Production method of pepper wheat fragrant liquor

Abstract

The present application belongs to the technical field of flavor liquor prepared by reusing pepper cake, and particularly relates to a method for extracting pepper insoluble dietary fiber (IDF) and producing pepper wheat-flavor liquor; pepper cake is used as raw material to prepare pepper soluble dietary fiber (SDF) and insoluble dietary fiber (IDF); the experimental comparison shows that the extraction yield of pepper IDF is higher, the antioxidant capacity is stronger, the porosity is larger, and the adsorption effect is better. In the fermentation process of the liquor, the pepper IDF is used to replace the rice husk used in the method for preparing wheat-flavor liquor, the pepper IDF can improve the composition of the microbial flora in the fermentation process of fermented grains, and then improve the composition of liquor components and flavor components, so as to prepare a kind of pepper wheat-flavor liquor.

Description

Technical Field

[0001] This invention belongs to the field of technology for preparing flavored liquor by reusing Sichuan pepper cakes, and particularly relates to a method for producing Sichuan pepper-flavored liquor. Background Technology

[0002] In the context of the "Big Health" era, people are paying increasing attention to healthy lifestyles and dietary habits, and the concept of "medicine and food sharing the same origin" has gradually become a focus of public attention. "Medicine and food sharing the same origin" means that many foods are also medicines, and there is no absolute dividing line between them. To date, the State Council's health administration department has released four batches of lists of substances that are both food and traditional Chinese medicine, totaling 106 substances, including Sichuan pepper. Sichuan pepper usually refers to the pericarp of mature Sichuan peppercorns, commonly used as a seasoning; the mature seeds are also called pepper seeds. Pepper seeds are bitter and cold in nature, and have the effects of promoting urination and relieving asthma, often used to treat edema, cough, asthma, and inability to lie flat. Pepper seeds can be physically pressed to produce Sichuan pepper oil; the remaining Sichuan pepper cake is mainly composed of fiber and also contains a large number of physiologically active substances (polyphenols, flavonoids, etc.), but these are not being utilized rationally.

[0003] Wheat-flavored baijiu is a type of baijiu made primarily from wheat, with wheat comprising over 50% of the raw material. Rice husks are an indispensable functional auxiliary material in baijiu brewing, widely used in stages such as grain steaming, fermentation, and distillation. During baijiu fermentation, rice husks mainly enhance the fluffiness of the mash, improve aeration, increase dissolved oxygen levels, and prevent excessive decomposition and rapid acidification. However, the raw bran flavor and bitter compounds inherent in rice husks can negatively impact the flavor of the baijiu. Therefore, minimizing the amount of rice husks used while maintaining the aeration of the mash has always been a significant technical challenge in baijiu brewing. Summary of the Invention

[0004] This invention aims to improve the dissolved oxygen content and increase the abundance of aerobic and facultative anaerobic microorganisms during the fermentation of baijiu (Chinese liquor) by preparing a Sichuan pepper IDF with antioxidant activity and high porosity. This alters the microbial community of the mash, resulting in a richer flavor profile and unique liquor characteristics. This innovative strategy will contribute new scientific evidence to the flavor diversification of malt-flavored baijiu and lay a theoretical foundation for the development of novel Sichuan pepper-malt-flavored baijiu.

[0005] To achieve the above objectives, the technical solution adopted by the present invention is as follows:

[0006] A method for producing Sichuan pepper and wheat-flavored baijiu includes the following steps:

[0007] S1. Raw material pretreatment: The fermentation raw materials are proportioned by weight as follows: wheat 50%–70%, sorghum 20%–35%, rice, glutinous rice and corn 5%–20% each; the sorghum and koji are crushed and passed through a 1.2mm sieve, and the sorghum, corn and wheat are weighed according to the proportion and then moistened at high temperature;

[0008] S2. Preparation of Sichuan pepper IDF: Sichuan pepper cake was crushed and passed through a 120-mesh sieve. Distilled water was added at a solid-liquid weight ratio of 1:5~10. The pH was adjusted to 8.0 with caustic soda and boiled for 30 min. The pH was adjusted to 5.5~6.5 with dilute sulfuric acid. 0.5%~1% of thermostable α-amylase was added and enzymatically hydrolyzed in a water bath at 60℃ for 1 h, followed by boiling for 5 min. 0.5%~1% of papain was added at pH 6.0 and enzymatically hydrolyzed in a water bath at 50℃ for 1 h, followed by boiling for 5 min. 0.5%~1% of cellulase was added at pH 6.0 and enzymatically hydrolyzed in a water bath at 45℃ for 1 h, followed by boiling for 5 min. The mixture was filtered, the precipitate was collected, and dried at 65℃ to obtain the final product.

[0009] S3. Steaming the raw materials: After soaking the sorghum, corn and wheat, add rice and glutinous rice, add 3% to 5% of the total weight of the raw grains and add pepper IDF. Mix well and then sprinkle them into the steamer. After the steam comes up, add 10% to 20% of the 50 to 60°C hot water and steam for 60 minutes.

[0010] S4. Cooling: Remove the steamed grains from the steamer while they are still hot and spread them out into a rectangle. Pour in 30% to 50% of the amount of raw materials in hot water at 50 to 60 degrees Celsius to allow the starch to further absorb water and swell. Then stir and toss the mixture to allow it to cool and ventilate.

[0011] S5. Add the crushed starter culture at 2% to 5% of the original grain weight and mix well.

[0012] S6. Stacking: Add 5% of the weight of the original grain of pepper IDF to the stacked material. Before stacking, the moisture content of the stacked material should be controlled at 70% to 80%. Stack the raw materials into a trapezoidal shape with a stacking height of 20 to 40 cm. During the stacking process, control the temperature of the center of the stack to not exceed 35℃. Turn the material over immediately after it reaches 35℃.

[0013] S7. Fermentation: The fermentation container is a stainless steel fermentation box. The packing quantity is calculated based on the dry grain raw material. Each fermentation box has a packing quantity of 200 kg and a fermentation cycle of 30 days.

[0014] S8. Distillation: After 30 days of fermentation, the mash is removed from the vat and mixed with auxiliary materials, including 2%–5% of the original grain weight of Sichuan pepper IDF. After mixing evenly, the mash is loaded into the still and the lid is closed to start distillation. 1 kg of the first distillate is collected from each still. Distillation is carried out in stages: high-proof liquor is below 60% alcohol content, medium-proof liquor is above 50% alcohol content, and low-proof liquor is above 35% alcohol content. When the alcohol content is below 35%, distillation is stopped and the mash is discarded.

[0015] S9. Storage and Aging: The high, medium and low grades of distilled spirits are stored in ceramic jars, and the sealed jars are placed in a cellar for aging. The cellar temperature is controlled at 15℃~20℃ and the humidity is controlled at 60%~70%. The aging time is no less than 12 months.

[0016] S10. Blending: Based on the quality standards and taste requirements of the finished product, base spirits from different years and batches are selected for blending. The blending ratio is determined according to the spirit design plan, generally using the main spirit in the middle section as a base, with the addition of appropriate amounts of high-proof and low-proof spirits. For finished spirits with a volume of 50% or higher, the proportion of the middle section spirits should not be less than 50%.

[0017] Furthermore, the moistening process in step S1 is as follows: after mixing sorghum, corn and wheat evenly, add 50% to 70% of their weight in hot water at 70°C to 80°C, stir evenly, pile up and moisten for 24 hours, turning over once every 6 hours during the moistening process.

[0018] Furthermore, the pepper cake in step S2 is the cake made by physically pressing pepper seeds to extract oil.

[0019] The advantages of this invention are as follows: This invention aims to prepare insoluble dietary fiber (IDF) and soluble dietary fiber (SDF) from Sichuan pepper cake as raw material. Experimental comparisons show that Sichuan pepper IDF has a higher extraction yield, stronger antioxidant capacity, larger porosity, and better adsorption effect. Using Sichuan pepper IDF to replace rice husks in the traditional method during baijiu fermentation can improve the composition of the microbial community during fermentation, thereby improving the composition and flavor of the liquor and producing a Sichuan pepper-flavored baijiu. Specific experimental data shows that replacing 5% rice husks with 5% Sichuan pepper insoluble fiber can reduce the abundance of Lactobacillus acetotolerans and Saccharomyces cerevisiae in the mash, while increasing the abundance of Weissella cibaria and Cyberlindnera fabianii, thus maintaining the stability of the microbial community during fermentation. Further results showed that the content of ethyl lactate and ethyl acetate, the skeletal aroma components, was higher in the Sichuan pepper-wheat aroma-type Baijiu. Correlation analysis indicated that the decrease in the abundance of *Saccharomyces* (brewing yeast) reduced the concentration of 4-methoxyphenol (CAS: 150-76-5, pungent, combustible aroma), while the increase in the abundance of *Cyberlindnera fabianii* and *Weissella cibaria* increased the concentrations of ethyl 3-methylvalerate (CAS: 5870-68-8, fruity aroma) and 2-hexanofuran (CAS: 14360-50-0, green bean aroma, honey aroma). The data demonstrate that the Sichuan pepper-wheat aroma-type Baijiu prepared by this method removes the pungent and irritating odor of Sichuan pepper, endowing it with unique flavor characteristics. Attached Figure Description

[0020] Figure 1 These are electron micrographs of Sichuan pepper fibers in an embodiment of the present invention (scale bar 50 μm).

[0021] Figure 2 The Top 10 represents the relative abundance of bacteria and fungi in the fermented mash of the control group and the Sichuan pepper group at 0 days and 30 days in this invention.

[0022] Figure 3This is a Pearson correlation analysis diagram of differential microorganisms and flavor components in the fermented mash of Sichuan pepper wine of the present invention; Note: The values ​​in the squares represent the Pearson correlation coefficients, and * indicates P < 0.05; 4-methoxyphenol (CAS: 150-76-5, odor, burning taste), 2-hexanoylfuran (CAS: 14360-50-0, green bean taste), 1,1-diethoxy-2-methylbutane (CAS: 3658-94-4, fruit taste) and ethyl 3-methylvalerate (CAS: 5870-68-8, pineapple, fruit taste). Detailed Implementation Example

[0023] 1. A method for producing a Sichuan pepper and wheat-flavored baijiu, comprising the following steps:

[0024] S1. Raw material pretreatment: The fermentation raw materials are proportioned by weight as follows: wheat 50%–70%, sorghum 20%–35%, rice, glutinous rice, and corn 5%–20% each; the sorghum and koji are crushed and passed through a 1.2mm sieve. After weighing the sorghum, corn, and wheat according to the proportion, they are moistened at high temperature. The moistening operation is as follows: after mixing the sorghum, corn, and wheat evenly, add 50%–70% of their weight of hot water at 70℃–80℃, stir evenly, and pile up for moistening for 24 hours. During the moistening process, the mixture is turned over once every 6 hours.

[0025] S2. Preparation of Sichuan pepper IDF: Sichuan pepper cake was crushed and passed through a 120-mesh sieve. The Sichuan pepper cake is the pepper cake after physical pressing to extract oil. Distilled water was added at a solid-liquid weight ratio of 1:5~10. The pH was adjusted to 8.0 with caustic soda and boiled for 30 min. The pH was adjusted to 5.5~6.5 with dilute sulfuric acid. 0.5%~1% of thermostable α-amylase was added and enzymatically hydrolyzed in a water bath at 60℃ for 1 h, followed by boiling for 5 min. Then, 0.5%~1% of papain was added at pH 6.0 and enzymatically hydrolyzed in a water bath at 50℃ for 1 h, followed by boiling for 5 min. Finally, 0.5%~1% of cellulase was added at pH 6.0 and enzymatically hydrolyzed in a water bath at 45℃ for 1 h, followed by boiling for 5 min. The mixture was filtered, the precipitate was collected, and dried at 65℃ to obtain the final product.

[0026] S3. Steaming the raw materials: After soaking the sorghum, corn and wheat, add rice and glutinous rice, add 3% to 5% of the total weight of the raw grains and add pepper IDF. Mix well and then sprinkle them into the steamer. After the steam comes up, add 10% to 20% of the 50 to 60°C hot water and steam for 60 minutes.

[0027] S4. Cooling: Remove the steamed grains from the steamer while they are still hot and spread them out into a rectangle. Pour in 30% to 50% of the amount of raw materials in hot water at 50 to 60 degrees Celsius to allow the starch to further absorb water and swell. Then stir and toss the mixture to allow it to cool and ventilate.

[0028] S5. Add the crushed starter culture at 2% to 5% of the original grain weight and mix well.

[0029] S6. Stacking: Add 5% of the weight of the original grain of pepper IDF to the stacked material. Before stacking, the moisture content of the stacked material should be controlled at 70% to 80%. Stack the raw materials into a trapezoidal shape with a stacking height of 20 to 40 cm. During the stacking process, control the temperature of the center of the stack to not exceed 35℃. Turn the material over immediately after it reaches 35℃.

[0030] S7. Fermentation: The fermentation container is a stainless steel fermentation box. The packing quantity is calculated based on the dry grain raw material. Each fermentation box has a packing quantity of 200 kg and a fermentation cycle of 30 days.

[0031] S8. Distillation: After 30 days of fermentation, the mash is removed from the vat and mixed with auxiliary materials, including 2%–5% of the original grain weight of Sichuan pepper IDF. After mixing evenly, the mash is loaded into the still and the lid is closed to start distillation. 1 kg of the first distillate is collected from each still. Distillation is carried out in stages: high-proof liquor is below 60% alcohol content, medium-proof liquor is above 50% alcohol content, and low-proof liquor is above 35% alcohol content. When the alcohol content is below 35%, distillation is stopped and the mash is discarded.

[0032] S9. Storage and Aging: The high, medium and low grades of distilled spirits are stored in ceramic jars, and the sealed jars are placed in a cellar for aging. The cellar temperature is controlled at 15℃~20℃ and the humidity is controlled at 60%~70%. The aging time is no less than 12 months.

[0033] S10. Blending: Based on the quality standards and taste requirements of the finished product, base spirits from different years and batches are selected for blending. The blending ratio is determined according to the spirit design plan, generally using the main spirit in the middle section as a base, with the addition of appropriate amounts of high-proof and low-proof spirits. For finished spirits with a volume of 50% or higher, the proportion of the middle section spirits should not be less than 50%.

[0034] Experimental Example

[0035] 2 Materials and Methods

[0036] 2.1 Materials and Equipment

[0037] Cellulase (10 U / g, catalog number: A8751), papain (100,000 U / g, catalog number: G8431), Sichuan pepper cake and radish seed cake were provided by Henan Langyan Biotechnology Development Co., Ltd.; anhydrous ethanol was from Tianjin Dengke Chemical Reagent Co., Ltd.; and high-temperature resistant α-amylase (4,000,000 U / g, catalog number: C8260) was purchased from Beijing Solarbio Technology Co., Ltd.

[0038] 2.2 Nutritional Composition Analysis of the Two Raw Material Cakes

[0039] After drying the Sichuan pepper cake and radish seed cake at 65℃ to constant weight, their nutritional composition was analyzed. Crude protein was determined using GB / T6432-201 (7.2 total content method), crude fat using GB / T6433-2006, crude ash using GB / T6433-2007, crude fiber using GB / T6434-2022 (6 filter bag method), and starch using GB / T20194-2018.

[0040] 2.3 Extraction of soluble and insoluble dietary fiber

[0041] Accurately weigh 10 g each of pre-dried Sichuan pepper cake and radish seed cake powder. Add distilled water according to a solid-liquid ratio of 1:10 (W / V), adjust the pH to 8.0 with caustic soda, boil for 30 min, adjust the pH to 5.5-6.5 with dilute sulfuric acid, add 0.5%–1% thermostable α-amylase, and hydrolyze in a 60℃ water bath for 1 h, followed by boiling for 5 min. Add 0.5%–1% papain at pH 6.0, hydrolyze in a 50℃ water bath for 1 h, followed by boiling for 5 min. Add 0.5%–1% cellulase at pH 6.0, hydrolyze in a 45℃ water bath for 1 h, followed by boiling for 5 min. After hydrolysis, centrifuge at 7000 r / min for 10 min and collect the corresponding precipitate and supernatant. Wash the precipitate twice with pure water and once with 75% ethanol, then remove moisture in a constant temperature drying oven to obtain insoluble dietary fiber (IDF). The supernatant was precipitated with 75% ethanol (volume ratio 1:4) for 12 h, centrifuged at 8500 r / min for 10 min, and then washed, dried and weighed to collect soluble dietary fiber (SDF).

[0042] 2.4 Detection of in vitro antioxidant properties

[0043] 2.4.1 Determination of total phenols and total flavonoids

[0044] Total phenol determination: Take 0.1 mL of the sample solution, add 0.5 mL of Folin-Ciocalteu reagent, mix well and let stand for 2 min, add 0.5 mL of sodium carbonate solution and 0.9 mL of distilled water, mix well and let stand for 10 min, then measure the absorbance at 760 nm. Total flavonoid determination: Take 0.4 mL of the sample solution, add 0.06 mL of 5% sodium nitrite solution, mix well, let stand at 25 ℃ for 6 min, then add 0.12 mL of 10% aluminum nitrate solution, mix well, let stand at 25 ℃ for 6 min, then add 0.42 mL of 4% sodium hydroxide solution, mix well, let stand at 25 ℃ for 15 min, then measure the absorbance at 510 nm.

[0045] 2.4.2 Effect of different fibers on glucose adsorption capacity

[0046] 0.1 g of insoluble and soluble fiber from Sichuan pepper were placed in 250 mL Erlenmeyer flasks, and 100 mL of a pre-prepared 1 mg / mL glucose solution was added. The mixture was reacted in a constant temperature water bath at 35 °C for 60 min, followed by vacuum filtration using a 0.45 μm PVDF membrane (50 mm diameter). The filtrate was collected, its volume was measured, and the glucose concentration in the filtrate was determined using the DNS method. The results are expressed as the amount of glucose adsorbed per g of sample (μmol / g).

[0047] 2.4.3 Scanning electron microscopy analysis of Sichuan pepper fibers

[0048] Samples were observed using a JSM-7900F scanning electron microscope. The samples were dispersed on conductive adhesive on the sample stage, sputtered with gold, and then observed and images were captured.

[0049] 2.5 Brewing of Sichuan Pepper Wheat Wine

[0050] Step 1: Raw Material Pretreatment. The fermentation raw material ratio is: wheat 50%–70%, sorghum 20%–35%, and rice, glutinous rice, and corn added at 5%–20%. Sorghum is crushed using a roller crusher, with the powder passing through a 1.2mm sieve controlled at 25%–35%. Corn and wheat are not crushed. After weighing the sorghum, corn, and wheat according to the ratio, the grains are moistened at high temperature. 50%–70% hot water (70℃–80℃) is added by weight, stirred evenly, and piled up for moistening for 24 hours to allow the grains to fully absorb water. During the moistening process, the mixture is turned over every 6 hours to ensure uniform moistening. The Daqu (fermentation starter) is pulverized, with ≤50% passing through a 1.2mm sieve.

[0051] Step 2: Preparation of Sichuan pepper IDF. Sichuan pepper cake is pulverized through a 120-mesh sieve. At a solid-liquid ratio of 1:5-10 (W / V), distilled water is added, and the pH is adjusted to 8.0 with caustic soda. The mixture is boiled for 30 min, and the pH is adjusted to 5.5-6.5 with dilute sulfuric acid. 0.5%–1% of thermostable α-amylase is added, and the mixture is enzymatically hydrolyzed in a 60°C water bath for 1 h, followed by boiling for 5 min. At pH 6.0, 0.5%–1% of papain is added, and the mixture is enzymatically hydrolyzed in a 50°C water bath for 1 h, followed by boiling for 5 min. Finally, at pH 6.0, 0.5%–1% of cellulase is added, and the mixture is enzymatically hydrolyzed in a 45°C water bath for 1 h, followed by boiling for 5 min. The mixture is filtered, the precipitate is collected, and dried at 65°C to obtain Sichuan pepper IDF.

[0052] Step 3: Steaming the raw materials. After soaking the sorghum, corn, and wheat, add rice and glutinous rice, and add Sichuan pepper (IDF) at 3%–5% of the total weight of the raw grains. Mix well and then sprinkle the mixture into the steamer. After the steam rises, add 10%–20% hot water (50-60℃) and steam for 60 minutes.

[0053] Step 4: Cooling. Remove the steamed grains from the steamer while they are still hot and spread them out into a rectangle. Pour in hot water (55-60℃) equal to 30% of the weight of the raw materials to allow the starch to further absorb water and swell. Then stir and toss the mixture to allow it to cool and ventilate.

[0054] Step 5: Add the starter culture. Add 2% to 5% of the total grains using the crushed starter culture, stir well, and mix thoroughly.

[0055] Step 6: Stacking. Add 5% Sichuan pepper IDF, and control the moisture content to 70%–80% before stacking. Stack the raw materials into a trapezoidal shape, with a stack height of 20–40 cm. During the stacking process, control the center temperature of the stack to not exceed 35℃. Turn the material over immediately after it reaches 35℃.

[0056] Step 7: Fermentation. The experiment was conducted at the Baijiu Brewing Training Center of the School of Biological and Food Engineering, Huanghuai University. Stainless steel fermentation tanks were used as fermentation containers. Three fermentation tanks were designed as replicates, with each tank containing 200 kg of dry grain. The fermentation period was 30 days.

[0057] Step 8: Distillation. After 30 days of fermentation, remove the mash from the vat and mix it with auxiliary materials, adding 2%–5% Sichuan pepper IDF and stirring thoroughly. After loading the still, cover it and begin distillation; collect 1 kg of the first distillate from each still; collect the distillate in stages: high-proof (alcohol content below 60% V / V), medium-proof (alcohol content above 50% V / V), and low-proof (alcohol content below 35% V / V). When the alcohol content drops below 35% (V / V), stop collecting the distillate and discard the mash.

[0058] Step 9: Storage and Aging. The high, medium, and low grades of distilled spirits are stored separately in ceramic jars. The sealed jars are then placed in a cellar for aging. The cellar temperature is controlled at 15℃-20℃, and the humidity is controlled at 60%-70%. The aging time is no less than 12 months.

[0059] Step 10: Blending. Based on the quality standards and taste requirements of the finished product, select base spirits from different years and batches for blending. The blending ratio is determined according to the spirit design plan, generally using the main spirit from the middle section as a base, adding appropriate amounts of high-proof and low-proof spirits. For finished spirits with a volume of 50% or higher, the proportion of the middle section spirit should not be less than 50%.

[0060] Three additional fermentation chambers were set up as a control group. In steps 3, 6, and 8, the same weight of rice husks was used to replace the Sichuan pepper IDF. The rice husks were pre-steamed, and the open-top steaming time was no less than 60 minutes. The remaining operations were the same.

[0061] 2.6 Microbial community analysis of mash fermented for 30 days

[0062] DNA was extracted from fermented mash samples after 30 days of fermentation. Bacterial PCR amplification of the V3-V4 variable region of the 16S rRNA gene was performed using 341 F (5'-CCTAYGGGRBGCASCAG-3') and 806 R (5'-GGACTACHVG GGTWTCTAAT-3'), respectively. PCR amplification of the 18S rRNA gene was performed using 547 F (5'-CAGCASCYGCGGTAATTCC-3') and 2043 R (5'-ACTTTCGTTCTTGATYRA-3'). The PCR products were then quantified and homogenized. Library construction was performed using the NEXTFLEX Rapid DNA-Seq Kit, and sequencing was performed using the Illumina Miseq PE300 platform. Raw data were uploaded to the SRA database for alignment analysis (https: / / www.arb-silva.de / ).

[0063] 2.7 Analysis of wine sample components

[0064] A 52% vol sample of naturally distilled spirits was collected for component analysis. Fourteen components, including ethyl acetate, ethyl butyrate, ethyl hexanoate, ethyl lactate, n-propanol, β-phenylethanol, acetic acid, hexanoic acid, and ethyl propionate, were determined according to the method in GB / T 10345-2022.

[0065] 2.8 Flavor component analysis (GC-MS)

[0066] Analysis of flavor components in Sichuan pepper cake. Sichuan pepper cake was pre-frozen at -80℃ for 48 h, then ground in liquid nitrogen and vortexed until homogeneous. Approximately 500 mg was collected in a headspace vial. Saturated NaCl solution and 20 μL of 10 μg / mL internal standard solution were added. Finally, sample extraction was performed using automated headspace solid-phase microextraction (HS-SPME). Under HS-SPME conditions, the sample was shaken at 60℃ for 5 min, followed by extraction in the headspace for 15 min using a 120 µm DVB / CWR / PDMS extraction headpiece, and finally eluented at 250℃ for 5 min. Chromatographic conditions: A DB-5MS capillary column was used with high-purity helium as the carrier gas at a flow rate of 1.2 mL / min and an injection port temperature of 250℃. Temperature program: 40℃ was held for 3.5 min, then increased to 100℃ at 10℃ / min, then to 180℃ at 7℃ / min, and finally to 280℃ at 25℃ / min and held for 5 min. Mass spectrometry conditions: Electron impact ionization (EI) source, ion source temperature 230℃, ion detection mode (SIM) selected for precise scanning of qualitative and quantitative ions. Data analysis was performed by Jiangsu Sanshu Biotechnology Co., Ltd.

[0067] Flavor component analysis of control group baijiu and pepper cake baijiu samples. 1 mL of each sample was placed in a headspace vial, and saturated NaCl and 20 μL of internal standard solution were added. Sample extraction was performed using fully automated headspace solid-phase microextraction (HS-SPME) for GS-MS analysis, following the same procedure as above.

[0068] 2.9 Correlation Analysis

[0069] Based on the flavor component analysis, four flavor components with the greatest significant differences and that have been labeled were selected and an environmental factor table was prepared (see Table 1). Correlation analysis was also performed with the differentially expressed microorganisms.

[0070] Table 1 Environmental Factors Table

[0071]

[0072] 2.10 Data Processing

[0073] All experimental data are expressed as mean ± standard deviation. Analysis of variance (ANOVA) was performed using SPSS 20.0, and Duncan's multiple-range test was used to compare differences in means. A p-value < 0.05 was considered statistically significant.

[0074] 3 Results and Analysis

[0075] 3.1 Nutritional composition analysis and extraction yield of the two raw materials

[0076] The nutritional composition analysis of the two raw materials is shown in Table 2. As can be seen from Table 2, the fiber content of Sichuan pepper cake is similar to that of rice husk, but it also contains more protein and fat.

[0077] Table 2. Nutritional composition analysis of the two raw materials (%)

[0078]

[0079] The yields of SDF and IDF extracted from the two types of pepper cakes are shown in Table 3. As shown in Table 3, SDF yielded the highest yield of pepper cake, reaching 8.2%, significantly higher than the other two groups (P < 0.05). IDF yielded the highest yield of pepper cake, reaching 40.10%, also significantly higher than the other two groups (P < 0.05).

[0080] Table 3. SDF and IDF yields (%) of the two types of cakes after the experiment.

[0081]

[0082] Note: Identical uppercase letters in the same row indicate no significant difference (P>0.05); different uppercase letters in the same row indicate significant difference (P<0.05); identical lowercase letters in the same row indicate no significant difference (P>0.05); different lowercase letters in the same row indicate significant difference (P<0.05); the same applies below.

[0083] 3.2 Analysis of total phenols and total flavonoids

[0084] As shown in Table 4, the total phenol content of Sichuan pepper SDF and IDF was the highest, at 3.97 and 4.14 mg / g, respectively; the total polyphenol content of Sichuan pepper SDF and IDF was also the highest, at 2.67 and 2.77 mg / g, respectively.

[0085] Table 4 Total phenolic content (mg / g) of SDF and IDF in the two cakes

[0086]

[0087] 3.3 Effect of different fibers on glucose adsorption capacity

[0088] As shown in Table 5, the glucose adsorption capacity of Sichuan pepper SDF and IDF was 14.18 and 17.25 mmol / g, respectively, which was significantly higher than that of radish seed SDF and IDF.

[0089] Table 5. Effects of different fibers on glucose adsorption capacity

[0090]

[0091] 3.4 Observation of the fiber structure of Sichuan pepper

[0092] Scanning electron microscopy results of Sichuan pepper cake, soluble fiber, and insoluble fiber from Sichuan pepper are shown below. Figure 1 ,Depend on Figure 1 It is evident that the structure of Sichuan pepper cake is compact, with fibers, proteins, and starches cross-linked to form a dense structure. In contrast, the structures of soluble and insoluble fibers in Sichuan pepper are significantly looser, containing numerous cavities, presumably left after the enzymatic hydrolysis of proteins and starches. These cavities further increase the surface area of ​​the fibers, thereby increasing dissolved oxygen capacity. This aligns with the results regarding glucose adsorption capacity, suggesting that Sichuan pepper IDF has a higher specific surface area and a greater number of micropores.

[0093] Comprehensive analysis shows that Sichuan pepper insoluble dietary fiber (IDF) has a higher extraction yield, stronger antioxidant capacity, larger fiber structure porosity, and better adsorption effect. Sichuan pepper IDF was selected for subsequent brewing experiments.

[0094] 3.5 Analysis of the microbial community of fermented mash

[0095] The relative abundance of bacteria and fungi in fermented mash at 0 days and 30 days are shown in the figures below. Figure 2 A and Figure 2 B. By Figure 2It was found that during the 30-day fermentation process, the abundance of *Lactobacillus acetotolerans* in the control group increased from 84.13% to 99.43%, while the relative abundance of *Weissella cibaria* decreased from 12.62% to 0.3% (P < 0.05). The addition of Sichuan pepper inhibited the growth of *Lactobacillus acetotolerans*, and there was no significant difference in the relative abundance of *Lactobacillus acetotolerans* and *Weissella cibaria* before and after fermentation (P > 0.05). Similar to the bacterial trends, the abundance of *Saccharomyces cerevisiae* increased from 84.71% to 99.45% during 30 days of fermentation, while the abundance of *Cyberlindnera fabianii* decreased from 14.59% to 0.59%. There were no significant differences in the abundance of the top two fungi in the *Zanthoxylum bungeanum* group before and after fermentation (P > 0.05). These results suggest that *Zanthoxylum bungeanum* may maintain the stability of the microbial community during fermentation by inhibiting the growth of lactic acid bacteria.

[0096] Table 6. Abundance composition of bacteria and fungi in fermented mash after 30 days of fermentation.

[0097]

[0098] 3.6 Analysis of Wine Components

[0099] The composition of the control group and the Sichuan pepper liquor is shown in Table 7. Table 7 shows that the ethyl lactate content was the highest in both liquors, with the Sichuan pepper liquor containing 1308.21 mg / L, significantly higher than the control group (P < 0.05). The furfural and ethyl hexanoate contents in the Sichuan pepper liquor were also significantly higher than those in the control group (P < 0.05). Compared with the control group, the sec-butanol and ethyl butyrate contents in the Sichuan pepper liquor were significantly lower (P < 0.05), and the methanol content in both liquors was far below the national standard of 600 mg / L.

[0100] Table 7. Analysis of wine components (mg / L)

[0101]

[0102] Note: Identical lowercase letters in the same row indicate no significant difference (P > 0.05); different lowercase letters in the same row indicate significant difference (P < 0.05); the same applies below.

[0103] 3.7 Flavor Component Analysis

[0104] 3.7.1 Analysis of flavor components in Sichuan pepper cake

[0105] The flavor analysis of the Sichuan pepper cake is shown in Table 8. Table 8 reveals that it contains 15 components, including terpenes, esters, and ketones. Terpenes, esters, and ketones are the most abundant, with 374, 324, and 199 species respectively. The D-limonene content among the terpenes is 720.12 mg / kg, significantly higher than other groups. P <0.05); the content of isomenthyl acetate in the ester was 106.64 mg / kg, which was significantly higher than that in other groups ( P <0.05); the content of 2-hydroxy-3,4-dimethyl-2-cyclopenten-1-one in the ketone was 71.61 mg / kg, which was significantly higher than that in other groups ( P <0.05).

[0106] Table 8. Analysis of flavor components in Sichuan pepper cake

[0107]

[0108]

[0109]

[0110] 3.7.2 Analysis of flavor components in Sichuan pepper liquor

[0111] The component analysis of Sichuan pepper liquor is shown in Table 9. The components were ranked according to their FC (Sichuan pepper liquor group / control group liquor) values ​​greater than 1 and less than 1, and the top 10 aroma components were selected for analysis. Table 9 shows that ethyl pentyl 3-methylvalerate and 1,1-diethoxy-2-methylbutane, among the ester components, were significantly enriched in Sichuan pepper, with contents increasing by 4840 and 4800 times, respectively, compared to the control group. Compared to the control group, 4-methoxyphenol and 2-hexanoylfuran were significantly reduced in the Sichuan pepper liquor, with contents decreasing by 2659 and 518 times, respectively.

[0112] Table 9. Analysis of Flavor Components in Sichuan Pepper Wine

[0113]

[0114] 3.8 Correlation Analysis

[0115] Based on the flavor component analysis results, four flavor components with significant differences were selected, and correlation analysis was performed with the abundance values ​​of differentially expressed fungi and bacteria (Table 6). The results are shown below. Figure 3 .Depend on Figure 3 It can be known that the Sichuan pepper wine mash contains... Saccharomyces The abundance of (Saccharomyces cerevisiae) was positively correlated with the content of CAS:150-76-5 (4-methoxyphenol). Cyberlindnera fabianii The abundance of ethyl 3-methylvalerate (CAS: 5870-68-8) was positively correlated with the content of (Febien Seberlindnerella vaginalis) (P < 0.05). Weissella cibaria Lactobacillus acetotoleransThe abundance of *Westernella esculenta* was positively correlated with the content of 2-hexanoylfuran (CAS: 14360-50-0) (P < 0.05).

[0116] 4. Conclusion

[0117] This invention compares the composition and antioxidant activity differences between Sichuan pepper fiber and radish seed fiber. The results show that Sichuan pepper insoluble dietary fiber (IDF) has a higher extraction yield, stronger antioxidant capacity, larger porosity, and better adsorption effect. Using Sichuan pepper IDF to replace rice husks in the traditional baijiu fermentation process can improve the composition of the microbial community during fermentation, thereby improving the composition and flavor of the liquor and producing a Sichuan pepper-flavored baijiu. The fiber with the highest dietary fiber content and strongest antioxidant activity from Sichuan pepper was selected. By using Sichuan pepper IDF to replace rice husks in the baijiu brewing process, a Sichuan pepper-flavored baijiu can be prepared. Data analysis shows that Sichuan pepper IDF can inhibit... Saccharomyces (Acid-fast Lactobacillus) and Saccharomyces The increased abundance of (Saccharomyces cerevisiae) maintains the stability of the microbial community in the mash and increases the content of ethyl lactate and ethyl acetate, which are the backbone aroma components in the liquor; correlation analysis shows that... Cyberlindnera fabianii The stability of (Saccharomyces cerevisiae) abundance reduced the concentration of odorous 4-methoxyphenol (CAS: 150-76-5). Weissella cibaria (Fibrian Seberlindnerella vaginalis) and ​ The increased abundance of *Westernella esculenta* increased the concentrations of ethyl 3-methylvalerate (CAS: 5870-68-8) and 2-hexanoylfuran (CAS: 14360-50-0), which have a fruity aroma.

Claims

1. A production method of a Zanthoxylum bungeanum-flavor Maotai-flavor liquor, characterized in that, Comprise the following steps: S1. Raw material pretreatment: the fermentation raw material is proportioned by weight as follows: wheat 50%~70%, sorghum 20%~35%, rice, glutinous rice and corn 5%~20%; the sorghum and Daqu are crushed to pass through a 1.2mm sieve, the sorghum, corn and wheat are weighed according to the proportion, and the high-temperature material is moistened; S2. Preparation of zanthoxylum bungeanum insoluble dietary fiber: after the zanthoxylum bungeanum cake is crushed to pass through a 120-mesh sieve, distilled water is added at a solid-liquid weight ratio of 1:5~10, NaOH is added to adjust the pH to 8.0, it is boiled for 30 min, dilute sulfuric acid is added to adjust the pH to 5.5~6.5, 0.5%~1% of high-temperature-resistant alpha amylase is added, it is hydrolyzed in a water bath at 60℃ for 1h, it is boiled for 5 min again, 0.5%~1% of papain is added at pH 6.0, it is hydrolyzed in a water bath at 50℃ for 1h, it is boiled for 5 min again, 0.5%~1% of cellulase is added at pH 6.0, it is hydrolyzed in a water bath at 45℃ for 1h, it is boiled for 5 min again, it is filtered, the precipitate is collected, and it is dried at 65℃ to obtain the product; S3. Raw material cooking: after the moistened sorghum, corn and wheat, rice and glutinous rice are added, 3%~5% of zanthoxylum bungeanum insoluble dietary fiber is added based on the total weight of the raw grains, it is mixed uniformly, and then it is put into a steamer together, after the steam is turned on, 10%~20% of hot water at 50~60℃ is added, and it is steamed for 60 min; S4. Cooling: after the steamed raw grains are taken out of the steamer, they are spread into a rectangle, 30%~50% of hot water at 50~60℃ is poured on them, the starch is allowed to further absorb water and swell, and then the grains are stirred and ventilated to cool down; S5. Daqu addition: 2%~5% of crushed Daqu is added based on the total weight of the grains, and it is mixed uniformly; S6. Stacking: 5% of zanthoxylum bungeanum insoluble dietary fiber is added based on the weight of the raw grains, the moisture content of the stacked material is controlled to be 70%~80% before stacking, the raw grains are stacked into a trapezoidal shape, the stacking height is 20~40 cm, the center temperature of the material pile is controlled to be not more than 35℃ during stacking, and the material is turned over immediately after the temperature reaches 35℃; S7. Fermentation: stainless steel fermentation boxes are used for fermentation, the loading capacity is 200 kg of dry grains per box, and the fermentation period is 30 d; S8. Distillation: after 30 d of fermentation, the fermented grains are taken out of the tank, auxiliary materials are added, 2%~5% of zanthoxylum bungeanum insoluble dietary fiber is added, it is stirred uniformly, the distillation is started after the distillation pot is closed, 1 kg of head wine is taken out per pot, the wine is taken out in stages, the high-grade wine has a degree of less than 60%, the medium-grade wine has a degree of more than 50%, the low-grade wine has a degree of more than 35%, the distillation is stopped when the degree is less than 35%, and the grains are discarded; S9. Storage and aging: the high, medium and low grade wines obtained by distillation are respectively stored in ceramic jars, the sealed jars are placed in a cellar for aging, the temperature of the cellar is controlled to be 15℃~20℃, the humidity is controlled to be 60%~70%, and the aging time is not less than 12 months; S10. Blending.

2. The production method of the Zanthoxylum bungeanum-flavored Chinese liquor according to claim 1, characterized in that: The material moistening operation in the step S1 is as follows: after the sorghum, corn and wheat are uniformly mixed, 50%-70% of the weight of the mixture is added with hot water at 70-80 DEG C, and stirred uniformly, and then the mixture is stacked for 24 hours, and the mixture is stirred every 6 hours during the stacking.

3. The production method of the Zanthoxylum bungeanum-flavored Chinese liquor according to claim 1, characterized in that: The Zanthoxylum bungeanum seed cake in the step S2 is the cake remained after the Zanthoxylum bungeanum seeds are physically pressed to extract oil.

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