗅闻法(GC-O)的频率检测法(DF)和香气提取稀释分析法(AEDA)两种方法考察了中温优级大曲和高温优级大曲,依据DF值和FD值的大小判断香气物质对大曲香气的贡献程度,结果表明:中温优级大曲中的特征香气成分可能主要是由己醛、未知化合物(no.u2)、苯乙醛和4-乙基愈创木酚等化合物组成;高温优级大曲中的特征香气可能主要是由己醛、2,6-二甲基吡嗪、壬醛、1-辛烯-3-醇、苯乙醛、4-乙基愈创木酚和未知化合物(no.u2、u3、u5和u7)组成;其它挥发性化合物可能作为背景香气物质。
从感官特征的角度,分析了不同等级的大曲在微生物组成、酶、理化成分等方面的区别,并分析了风味物质形成的外部条件。结果表明,优级大曲的“穿衣”情况要比普级大曲好且均匀,其微生物数量多,尤其是霉菌数量更为明显;优级大曲中主要酶的活力均高于普级大曲,优级大曲的酯化力高于普级大曲,而酯分解率低于普级大曲,有利于促进风味物质的形成,优级大曲的发酵力和游离氨基酸总量均高于普级大曲。对大曲在发酵期间的各项指标,包括微生物数量、理化指标、酶、风味变化和感官变化进行跟踪测定发现:随着发酵时间的延长,中、高温大曲中的水分含量和水活度都呈现下降的趋势;温度表现为先升后降;大曲中微生物的数量和种类与曲醅的温度、水分含量、水活度和pH等多种因素息息相关,中温大曲的微生物数量在发酵起始均有小幅度增加,但是随温度的增加和水活度的降低,大曲中的一些不耐热的微生物大量死亡;而高温大曲由于其特殊的工艺条件,大曲维持在一个高温高湿的环境,耐热的芽孢杆菌能够正常生长代谢;两类大曲在发酵过程中均出现一个产酸高峰期,随着微生物数量的递减,酸度也减低。使用顶空固相微萃取-质谱联用技术考察了中温大曲在发酵和贮存培菌期间的风味物质的变化,共检测出46种化合物,在大曲发酵的第5天多数风味物质含量达到最大值,而在大曲发酵的第9天含氮类化合物含量才达到最大,在大曲发酵30天时挥发性风味物质含量趋于稳定,这为优化大曲生产工艺提供了理论依据。对大曲在发酵期间的香气物质进行定量描述和分析,大曲的果香、花香和辛香等香气物质在发酵的前5天快速增加,随着发酵的进行这些香气物质在第5天后开始下降,香气变化的规律与利用气质联用方法检测到的化合物含量变化规律较为相似。
对大曲发酵和贮存各个时期的微生物进行了分离、纯化、筛选和鉴定,对产香微生物模拟发酵产生香气成分的机理进行了探索。利用多种培养基进行微生物分离,得到霉菌93株,酵母菌112株,嗜热芽孢杆菌45株。通过初筛和复筛从中温大曲和高温大曲中分别筛选到能产香的酵母菌ZY-1和GY-3和产香芽孢杆菌ZL-1和GL-4;利用分子生物学和生理生化鉴定方法确定,ZY-1属于东方伊萨酵母,GY-3属于假丝酵母属的一种,ZL-1是枯草芽孢杆菌,GL-4是地衣芽孢杆菌。对ZL-1和GL-4菌株产香条件进行优化,考察了美拉德模式反应,ZL-1和GL-4均能促进培养基褐变物质的生成,采用小麦浸出液在37℃~55℃(37℃、45℃和55℃各2天)发酵的第6天褐变程度最高;对发酵液在发酵过程中蛋白酶活力、游离氨基酸和还原糖含量进行了跟踪测定,考察了除菌灭酶对发酵液香气的影响。利用气质联用技术测定ZL-1和GL-4发酵液,发现2,3-丁二酮、三甲基吡嗪、四甲基吡嗪和愈创木酚可能与大曲香气成分的形成有一定的关系。利用小麦浸出液培养ZY-1和GY-3两种酵母,酵母在发酵过程中主要生成一些酯类、醇类和酮类等挥发性风味物质,可见产香酵母是大曲中风味物质形成的重要原因。
进行了大曲单独酿酒实验和大曲安全性研究,发现大曲质量与白酒产量、品质和风味有密切联系。两种温度类型大曲的优级大曲发酵产酒、总酸和总酯量均高于普级大曲,所酿白酒的品质在很大程度由大曲质量决定,四类大曲发酵所产白酒中的固形物及总醛含量差异较小,但酒精的含量却差异显著,同时在氨基酸总量也不同,高温优级大曲酒的挥发性化合物总量明显高于中温优级大曲酒,但是挥发性风味物质的总量上相差不是太大,这与检测出的高温优级大曲和中温优级大曲中的挥发性风味成分数量上的趋势一致,安琪高活性酿酒酵母组挥发性风味组分的总量与大曲酒相差不大,但是在挥发性化合物数目上相差较多,这也从一个侧面反映出,大曲在提高大曲酒风味成分上的作用。利用HPLC方法测定了大曲中4种具有代表性的真菌毒素,该方法具有很好的精密度和回收率,大曲中检测到的4种真菌毒素含量均未超过国家或国际上通用的限量标准。由于白酒酿造的后续工艺,大曲中毒素被最终带入到白酒成品的可能性极小。
In China, using Daqu to initiate the solid fermentations for the production of Chinese liquor is the key technology which is a major difference from the other famous distilled spirits in the world. Daqu is a type of grain Qu, which is mainly made from raw wheat and by natural inoculation. Daqu is the major source of microorganisms, enzymes, flavour compounds and their precursors in Chinese liquor process. Its quality is directly related to the yield and the quality of Chinese liquor. Medium and high temperature Daqu which were produced by Luzhou Laojiao Company located in Luzhou China was studied here. Characteristic flavours, physicochemical indexes and enzymes of medium and high temperature Daqu were analyzed. Aroma-producing microorganisms were screened from Daqu and the relationship between the changes of microbial population and the aroma formation was studied. This article also preliminary study the safety problems of Daqu. The main research contents are as follows:
Volatile compounds in Daqu samples were extracted by headspace solid phase microextraction and analyzed by gas chromatography-mass spectrum (GC-MS). Comparing volatiles with the quality of Daqu by sensory analysis, electronic noses (EN) method was adopted to analyse Daqu with GC-MS. The method is quick, simple and less sample consumption. Most volatiles of Daqu can be extracted by this method, and the repeatability and recovery of some compounds were satisfactory. A total of 75 volatile compounds were characterized by GC-MS, including alcohols, esters, acids, aromatic compounds, phenols, furans, nitrogen-containing compounds, aldehydes and ketones. By a principal component analysis (PCA), the ten Daqu samples could be classified into three groups according to their origins, and in particular, the production technologies. In this case, Daqu samples fermented by middle temperature procedure formed a clear group; Daqu samples fermented by high temperature procedure formed two different groups. Daqu also be analyzed by electronic noses (EN) method, different samples of daqu has certain response to electronic nose. As can be seen from the radar map, the trend of common and high quality of medium temperature Daqu and common quality of high temperature Daqu were similar, but the trend of high quality of high temperature Daqu was different. Odorants of Daqu extracted by solvent-assisted flavour evaporation (SAFE) were investigated by gas chromatography-olfactometry (GC-O) system with two olfactometric methods: detection frequency (DF) method and aroma extract dilution analysis (AEDA). Based on the results of the two olfactometric method (FD and DF), the aroma of medium temperature Daqu could be primarily attributed to hexanal, unknown (no.u2), phenylacetaldehyde and 4-ethyl guaiacol; the aroma of high temperature Daqu could be primarily attributed to hexanal, 2,6-dimethylpyrazine, nonanal, 1-octene-3-ol, phenylacetaldehyde, 4-ethyl guaiacol and unknown (no.u2, u3, u5 and u7).
Based on sensory properties, the relationship of microorganisms, physicochemical indexes and enzymes of different quality of Daqu were analyzed. The results show that the numbers of microorganisms in good clothing Daqu were more than the numbers of microorganisms in poor clothing Daqu, especially the number of moulds. The activities of most enzymes and esterifying capability in commom quality Daqu were lower than those in high quality Daqu, but the esterifying power of breaking was lower in high quality Daqu than commom quality Daqu, which would be good for producing volatile compounds. Besides, fermentation ability and total free amino acids of high quality Daqu was higher than that of commom quality Daqu too. The changes of microorganisms, physicochemical indexes, enzymes, volatile compounds and sensory during Daqu fermentation and storage were studied. The water content and humidity decreased gradually during fermentation and then remained stable during storage and the temperature rose rapidly as fermentation progressed during the first 3 days and peaked on the seventh day. The evolutions of physicochemical indexes, enzymes, flavour and sensory was related to microbial growth. The total microbial population including bacillus, yeast and mould proliferated rapidly at the preliminary stage of fermentation. With the rising of temperature and declining of water content and humidity, the environment was no longer suitable for the growth of microorganisms in medium temperature Daqu. Bacillus species have a better ability than other microorganism to survive under high water content and high temperature in high temperature Daqu. There were two peak hours of producing acidity in Daqu, and the acidity decreased as the the numbers of microorganisms decreased. A total of 46 volatile compounds were identified and measured in the Daqu samples using HS-SPME-GC-MS. The sum of the nitrogen-containing compounds showed a slowly increase from the first day to the third day and followed by a sharp increase from the third day to the ninth day of fermentation, and then decreased gradually. The evolution of each group of volatile compounds during fermentation and storage of Daqu had a relationship with the change of physical index and microflora and determined the aroma intensity of Daqu. This made it possible to optimize the productive technology of Daqu on the basis of the contents of volatile compounds. The aroma intensity of fruity, flowery and clove increased on the first five days and then decreased gradually. The result was in line with the change of aroma content and showed that fermentation period had significant impacts on the aroma score.
A total of 93 moulds, 112 yeasts and 45 bacilli were screened and identified using different culture during during Daqu fermentation and storage. After primary screening and secondary screening, ZY-1 and GY-3 were identified as Issatchenkia orientalis and Candida xylopsoci through ITS sequence analysis, ZL-1 and GL-4 were identified as Bacillus subtilis and Bacillus licheniformis through 16SrDNA sequence analysis. The aroma-producing conditions of ZL-1 and GL-4 were optimized. ZL-1 and GL-4 have a great influence in promoting brown of medium through model Maillard reaction, and the brown reached a maximum on 6th day. The changes of total free amino acid, the activity of proteases and reducing sugar during fermentation were studied. Compared with the fermentation products after sterilization and inactivation of enzyme by high temperature, the fermentation products after sterilization by membrane filtration smelled stronger sauce aroma. The volatile compounds of ZL-1 and GL-4 fermentation product were analyzed by GC-MS. 2,3-butanedione, 2,3,5-trimethyl pyrazine, 2,3,5,6-Tetramethylpyrazine and guaiacol could have a relationship with characteristic flavour of Daqu. The volatile compounds of ZY-1 and GY-3 fermentation product were esters, alcohols and ketones which could have a relationship with aroma-producing of Daqu.
Brewing experiment was carried out using different quality of Daqu. The results indicated that the total content of esters, free amino acids and acids in liquor produced by high quality Daqu were better than those in liquor produced by common quality Daqu. The total aldehydes and solid content had little difference in the different quality Daqu, but the alcohol content had features obviously difference from each other. The volatile compounds of high quality Daqu was higher than those of common quality Daqu. Numbers of the volatile compounds producing by angel yeast were less than those producing by Daqu, which reflects the importance of Daqu in producing aroma during liquor production. Four typical toxin producing by moulds were tested by HPLC which had a satisfactory repeatability and recovery. The content of four typical toxin producing by moulds did not exceed national or international standard. Because of the complexity of the special traditional techniques of Chinese liquor, there is little chance to bring toxin producing by moulds to Chinese liquor.
引文
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