Optimization of Chief Fermentation Process and Quality Evaluation of Mulberry Wine Based on Response Surface Method

doi:10.6048/j.issn.1001-4330.2022.03.013

Abstract

Abstract:

【Objective】 To study the chief fermentation technology of mulberry wine with Xinjiang native variety “Qiangeli” mulberry as raw material. 【Methods】 Based on the single factor test, the box Behnken response surface optimization test was carried out and the optimal main fermentation technology parameters of mulberry wine were determined through the test: yeast addition 0.22 g/kg, fermentation temperature 21-23℃, sulfur dioxide addition 80 mg/kg. 【Results】 The results showed that mulberry wine not only had good taste, but also was rich in total flavonoids (2.66 g/L), anthocyanins (0.34 g/L) and other active substances. Meanwhile, 24 volatile aroma compounds were identified, including esters 77.86% of the total aroma substances, followed by 19.07% of the alcohols. 【Conclusion】 The optimal main fermentation parameters of mulberry fruit wine were obtained: the addition of yeast was 0.22 g/kg, the fermentation temperature was 21-23 ℃, and the addition of sulfur dioxide was 80 mg / kg.

Key words: response surface design; mulberry wine; technology; aroma; quality

摘要：

【目的】基于响应面法研究对桑葚果酒的主发酵工艺,评价其品质,为新疆桑葚果酒的工业化生产提供科学依据。【方法】以新疆桑葚品种仟格丽桑葚果为原材料,在单因素试验的基础上进行Box-Behnken响应面优化试验,确定桑葚果酒最优主发酵工艺参数:酵母添加量0.22 g/kg、发酵温度21~23℃、二氧化硫(SO₂)添加量为80 mg/kg。并对最优主发酵工艺酿造出的桑葚果酒理化指标、感官风味、挥发性香气进行分析。【结果】桑葚果酒不仅口感佳,且富含总黄酮(2.66 g/L)、花色苷(0.34 g/L)等活性物质,鉴定出桑葚果酒中24种挥发性香气化合物主要挥发性香气化合物,其中酯类物质含量占总香气物质含量的77.86%,其次是醇类物质占19.07%。【结论】桑葚果酒最优主发酵工艺参数:酵母添加量0.22 g/kg、发酵温度21~23 ℃、二氧化硫添加量为80 mg/kg。

关键词: 响应面设计, 桑葚果酒, 工艺, 香气, 品质

CLC Number:

S663.9
S38

YANG Lu, FAN Shaoli, LI Hong, CHENG Ping, ZHANG Zhigang. Optimization of Chief Fermentation Process and Quality Evaluation of Mulberry Wine Based on Response Surface Method[J]. Xinjiang Agricultural Sciences, 2022, 59(3): 634-644.

杨璐, 范少丽, 李宏, 程平, 张志刚. 基于响应面法优化桑葚果酒主发酵工艺及其品质评价[J]. 新疆农业科学, 2022, 59(3): 634-644.

Figures/Tables 11

Table 1 factors of box-behnken scheme design and horizontal coding

水平编码 Horizontal coding	A	B	C
水平编码 Horizontal coding	发酵温度 Fermentation temperature (℃)	酵母浓度 Yeast concentration (g/kg)	SO₂添加量 SO₂ addition (mg/kg)
-1	16~18	0.1	30
0	20~22	0.2	50
1	24~26	0.3	80

Table 2 Chromatographic conditions: heating procedure

升温速率 Heating rate (℃/min)	温度 Temperature (℃)	保持时间 Holding time (min)
/	50	2
5	120	2
6	250	10

Fig.1 Effect of yeast varieties on the alcohol content, pH value, reducing sugar, residual sugar content, total acid of mulberry wine Note: There are significant differences in the expression of different lowercase letters (P < 0.05), the same as below

Fig.2 Effect of yeast concentration on the alcohol content, pH value, reducing sugar, residual sugar content, total acid, of mulberry wine

Fig.3 Effect of fermentation temperature on the alcohol content, pH value, reducing sugar, residual sugar content, total acid of mulberry wine

Table 3 Design and results of response interview experiments

序号 No.	A酵母浓度 Yeast concentration (g/kg)	B发酵温度 Fermentation temperature(℃)	CSO₂添加量 SO₂ dosage (mg/kg)	酒精度 Alcohol content (%vol)
1	-1	0	-1	10.2
2	1	0	1	10.9
3	1	-1	0	9.8
4	-1	1	0	10.6
5	0	0	0	11.2
6	0	-1	1	10.3
7	0	0	0	11.4
8	0	1	1	11.1
9	1	0	-1	10.7
10	-1	-1	0	9.6
11	0	1	-1	11.5
12	-1	0	1	11.5
13	0	0	0	11.2
14	0	0	0	11.3
15	1	1	0	11.0
16	0	-1	-1	9.8
17	0	0	0	11.3

Table 4 Experimental results regression model variance analysis

方差来源	平方和	自由度	均方	F值	P值	显著性
模型 Model	6.05	9	0.67	13.62	0.001 2	${^{}}^{}$
A-酵母浓度Yeast concentration	0.031	1	0.031	0.63	0.452 3
B-发酵温度Fermentation temperature	2.76	1	2.76	55.94	0.000 1	${^{}}^{}$
C-SO₂添加量Content of SO₂	0.32	1	0.32	6.48	0.038 3	^*
AB	1.00E-02	1	1.00E-02	0.2	0.666 2
AC	0.3	1	0.3	6.13	0.042 5	^*
BC	0.2	1	0.2	4.1	0.082 5
A^2	0.82	1	0.82	16.52	0.004 8	${^{}}^{}$
B^2	1.47	1	1.47	29.7	0.001	${^{}}^{}$
C^2	9.47E-04	1	9.47E-04	0.019	0.893 7
残差 Residual	0.35	7	0.049
失拟项 Lack of Fit	0.32	3	0.11	15.12	0.012	^*
纯误差Pure Error	0.028	4	7.00E-03
总和Cor Total	6.4	16

Table 4 Experimental results regression model variance analysis

方差来源	平方和	自由度	均方	F值	P值	显著性
模型 Model	6.05	9	0.67	13.62	0.001 2	${^{}}^{}$
A-酵母浓度Yeast concentration	0.031	1	0.031	0.63	0.452 3
B-发酵温度Fermentation temperature	2.76	1	2.76	55.94	0.000 1	${^{}}^{}$
C-SO₂添加量Content of SO₂	0.32	1	0.32	6.48	0.038 3	^*
AB	1.00E-02	1	1.00E-02	0.2	0.666 2
AC	0.3	1	0.3	6.13	0.042 5	^*
BC	0.2	1	0.2	4.1	0.082 5
A^2	0.82	1	0.82	16.52	0.004 8	${^{}}^{}$
B^2	1.47	1	1.47	29.7	0.001	${^{}}^{}$
C^2	9.47E-04	1	9.47E-04	0.019	0.893 7
残差 Residual	0.35	7	0.049
失拟项 Lack of Fit	0.32	3	0.11	15.12	0.012	^*
纯误差Pure Error	0.028	4	7.00E-03
总和Cor Total	6.4	16

Fig.4 3D response surface of interaction between factors

Table 5 GC-MS analysis of volatile aroma compounds

序号 No.	香气化合物 Aroma compounds	保留时间 Retention time (min)	含量 Content (%)	气味描述 Odor description
A	酯类
1	己酸乙酯	9.311	8.483	果香、草莓香^[17]
2	琥珀酸氢乙酯	14.350	0.477	/
3	丁二酸二乙酯	14.678	4.786	/
4	辛酸乙酯	15.185	9.659	果香、奶油味^[18]
5	甘油1,2-二乙酸酯	16.436	0.343	/
6	苯乙酸乙酯	16.488	0.304	蜂蜜香^[17]
7	乙酸苯乙酯	16.835	0.459	玫瑰、茉莉花香^[17]
8	壬酸乙酯	17.963	0.602	酒心巧克力香味^18]
9	苯丙酸乙酯	19.417	8.291	草莓香、奶酪味^[18]
10	癸酸乙酯	20.657	20.163	奶油味、果香^[19]
12	月桂酸乙酯	25.560	16.716	甜香、蜂蜡香^[18]
13	苯甲酸乙基己酯	28.139	0.224	/
14	肉豆蔻酸乙酯	29.970	4.423	椰子、蜂蜡香^[17]
15	棕榈酸乙酯	34.001	2.705	水果味、奶油味^[17]
序号 No.	香气化合物 Aroma compounds	保留时间 Retention time (min)	含量 Content (%)	气味描述 Odor description
16	亚油酸乙酯	37.084	0.226	/
B	醇类
17	乙醇	1.133	17.972	/
18	苯乙醇	12.717	1.094	玫瑰花香、甜香^[20]
C	酸类
19	己酸	8.823	0.777	乳酪、甜香^[18]
20	辛酸	14.457	0.603	脂肪味、奶油味^[18]
F	其他
21	2,3-二氢-3,5-二羟基-6-甲基-4H-吡喃-4-酮	13.574	0.574	/
22	丁香酚	19.502	0.433	丁香香气^[21]
23	二氢大马酮	20.234	0.354	/
24	4-羟基-4-甲基-4H-萘-1-酮	20.391	0.331	/

Table 6 Results of physical and chemical indexes of mulberry wine

项目 Project		测定结果 Determination results
pH		4.11±0.02
色差 Chromatic aberration	L值	22.3±0.6
	a值	3.3±2.1
	b值	-6.3±1.5
可溶性固形物 Soluble solids (%)		12.27±0.06
总糖 Total sugar (g/L)		20.22±0.77
可滴定酸 Total acid (g/L)		13.26±0.03
酒精度 Alcohol content (%vol)		11.3±0.29
总酚 Total phenols (g GAE/L)		17.29±0.22
总黄酮 Total flavonoids (g/L)		2.66±0.06
花色苷 Anthocyanins (g/L)		0.34±0.04

Fig.5 Radar map of sensory analysis

References 21

[1]	杨璐, 卢晓丽, 程平, 等. 基于灰色关联度和主成分分析法的桑葚品质综合评价体系构建[J]. 新疆农业科学, 2017(5): 862-870.
	YANG Lu, LU Xiaoli, CHENG Ping, et al. Establishing Comprehensive Evaluation System for Mulberry Based on Grey Relational Grade Analysis and Principal Component Analysis[J]. Xinjiang Agricultural Sciences, 2017,(5): 862-870.
[2]	王贺, 韩爱芝, 贾清华, 等. 新疆药桑和黑桑营养成分及活性成分分析[J]. 食品科学, 2016, 37(8): 91-96.
	WANG He, HAN Aizhi, JIA Qinghua, et al. Analysis of Nutrient Components and Active Ingredients of Morusnigra L. and M.alba L.var.tatarica in Xinjiang Autonomous Region[J]. Food Science, 2016, 37(8): 91-96.
[3]	张荷兰, 陆鸿奎, 郭晓敏, 等. 桑葚保健食品的研究与分析[J]. 食品与发酵科技, 2018, 54(5): 125-128.
	ZHANG Helan, LU Hongkui, GUO Xiaomin, et al. Research and Analysis of Mulberry Health Food[J]. Food and Fermentation Sciences & Technology, 2018, 54(5): 125-128.
[4]	Sun Z, Li L I, Wenfang M A. Research and Prospect of Mulberry (Morus alba L.)[J]. Agricultural Biotechnology, 2019, 8(4): 136-139.
[5]	叶学林, 程水明, 温露文, 等. 响应面法优化桑葚果酒发酵工艺[J]. 中国酿造, 2017, 36(12): 105-109.
	YE Xuelin, CHENG Shuiming, WEN Luwen, et al. Optimization of fermentation technology for mulberry wine by response surface methodology[J]. Agricultural Biotechnology, 2017, 36(12): 105-109.
[6]	杨芳, 王中兴, 王克刚, 等. 星点设计-响应面法优化桑葚果酒发酵工艺[J]. 酿酒科技, 2017,(12): 21-26.
	YANG Fang, WANG Zhongxing, WANG Kegang, et al. Optimization of the Fermentation Process of Mulberry Wine by Central Composite Design-Response Surface Method[J]. Liquor-Making Science & Technology, 2017,(12): 21-26.
[7]	王婷, 毛亮, 雷静, 等. 优质桑葚酒酿造工艺的研究[J]. 酿酒科技, 2015,(1): 86-88, 92.
	WANG Ting, MAO Liang, LEI Jing, et al. The Producing Techniques of Quality Mulberry Wine[J]. Liquor-Making Science & Technology, 2015,(1): 86-88, 92.
[8]	孔瑾, 李双银, 娄文娟, 等. 生料法制取山楂发酵果酒及果醋工艺技术研究[J]. 食品研究与开发, 2016, 37(17): 92-97.
	KONG Jin, LI Shuangyin, LOU Wenjuan, et al. Study on the Process of Hawthorn Vinegar and Hawthorn Wine[J]. Food Research and Development, 2016, 37(17): 92-97.
[9]	高海生, 蔺毅峰, 李春华, 等. 干红毛樱桃酒酿造工艺研究[J]. 中国食品学报, 2002,(1): 17-21.
	GAO Haisheng, LIN Yifeng, LI Chunhua, et al. Study on the Technique of Producing "Prunus tomentosa Thunb" Wine[J]. Journal of Chinese Institute of Food Science and Technology, 2002,(1): 17-21.
[10]	杨宁, 王伟明, 姚琳, 等. 3,5-二硝基水杨酸法测定发酵型果露酒中总糖含量[J]. 中国酿造, 2018, 37(1): 181-184.
	YANG Ning, WANG Weiming, YAO Lin, DONG Kun. Determination of total sugar content in fermented fruit wine by 3,5-dinitrosalicylic acid method[J]. China Brewing, 2018, 37(1): 181-184.
[11]	GBT 12456-2008. 食品中总酸的测定[S].
	GBT 12456-2008. Determination of total acid in foods[S].
[12]	张红娟. 陕西关中平原与渭北旱塬生态区红色酿酒葡萄品质研究[D]. 杨凌:西北农林科技大学, 2018.
	ZHANG Hongjuan. Study on the quality of red wine grape in Shaanxi Guanzhong Plain and Weibei dryland ecological region[D]. Yangling: Northwest A&F University, 2018.
[13]	李傲然, 胡倬瑜, 杨宁, 等. 银杏大麦酒的酿造工艺及品质分析[J]. 中国酿造, 2019, 38(1): 200-206.
	LI Aoran, HU Zhuoyu, YANG Ning, et al. Brewing process and quality analysis of ginkgo-barley wine[J]. China Brewing, 2019, 38(1): 200-206.
[14]	郭浩然, 郑心怡, 张静, 等. 桑葚酒中花青素含量的测定方法优化[J]. 食品工业科技, 2020, 41(9): 255-259.
	GUO Haoran, ZHENG Xinyi, ZHANG Jing, et al. Optimization of Determination Method of Anthocyanin Content in Mulberry Wine[J]. Science and Technology of Food Industry, 2020, 41(9): 255-259.
[15]	蔡德萍, 谈安群, 孙志高, 等. 不同脱气温度下溶解氧含量对非浓缩还原橙汁品质的影响[J]. 食品与发酵工业, 2019, 45(20): 169-175.
	CAI Deping, TAN Anqun, SUN Zhigao, et al. Effect of dissolved oxygen content on the quality of NFC orange juice degassed at different temperatures[J]. Food and Fermentation Industries, 2019, 45(20): 169-175.
[16]	鲁榕榕, 马腾臻, 张波, 等. 不同澄清剂对起泡葡萄酒原酒的澄清作用及对香气品质的影响[J]. 食品科学, 2018, 39(12): 146-153.
	LU Rongrong, MA Tengzhen, ZHANG Bo, et al. Effect of Different Clarifying Agents on Clarification and Aroma Quality of Sparkling Base Wine[J]. Food Science, 2018, 39(12): 146-153.
[17]	陈霞, 李敏, 张波, 等. 扩展青霉对‘蛇龙珠’葡萄酒棒曲霉素及风味品质的影响[J]. 食品科学, 2016, 37(20): 126-133.
	CHEN Xia, LI Min, ZHANG Bo, et al. Effect of Penicillium expansum Infection of Grapes on Patulin Content and Flavor Quality of Cabernet Gernischt Wine[J]. Food Science, 2016, 37(20): 126-133. DOI URL
[18]	Englezos V, Torchio F, Cravero F, et al. Aroma profile and composition of Barbera wines obtained by mixed fermentations of Starmerella bacillaris (synonym Candida zemplinina) and Saccharomyces cerevisiae[J]. LWT-Food Science and Technology, 2016, (73): 567-575.
[19]	谢春梅, 焦红茹, 曹芳玲. 宁夏青铜峡小产区不同品种干红葡萄酒的香气成分分析[J]. 中国酿造, 2018, 37(1): 170-176.
	XIE Chunmei, JIAO Hongru, CAO Fangling. Analysis on aroma components of dry red wines with different varieties of grape from Ningxia Qingtongxia region[J]. China Brewing, 2018, 37(1): 170-176.
[20]	丁吉星, 何玉云, 梁艳英, 等. 新型嘉宝果起泡酒香气成分及特征香气分析[J]. 食品科学, 2014, 35(24): 145-150.
	DING Jixing, HE Yuyun, LIANG Yanying, et al. Analysis of Volatile Aroma Compounds and Aromatic Characteristics from Jaboticaba Sparkling Wine[J]. Food Science, 2014, 35(24): 145-150.
[21]	周强, 沈旭, 付梦, 等. 炒制与烤制工艺对洽洽香瓜子呈香组分的影响[J]. 食品工业, 2017, 38(1): 53-57.
	ZHOU Qiang, SHEN Xu, FU Meng, et al. Effect of Frying and Roasting Processing Technologies on Aroma Components in Chacheer Aromatic Sunflower Seeds[J]. Food Industry, 2017, 38(1): 53-57.