Brewing method for enhancing radix aucklandiae flavor of white spirit

Abstract

The invention discloses a brewing method for enhancing radix aucklandiae flavor of baijiu, and belongs to the field of baijiu brewing. The preparation method comprises the following steps: uniformly mixing a nano material, pottery clay and water, and molding to obtain a costus root regulator; wherein the nano material is selected from more than two of Pt-Pb coated SiO2-Al2O3, SiO2 and Al2O3; and then adding a radix aucklandiae regulator in the process of storing the aged white spirit to enhance the radix aucklandiae flavor of the white spirit. According to the preparation method, the radix aucklandiae regulator is added during preparation of the pottery jar, so that the flavor components of the Baijiu are improved, and characteristic substances such as radix aucklandiae are greatly improved; according to the present invention, the contents of the raw materials such as acetovanillin, fenugreek lactone, 4-ethyl phenol, 4-vinyl guaiacol, 3-methyl-2, 4-nonanedione, piperonone and the like are substantially improved.

Description

Technical Field

[0001] The invention relates to a brewing method for enhancing the woody flavor of liquor, and belongs to the field of liquor brewing. Background Art

[0002] The woody flavor in liquor is a complex aroma that is popular with consumers. It usually comes from a series of volatile compounds produced during the fermentation and aging process of liquor. The woody flavor can increase the layering and depth of liquor and bring a pleasant sensory experience to drinkers.

[0003] At present, the method of regulating the woody flavor in liquor is usually carried out in multiple links such as raw material selection, fermentation process, aging process and post-seasoning. Raw material selection is to use raw materials with specific woody precursors, such as certain types of grains or add specific wood extracts; fermentation process optimization is to use specific yeast strains that can produce more woody compounds for fermentation and promote the production of woody compounds by controlling fermentation conditions (such as temperature, humidity, fermentation time); aging technology is to age in specific aging containers (such as oak barrels) to allow the wine to absorb wood components and increase woody aroma; or use specific enzyme treatment to promote the conversion of woody precursors; post-seasoning is to add a certain proportion of woody flavoring agents to the liquor or enhance the woody aroma through spice extracts, etc.

[0004] However, the above-mentioned methods for regulating the woody flavor in liquor have problems such as high cost (using special raw materials or yeast strains may increase production costs), high technical difficulty (precise control of fermentation and aging conditions requires professional technology and experience), difficulty in flavor balance (over-emphasis on woody flavor may destroy the overall flavor balance of liquor), and long aging time (the traditional aging process may take a long time, affecting production efficiency).

[0005] Therefore, how to use a simple, efficient and convenient method to regulate and enhance the woody flavor of liquor is an urgent problem to be solved in the field of liquor brewing. Summary of the invention

[0006] [Technical issues]

[0007] Conventional methods for regulating the woody flavor in liquor have problems such as high cost, high technical difficulty, long aging time, and difficulty in balancing flavors.

[0008] [Technical solution]

[0009] In order to solve the above problems, the present invention provides a brewing method for enhancing the woody flavor of liquor, wherein the method comprises firstly mixing nanomaterials, clay and water evenly, and molding to obtain a woody flavor regulator; wherein the nanomaterial is Pt-Pb@SiO 2 -Al 2 O 3 、SiO2 、Al 2 O 3 Then, during the storage of aged liquor, a woody aroma regulator is added to enhance the woody aroma of the liquor. The method of the present invention is simple to operate and can enhance the woody aroma of the liquor in a short time.

[0010] The first object of the present invention is to provide a brewing method for enhancing the woody flavor of liquor, comprising the following steps:

[0011] (1) Mixing nanomaterials, clay and water uniformly, and molding to obtain a wood fragrance regulator; wherein the nanomaterial is Pt-Pb@SiO 2 -Al 2 O 3 、SiO 2 、Al 2 O 3 Two or more of the following;

[0012] (2) Adding a woody aroma regulator during the storage of aged liquor to enhance the woody aroma of the liquor; wherein the amount of the woody aroma regulator added is 1-15% of the weight of the liquor.

[0013] In one embodiment of the present invention, in step (1), the mass ratio of nanomaterial, clay and water is 5-30:100:20-40.

[0014] In one embodiment of the present invention, the nanomaterial in step (1) is Pt-Pb@SiO 2 -Al 2 O 3 、SiO 2 、Al 2 O 3 The mass ratio is 0.5-5:0.5-5:0.5-5.

[0015] In one embodiment of the present invention, the nanomaterial in step (1) is Pt-Pb@SiO 2 -Al 2 O 3 、SiO 2 The mass ratio is 0.5-5:2-6.

[0016] In one embodiment of the present invention, the nanomaterial in step (1) is Pt-Pb@SiO 2 -Al 2 O 3 、Al 2 O 3 The mass ratio is 0.5-5:2-6.

[0017] In one embodiment of the present invention, the particle size of the nanomaterial and clay in step (1) is 0.01-1 mm.

[0018] In one embodiment of the present invention, the modeling in step (1) includes forming and firing; the forming is performed by using a mold, and the shape can be a sheet, a sphere, a regular hexahedron, a cylinder, a cone, a cube, etc.; the firing is performed at 800-1200° C. for 5-10 hours.

[0019] In one embodiment of the present invention, the container used for storing the aged liquor in step (2) is a ceramic jar, a stainless steel tank, or a glass jar.

[0020] In one embodiment of the present invention, step (2) specifically comprises:

[0021] The newly distilled liquor is put into a container, and a woody aroma regulator is added, and the container is stored for aging to obtain woody aroma liquor.

[0022] In one embodiment of the present invention, the liquor in step (2) is one or more of Maotai-flavor liquor, Qing-flavor liquor, and Luzhou-flavor liquor.

[0023] In one embodiment of the present invention, the storage and aging in step (2) is storage and aging at 10-40° C. for more than 2 months.

[0024] In one embodiment of the present invention, step (2) may be assisted by one or more of dissolved oxygen, irradiation, ultrasound, and electromagnetic radiation; wherein, dissolved oxygen is ventilated 1-5 times per month; irradiation is irradiated by one or more of electron beam, ray, and ultraviolet light; the intensity of electron beam irradiation is 0.5-2.5 kGy, and the time is 10-60 days; the intensity of Co-γ ray is 0.5-4 kGy, and the time is 10-60 days; the ultraviolet light wavelength of ultraviolet light irradiation is 340-400 nm, the duration is 5-300 h, and the power is 0.6-5 KW.

[0025] In one embodiment of the present invention, the characteristic flavor substance of wood fragrance in step (2) is one or more of 4-terpineol, 4-methylguaiacol, vanillyl acetone, fenugreek lactone, 5-methylfurfural, furfural, 3-methyl-2,4-nonanedione, 3-methylbutyraldehyde, acetal, 2-methylpropanal, benzaldehyde, nonanal, hexanal, geranylacetone, 4-ethylphenol, phenol, 4-vinylguaiacol, cedar alcohol, ethyl cinnamate, and piperitone.

[0026] In one embodiment of the present invention, in step (1), Pt-Pb@SiO 2 -Al 2 O 3 The preparation method is as follows:

[0027] (1) 150 μL of a mixed solution of aluminum sec-butoxide and sec-butanol (0.01 g of aluminum sec-butoxide dispersed in 150 μL of sec-butanol), 300 μL of tetramethyl orthosilicate, 20 μL of acetic acid, and 10 μL of ethyl acetoacetate were mixed to obtain a mixed solution A;

[0028] (2) Add 5 g of chloroplatinic acid (H 2 PtCl 6 6H 2 O) and 5gPdCl 2 Dissolve in 15 mL of 0.2 mol / L dilute hydrochloric acid aqueous solution to obtain mixed solution B, then mix mixed solution B with mixed solution A at a volume ratio of 1:1, and stir at 25°C (normal temperature) and 500 rpm for 3 h to obtain mixed solution C;

[0029] (3) The mixed solution C was dried under microwave for 30 min and then calcined in a muffle furnace (heated to 550 °C at 2 °C / min and maintained for 5 h) to obtain Pt-Pb@SiO 2 -Al 2 O 3 .

[0030] The second object of the present invention is the woody fragrant liquor brewed by the method described in the present invention.

[0031] The third object of the present invention is the application of the costus-fragrant liquor described in the present invention in the field of liquor processing.

[0032] The fourth object of the present invention is to provide a finished liquor, which is obtained by blending the wood-fragrant liquor described in the present invention.

[0033] [Beneficial Effects]

[0034] (1) The method of the present invention is simple to operate and can significantly enhance the woody flavor intensity of aged liquor in a relatively short period of time.

[0035] (2) The present invention adds a woody aroma regulator in the preparation of the pottery jar, which is beneficial to improving the flavor components of the liquor and greatly improving the woody aroma characteristic substances; in particular, the contents of vanillin, fenugreek lactone, 4-ethylphenol, 4-vinylguaiacol, 3-methyl-2,4-nonanedione, piperitone, etc. are greatly improved. BRIEF DESCRIPTION OF THE DRAWINGS

[0036] Figure 1 This is the GC-MS chromatogram of the liquor prepared in Example 1.

[0037] Figure 2 This is the full two-dimensional chromatogram of the liquor prepared in Example 1. DETAILED DESCRIPTION

[0038] The preferred embodiments of the present invention are described below. It should be understood that the embodiments are for better explaining the present invention and are not used to limit the present invention.

[0039] Test method:

[0040] 1. Determination method of aroma substances

[0041] (1) Detection of furanones:

[0042] ① Liquid-liquid extraction sample pretreatment:

[0043] 20 mL of liquor sample was diluted with saturated saline to an alcohol content of 10% vol, and then the isotope internal standard of fenugreek lactone was added, followed by extraction with 20 mL of dichloromethane as an extractant, and extracted 3 times in total, each time for 5 min; 60 mL of the extracted components were collected, 30 g of anhydrous sodium sulfate was added thereto, and stored at -20°C overnight; 60 mL of the extracted components were then concentrated to 200 μL by nitrogen blowing and waited for injection;

[0044] ②Use gas chromatography-mass spectrometry (GC-MS) to analyze samples in selected ion monitoring mode (SIM);

[0045] The GC conditions are as follows:

[0046] Agilent 7890 gas chromatograph tandem with 5975 mass spectrometer was used;

[0047] The chromatographic column was DB-FFAP (60 m × 0.25 mm × 0.25 μm, Agilent, America);

[0048] Chromatographic column (DB-FFAP) temperature program: initial temperature was 45 °C for 2 min, then increased to 230 °C at 6 °C / min and maintained for 10 min; He (>99.999%) was used as carrier gas at a flow rate of 2 mL / min and the injection port temperature was 230 °C;

[0049] The MS conditions are as follows:

[0050] The sample solvent delay time was 8 min; the EI ionization source, ionization energy was 70 eV, ion source temperature was 230 °C, and the mass spectrometry ion scanning range was 35-350 amu;

[0051] The quantification of fenugreek lactone, furanone HDMF, and ethyl furanone HEMF was performed using the selected ion monitoring (SIM) mode, with characteristic ions at 128 m / z, 128 m / z, and 142 m / z, respectively;

[0052] ③ Standard curve drawing:

[0053] Use chromatographic grade ethanol and ultrapure water to prepare a simulated liquor matrix solution (pH = 3.5, alcohol content 53% vol) for later use;

[0054] Accurately weigh a certain mass of standard furanone compounds (trigonelline lactone, HDMF and ethyl furanone HEMF) and dissolve them in a simulated liquor solution to prepare a series of standard solutions with different concentration gradients; treat the standard solutions according to the sample pretreatment method of step (1), perform instrumental analysis according to step ②, and prepare a standard curve based on the peak area ratio and concentration ratio of the target substance to the internal standard substance as the horizontal and vertical coordinates respectively;

[0055] ④Detection:

[0056] The liquor to be tested is tested according to steps ① and ② to obtain the peak area, which is then substituted into the standard curve of step ③ to obtain the concentration of the substance to be tested.

[0057] (2) Detection of other substances:

[0058] ①Pretreatment of liquor samples:

[0059] The liquor sample was diluted with ultrapure water to an alcohol content of 10% vol, and then 5 mL was added to a 20 mL headspace bottle, followed by 1.5 g NaCl and 2-methylpyrazine-d6, guaiacol-d3, and diisopropyl disulfide as internal standards;

[0060] After the samples were mixed, HS-SPME was performed using a MPS2 (Gerstel, Germany) multifunctional autosampler. The conditions were as follows: the samples were equilibrated at 40°C for 5 minutes, stirred and extracted at 250 rpm for 40 minutes, and the extraction head model was DVB / CAR / PDMS (2 cm, 50 / 30 μm, Supelco, America). After the extraction, desorption was performed at 250°C for 5 minutes.

[0061] ② Determination of compound content in liquor samples by comprehensive two-dimensional gas chromatography:

[0062] Chromatographic conditions: The gas chromatograph was Agilent 7890B (Agilent, America), the first-dimension chromatographic column was a DB-FFAP capillary column (60m×0.25mm×0.25μm, Agilent, America), and the second-dimension chromatographic column was an Rx-17 Si capillary column (0.8m×0.25mm×0.36μm, Restek, America); the first-dimension chromatographic column and the second-dimension chromatographic column were connected in series through a four-nozzle two-stage thermal modulator, and the transmission temperature was 240°C; He (>99.999%) was used as the carrier gas, the flow rate was 1mL / min, and the injection port temperature was 250°C;

[0063] The temperature program of the one-dimensional column is mainly divided into four stages. The starting temperature of the first stage is set to 45℃ and maintained for 3min; the second stage is heated to 150℃ at a heating rate of 4℃ / min and then maintained for 2min; the third stage is heated to 200℃ at a heating rate of 6℃ / min; the last stage is heated to 230℃ at a heating rate of 10℃ / min and then maintained for 10min.

[0064] The total time of the entire analysis process was 53 minutes, and the temperature of the second-dimensional column oven was 5°C higher than that of the first-dimensional column oven throughout the process; the compensation temperature of the modulator was set to 20°C, the modulation cycle of the modulator was 4s, and the thermal pulse time was 0.8s. Mass spectrometry conditions: ion source voltage 70eV, temperature 230°C, transmission line temperature 240°C, ion scanning range 35-400amu, scanning frequency 100spestra / s.

[0065] ③ Standard curve drawing:

[0066] Use chromatographic grade ethanol and ultrapure water to prepare a simulated liquor matrix solution (pH = 3.5, alcohol content 53% vol) for later use;

[0067] Accurately weigh a certain mass of the compound standard and dissolve it in the simulated liquor solution to prepare a series of standard solutions with different concentration gradients. The standard solution is treated according to the above sample pretreatment method and then analyzed by the instrument. The peak area ratio and concentration ratio of the target substance to the internal standard substance are used as the horizontal and vertical coordinates to prepare the standard curve.

[0068] ④Detection:

[0069] The liquor to be tested is tested according to steps ① and ② to obtain the peak area, which is then substituted into the standard curve of step ③ to obtain the concentration of the substance to be tested.

[0070] 2. Test of the characteristic flavor of woody aroma:

[0071] A standard olfactory product with woody characteristics was prepared into a certain concentration and diluted to a certain concentration range. An intensity scale was established, and a unified scale was reached through discussion by the tasting panel. After two weeks of training, a scale test was conducted.

[0072] Evaluators rated the intensity of the woody character on a scale of 0 (none) to 100 (very strong).

[0073] The evaluation team consisted of 40 people (22 women and 18 men, aged 25 to 40) with extensive sensory evaluation experience. All evaluators had previously received more than one year of training in odor attribute description.

[0074] Evaluators scored the sensory characteristics of the liquor samples on three levels: color, aroma, and taste, using a scale of 0 (none) to 100 (very strong).

[0075] The score is calculated by removing the highest value, removing the lowest value, and then taking the average value as the final sensory score.

[0076] The raw materials used in the examples are:

[0077] 1. Pt-Pb@SiO 2 -Al 2 O 3 The preparation method is as follows:

[0078] (1) 150 μL of a mixed solution of aluminum sec-butoxide and sec-butanol (0.01 g of aluminum sec-butoxide dispersed in 150 μL of sec-butanol), 300 μL of tetramethyl orthosilicate, 20 μL of acetic acid, and 10 μL of ethyl acetoacetate were mixed to obtain a mixed solution A;

[0079] (2) Add 5 g of chloroplatinic acid (H 2 PtCl 6 6H 2 O) and 5g PdCl 2 Dissolve in 15 mL of 0.2 mol / L dilute hydrochloric acid aqueous solution to obtain mixed solution B, then mix mixed solution B with mixed solution A at a volume ratio of 1:1, and stir at 25°C (normal temperature) and 500 rpm for 3 h to obtain mixed solution C;

[0080] (3) The mixed solution C was dried under microwave for 30 min and then calcined in a muffle furnace (heated to 550 °C at 2 °C / min and maintained for 5 h) to obtain Pt-Pb@SiO 2 -Al 2 O 3 .

[0081] 2. Pt-Pb@SiO 2 -Al 2 O 3 、SiO 2 、Al 2 O 3 The particle size is 0.2mm.

[0082] 3. Clay: Clay used for preparing pottery jars, without modification or treatment, with a particle size of 0.2 mm.

[0083] 4. Pottery powder and pottery fragments: They come from pottery jars and are the powder obtained by grinding the pottery jars. The particle size is 0.2mm. Pottery fragments are fragments of the pottery jars.

[0084] 5. The sauce-flavor liquor is new liquor that has not been stored and is purchased from Sichuan.

[0085] 6. Ceramic jars, stainless steel tanks, and glass jars: Ceramic jars, stainless steel tanks, and glass jars are commonly used to store liquor.

[0086] Example 1

[0087] A brewing method for enhancing the woody flavor of liquor comprises the following steps:

[0088] (1) 10 g Pt-Pb@SiO 2 -Al 2 O 3 、10g SiO 2 , 10g Al 2 O 3 , 100g of clay and 30g of water were mixed evenly, put into a cube mold (with a side length of 0.4cm) to form, and fired at 1200℃ for 7h to obtain a wood fragrance regulator;

[0089] (2) The newly distilled liquor (sauce-flavor liquor) is placed in a stainless steel tank, and 8% (mass percentage relative to the liquor) of a woody aroma regulator is added, and the tank is stored and aged at 30° C. for 2 months. At the same time, the tank is aerated once a month until the oxygen is saturated, and irradiated (ultraviolet light wavelength 350 nm, power 2 kW, time 20 days) to obtain a woody aroma liquor.

[0090] The obtained woody liquor was subjected to performance tests, and the test results are as follows:

[0091] Table 1 Performance test results of Muxiang liquor

[0092]

[0093]

[0094] Example 2

[0095] In the storage and aging step (2) of Example 1, oxygenation once a month to oxygen saturation was omitted, and the other steps were the same as in Example 1 to obtain Muxiang Baijiu.

[0096] Example 3

[0097] In the storage aging step (2) of Example 1, irradiation (ultraviolet light wavelength 350nm, power 2KW, time 20 days) was omitted, and the rest was consistent with Example 1 to obtain Muxiang Baijiu.

[0098] Example 4

[0099] In the storage and aging of step (2) of Example 1, oxygenation once a month to oxygen saturation and irradiation (ultraviolet light wavelength 350nm, power 2KW, time 20 days) were omitted, and the rest was consistent with Example 1 to obtain Muxiang Baijiu.

[0100] Example 5

[0101] Adjust the "10 g Pt-Pb@SiO 2 -Al 2 O 3 、10g SiO 2 , 10g Al 2 O 3 ” is “10gPt-Pb@SiO 2 -Al 2 O 3 , 5g SiO 2 , 5g Al 2 O 3 ", the rest is consistent with Example 1 to obtain Muxiang Baijiu.

[0102] Example 6

[0103] Adjust the "10 g Pt-Pb@SiO 2 -Al 2 O 3 、10g SiO 2 , 10g Al 2 O 3 ” is “10gPt-Pb@SiO 2 -Al 2 O 3 , 20g SiO 2 ", the rest is consistent with Example 1 to obtain Muxiang Baijiu.

[0104] Example 7

[0105] Adjust the "10 g Pt-Pb@SiO 2 -Al 2 O 3 、10g SiO 2 , 10g Al 2 O 3 ” is “10gFe 2 O 3 @SiO 2 -Al 2 O 3 , 15g Al 2 O 3 ", the rest is consistent with Example 1 to obtain Muxiang Baijiu.

[0106] Example 8

[0107] The amount of the costus aroma regulator in step (2) of Example 1 was adjusted to 5%, and the other contents were kept the same as in Example 1 to obtain costus aroma liquor.

[0108] Example 9

[0109] The amount of the costus aroma regulator in step (2) of Example 1 was adjusted to 12%, and the other contents were kept the same as in Example 1 to obtain costus aroma liquor.

[0110] Example 10

[0111] The "stainless steel tank" in step (1) of Example 1 is adjusted to a "ceramic jar", and the rest is kept consistent with Example 1 to obtain Muxiang Baijiu.

[0112] The obtained woody liquor was subjected to performance tests, and the test results are as follows:

[0113] Table 2 Characteristic substances test of costus root

[0114]

[0115] Table 3 Characteristic substances test of costus root

[0116]

[0117] Table 4 Sensory test results

[0118]

[0119] Comparative Example 1

[0120] The addition of the wood fragrance regulator in step (2) of Example 1 is omitted, and the other steps are kept consistent with Example 1 to obtain white wine.

[0121] Comparative Example 2

[0122] Adjust the "10 g Pt-Pb@SiO 2 -Al 2 O 3 、10g SiO 2 , 10g Al 2 O 3 ” is “30gAl 2 O 3 Nanomaterial (0.2 mm)", the rest is consistent with Example 1 to obtain white wine.

[0123] Comparative Example 3

[0124] Adjust the "10 g Pt-Pb@SiO 2 -Al 2 O 3 、10g SiO 2 , 10g Al 2 O 3” is “30g of Fe with a mass ratio of 5:5:10:10 2 O 3 ,CuO,SiO 2 、Al 2 O 3 A mixture of nanomaterials (0.2 mm) was prepared, and the rest was consistent with Example 1 to obtain white wine.

[0125] Comparative Example 4

[0126] Step (1) of Example 1 is omitted, and the costus aroma regulator in step (2) is adjusted to pottery pieces (50×50 mm). The rest is consistent with Example 1 to obtain white wine.

[0127] Comparative Example 5

[0128] Adjust the "10 g Pt-Pb@SiO 2 -Al 2 O 3 、10g SiO 2 , 10g Al 2 O 3 ” is “30g of pottery powder”, and the rest is consistent with Example 1 to obtain white wine.

[0129] The obtained liquor was subjected to performance test, and the test results are as follows:

[0130] Table 5 Characteristic substances test of costusroot

[0131]

[0132] Table 6 Sensory test results

[0133]

[0134] Although the present invention has been disclosed as above in the form of a preferred embodiment, it is not intended to limit the present invention. Anyone familiar with this technology can make various changes and modifications without departing from the spirit and scope of the present invention. Therefore, the scope of protection of the present invention should be based on the definition of the claims.

Claims

1. A brewing method for enhancing the woody flavor of liquor, characterized in that: The steps include: (1) mixing nanomaterials, clay and water uniformly, and molding to obtain a wood fragrance regulator; wherein the nanomaterials are two or more of Pt-Pb@SiO2-Al2O3, SiO2, and Al2O3; (2) Adding a woody aroma regulator during the storage of aged liquor to enhance the woody aroma of the liquor; wherein the amount of the woody aroma regulator added is 1-15% of the weight of the liquor.

2. The method according to claim 1, characterized in that: In step (1), the mass ratio of the nano material, clay and water is 5-30:100:20-40.

3. The method according to claim 1, characterized in that The mass ratio of Pt-Pb@SiO2-Al2O3, SiO2 and Al2O3 in the nanomaterial of step (1) is 0.5-5:0.5-5:0.5-5.

4. The method according to claim 1, characterized in that The mass ratio of Pt-Pb@SiO2-Al2O3 to SiO2 in the nanomaterial of step (1) is 0.5-5:2-6.

5. The method according to claim 1, characterized in that The mass ratio of Pt-Pb@SiO2-Al2O3 to Al2O3 in the nanomaterial of step (1) is 0.5-5:2-6.

6. The method according to claim 1, characterized in that In step (2), the liquor is one or more of sauce-flavor liquor, light-flavor liquor, and strong-flavor liquor.

7. The method according to claim 1, characterized in that The storage and aging in step (2) is performed at 10-40° C. for more than 2 months.

8. A wood-fragrant liquor prepared by the method according to any one of claims 1 to 7.

9. Use of the costusroot liquor according to claim 8 in the field of liquor processing.

10. A finished liquor, characterized in that: The method is obtained by blending the woody liquor described in claim 8.

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