Method for increasing radix aucklandiae flavor of Baijiu through pottery jar

Abstract

The invention discloses a method for increasing radix aucklandiae flavor of baijiu through a pottery jar, and belongs to the field of baijiu brewing. The method for increasing the flavor of the radix aucklandiae in the white spirit through the pottery jar comprises the following steps: uniformly mixing pottery clay and a radix aucklandiae regulator, and adding mud to prepare a mud cake; forming the mud cake to obtain a pottery jar green body; drying the pottery jar green body; performing high-temperature firing to obtain the pottery jar for increasing the flavor of the radix aucklandiae of the white spirit; wherein the radix aucklandiae conditioning agent is more than two of Pt-Pb-coated SiO2-Al2O3, SiO2 and Al2O3. The pottery jar for increasing the radix aucklandiae flavor of the white spirit, prepared by the preparation method, is stable in aging effect and short in aging period; the radix aucklandiae flavor of the Baijiu can be greatly improved.

Description

Technical Field

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

[0002] Baijiu, as a traditional Chinese distilled liquor, is deeply loved by consumers for its unique taste and aroma. In the production process of baijiu, aging is a key step to improve the quality and flavor of the liquor, and woody flavor, as an important aroma type in baijiu, is of great significance to improving the overall quality and market competitiveness of baijiu.

[0003] In the traditional liquor production process, aging is usually carried out in stainless steel tanks or ceramic jars. Among them, ceramic jars are considered to be one of the best aging containers due to their unique material and structure. The microporous structure of the ceramic jar can promote the moderate exchange of the liquor with the outside world, which is conducive to the aging of the liquor and the formation of its flavor. However, in the prior art, there is still a lack of systematic research and methods on how to increase the woody flavor of liquor through ceramic jar aging.

[0004] Moreover, although pottery jar aging can improve the overall flavor of liquor, the existing technology has the following limitations in increasing the woody flavor:

[0005] (1) The flavor formation mechanism is unclear:

[0006] In the prior art, there is a lack of in-depth research on the formation mechanism of woody flavor during pottery jar aging, which makes it impossible to optimize the aging conditions in a targeted manner to enhance the woody flavor.

[0007] (2) The aging effect is unstable:

[0008] Due to the lack of precise control over the conditions for the formation of woody flavor, the woody flavor of liquor aged in pottery jars has large fluctuations, making it difficult to ensure the consistency of each batch of products.

[0009] (3) Long aging period:

[0010] The traditional ceramic jar aging method has a long cycle, which is not conducive to quickly responding to market demand and limits the flexibility and efficiency of liquor production.

[0011] Therefore, it is urgent to find a method for increasing the woody flavor of liquor through pottery jars, so that the aging effect of the liquor after storage is stable and the woody flavor can be well regulated; and the aging time is short and the efficiency is high. Summary of the invention

[0012] [Technical issues]

[0013] When it comes to increasing the woody flavor, ceramic jars have problems such as unclear flavor formation mechanism, unstable aging effect, and long aging cycle.

[0014] [Technical solution]

[0015] In order to solve the above problems, the present invention provides a method for increasing the woody flavor of liquor through a pottery jar, wherein the method comprises: mixing clay and a woody flavor regulator evenly, adding mud to prepare a mud cake; shaping the mud cake to obtain a pottery jar blank; drying the pottery jar blank; and then firing at a high temperature to obtain a pottery jar with increased woody flavor of liquor; wherein the woody flavor regulator is Pt-Pb@SiO 2 -Al 2 O 3 、SiO 2 、Al 2 O 3 The ceramic jar for increasing the woody flavor of liquor prepared by the present invention has a stable aging effect and a short aging period, and can greatly increase the woody flavor of liquor.

[0016] The first object of the present invention is to provide a method for preparing a pottery jar for increasing the woody flavor of liquor, comprising the following steps:

[0017] The clay and the woody aroma regulator are mixed evenly, and mud is added to prepare a mud cake; the mud cake is molded to obtain a pottery jar blank; the pottery jar blank is dried; and then high-temperature firing is performed to obtain a pottery jar with increased woody aroma flavor of liquor;

[0018] Among them, the wood fragrance regulator is Pt-Pb@SiO 2 -Al 2 O 3 、SiO 2 、Al 2 O 3 Two or more of the above.

[0019] Furthermore, the mass ratio of the wood fragrance regulator, clay and mud is 5-30:100:80-120.

[0020] Furthermore, the wood fragrance regulator is Pt-Pb@SiO 2 -Al 2 O 3 、SiO 2 、Al 2 O 3 A composition; more preferably a Pt-Pb@SiO with a mass ratio of 2:2:1 2 -Al 2 O 3 、SiO 2 、Al 2 O 3 The composition of

[0021] or

[0022] The wood fragrance regulator is Pt-Pb@SiO with a mass ratio of 1-3:1-3 2 -Al 2 O 3 、SiO 2 A composition; more preferably a Pt-Pb@SiO 2 -Al 2 O 3 、SiO 2 The composition of

[0023] or

[0024] The wood fragrance regulator is Pt-Pb@SiO with a mass ratio of 1-3:1-3 2 -Al 2 O 3 、Al 2 O 3 A composition; more preferably a Pt-Pb@SiO 2 -Al 2 O 3 、Al 2 O 3 composition.

[0025] Furthermore, the particle size of the wood fragrance regulator and the clay is 0.01-1 mm.

[0026] Furthermore, the mud is a water solution of armor mud, the particle size of the armor mud is 50-60 meshes, and the water content is 15-25% (mass percentage); the armor mud is weathered armor mud.

[0027] Furthermore, the forming is performed by an integrated roller forming device to form a ceramic jar blank.

[0028] Furthermore, the drying is performed so that the moisture content of the green body is less than 2% (mass percentage).

[0029] Furthermore, high temperature firing is firing at 800-1200°C to form a pottery jar.

[0030] Furthermore, Pt-Pb@SiO 2 -Al 2 O 3 The preparation method is as follows:

[0031] (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;

[0032] (2) Add 5 g of chloroplatinic acid (H 2 PtCl6 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;

[0033] (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 .

[0034] The second object of the present invention is a pottery jar with increased woody flavor of liquor prepared by the method of the present invention.

[0035] The third object of the present invention is to use the pottery jar for increasing the woody flavor of liquor in the field of liquor processing.

[0036] The fourth object of the present invention is to provide a method for regulating the woody flavor in liquor, which uses the pottery jar for increasing the woody flavor of liquor described in the present invention.

[0037] Furthermore, the method for regulating the woody flavor in liquor comprises the following steps:

[0038] The newly distilled liquor is put into a ceramic jar to increase the woody flavor of the liquor, and stored and aged at room temperature to obtain a liquor with a woody flavor.

[0039] Furthermore, the liquor is one or more of the following: sauce-flavor liquor, light-flavor liquor, and strong-flavor liquor.

[0040] Furthermore, the storage aging is storage aging at 10-40° C. for more than 2 months.

[0041] Furthermore, one or more of dissolved oxygen, irradiation, ultrasound, and electromagnetic radiation can be used as auxiliary. Among them, dissolved oxygen is 1-5 times a month. Irradiation is one or more of electron beam, ray, and ultraviolet light. The intensity of electron beam irradiation is 0.5-2.5kGy, and the time is 10-60 days. The intensity of Co-γ ray is 0.5-4kGy, and the time is 10-60 days. The wavelength of ultraviolet light in ultraviolet irradiation is 340-400nm, the duration is 5-300h, and the power is 0.6-5KW.

[0042] Furthermore, the characteristic flavor substances of woody fragrance are one or more of 4-pineol, 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.

[0043] The fifth objective of the present invention is the woody flavor liquor prepared by the method of the present invention.

[0044] The sixth object of the present invention is to provide a finished liquor, which is obtained by blending the woody flavor liquor described in the present invention.

[0045] [Beneficial Effects]

[0046] (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.

[0047] (2) The ceramic jar for increasing the woody flavor of liquor prepared by the present invention is beneficial to improving the flavor components of liquor, and greatly improves the characteristic substances of woody flavor; in particular, the contents of vanillin, fenugreek lactone, 4-ethylphenol, 4-vinylguaiacol, piperitone, and 3-methyl-2,4-nonanedione are greatly improved. BRIEF DESCRIPTION OF THE DRAWINGS

[0048] Figure 1 This is a comprehensive two-dimensional gas chromatogram of the liquor prepared in Example 1. DETAILED DESCRIPTION

[0049] 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.

[0050] Test method:

[0051] 1. Determination method of aroma substances

[0052] (1) Detection of Furanone Substances:

[0053] ① Liquid-liquid extraction sample pretreatment:

[0054] 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;

[0055] ②Use gas chromatography-mass spectrometry (GC-MS) to analyze samples in selected ion monitoring mode (SIM);

[0056] The GC conditions are as follows:

[0057] Agilent 7890 gas chromatograph tandem with 5975 mass spectrometer was used;

[0058] The chromatographic column was DB-FFAP (60 m × 0.25 mm × 0.25 μm, Agilent, America);

[0059] 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;

[0060] The MS conditions are as follows:

[0061] 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;

[0062] 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;

[0063] ③ Standard curve drawing:

[0064] A simulated liquor matrix solution (pH=3.5, alcohol content 53% vol) was prepared with chromatographic grade ethanol and ultrapure water for later use; a certain amount of furanone compound standard (trigonelline lactone, HDMF and ethyl furanone HEMF) was accurately weighed and dissolved in the simulated liquor solution to prepare a series of standard solutions with different concentration gradients;

[0065] The standard solution is treated according to the sample pretreatment method of step (1), and the instrument analysis is performed according to step ②. The standard curve is prepared according to the peak area ratio and concentration ratio of the target substance and the internal standard substance as the horizontal and vertical coordinates respectively;

[0066] ④Detection:

[0067] 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.

[0068] (2) Detection of other substances:

[0069] ①Pretreatment of liquor samples:

[0070] Dilute the liquor sample with ultrapure water to an alcohol content of 10% vol, then take 5 mL and add it to a 20 mL headspace bottle, then add 1.5 g NaCl and 2-methylpyrazine-d6, guaiacol-d3, and diisopropyl disulfide as internal standards;

[0071] 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.

[0072] ② Determination of compound content in liquor samples by comprehensive two-dimensional gas chromatography:

[0073] Chromatographic conditions:

[0074] 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;

[0075] 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.

[0076] 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 4 seconds, and the heat pulse time was 0.8 seconds.

[0077] Mass spectrometry conditions:

[0078] The ion source voltage was 70 eV, the temperature was 230 °C, the transfer line temperature was 240 °C, the ion scanning range was 35-400 amu, and the scanning frequency was 100 spestra / s.

[0079] ③ Standard curve drawing:

[0080] Use chromatographic grade ethanol and ultrapure water to prepare a simulated liquor matrix solution (pH = 3.5, alcohol content 53% vol) for later use;

[0081] 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.

[0082] The standard solution was treated according to the above sample pretreatment method and then subjected to instrumental analysis. The peak area ratio and concentration ratio of the target substance to the internal standard substance were used as the horizontal and vertical coordinates to prepare the standard curve.

[0083] ④Detection:

[0084] 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.

[0085] 2. Test of the characteristic flavor of woody aroma:

[0086] 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.

[0087] The evaluators rated the intensity of the woody aroma on a scale of 0 (none) to 100 (very strong). The evaluation panel 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 the description of odor attributes.

[0088] 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).

[0089] The score is calculated by removing the highest value, removing the lowest value, and then taking the average value as the final sensory score.

[0090] The raw materials used in the examples are:

[0091] 1. Pt-Pb@SiO 2 -Al 2 O 3 The preparation method is as follows:

[0092] (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;

[0093] (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;

[0094] (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 .

[0095] 2. Pt-Pb@SiO 2 -Al 2 O 3 、SiO 2 、Al 2 O 3 The particle size is 0.2mm.

[0096] 3. Clay: Clay used for preparing pottery jars, without modification or treatment, with a particle size of 0.2 mm.

[0097] 4. Pottery powder: It comes from the pottery jar, which is the powder obtained by grinding the pottery jar, with a particle size of 0.2mm.

[0098] 5. The sauce-flavor liquor, light-flavor liquor, and strong-flavor liquor are new liquors that have not been stored and are purchased from Sichuan.

[0099] 6. Mud: A mud aqueous solution, the particle size of A mud is 50 mesh, and the water content is 20% (mass percentage); A mud is weathered A mud.

[0100] Example 1

[0101] A method for preparing a pottery jar for increasing the woody flavor of liquor comprises the following steps:

[0102] Mix the clay and wood fragrance regulator evenly, add mud to prepare mud cake;

[0103] The mud cake is formed by an integrated roller pressing device to obtain a pottery jar blank;

[0104] The ceramic jar body is dried to make the moisture content of the body less than 2%; and then fired at 1000°C for 72 hours to obtain a ceramic jar with increased woody flavor of liquor;

[0105] Among them, the wood fragrance regulator is Pt-Pb@SiO with a mass ratio of 2:2:1 2 -Al 2 O 3 、SiO 2 、Al 2 O 3 The composition of

[0106] The mass ratio of wood fragrance regulator, clay and mud is 20:100:100.

[0107] Example 2

[0108] The wood fragrance regulator in Example 1 was adjusted to Pt-Pb@SiO with a mass ratio of 2:1. 2 -Al 2 O 3 、SiO 2 The composition is the same as in Example 1 to obtain a pottery jar.

[0109] Example 3

[0110] The wood fragrance regulator in Example 1 was adjusted to Pt-Pb@SiO with a mass ratio of 2:1. 2 -Al 2 O 3 、Al 2 O 3 The composition is the same as in Example 1 to obtain a pottery jar.

[0111] Example 4

[0112] The wood fragrance regulator in Example 1 was adjusted to Pt-Pb@SiO with a mass ratio of 1:1. 2 -Al 2 O 3 、SiO 2 The composition is the same as in Example 1, and a pottery jar is obtained.

[0113] Example 5

[0114] The wood fragrance regulator in Example 1 was adjusted to Pt-Pb@SiO with a mass ratio of 1:1. 2 -Al 2 O 3 、Al 2 O 3 The composition is the same as in Example 1 to obtain a pottery jar.

[0115] Comparative Example 1

[0116] Adjust the wood fragrance regulator in Example 1 to Pt-Pb@SiO 2 -Al 2 O 3 , the rest are the same as in Example 1 to obtain a pottery jar.

[0117] Comparative Example 2

[0118] Adjust the costus root modifier in Example 1 to SiO 2 , the rest are the same as in Example 1 to obtain a pottery jar.

[0119] Comparative Example 3

[0120] Adjust the costus root regulator in Example 1 to Al 2 O 3 , the rest are the same as in Example 1 to obtain a pottery jar.

[0121] Comparative Example 4

[0122] The costus root regulator in Example 1 is adjusted to pottery powder, and the rest is kept consistent with Example 1 to obtain a pottery jar.

[0123] Comparative Example 5

[0124] The costus root regulator in Example 1 was omitted, and the other parts were kept the same as in Example 1 to obtain a pottery jar.

[0125] Example 6

[0126] A method for regulating woody flavor in liquor comprises the following steps:

[0127] The newly distilled liquor (sauce-flavor liquor) was put into the pottery jars of the embodiment and the comparative example, and stored for aging at 30° C. for 2 months, and oxygenated once a month until the liquor was saturated with oxygen, to obtain a liquor with a woody flavor.

[0128] The obtained liquor was subjected to performance test, and the test results are as follows:

[0129] Table 1 Performance test results of Muxiang liquor

[0130]

[0131] Table 2 Characteristic substances test of costus root

[0132]

[0133] Table 3 Sensory test results

[0134]

[0135] Table 4 Characteristic substances test of costusroot

[0136]

[0137] Table 5 Sensory test results

[0138]

[0139] Example 7

[0140] A method for regulating woody flavor in liquor comprises the following steps:

[0141] The newly distilled Maotai-flavor liquor, Qing-flavor liquor, and Luzhou-flavor liquor were put into the pottery jar prepared in Example 1, and stored and aged at room temperature (25° C.) for 3 months to obtain liquor.

[0142] The obtained liquor was subjected to performance test, and the test results are as follows:

[0143] Table 6 Characteristic substances test of costusroot

[0144]

[0145] Table 7 Sensory test results

[0146]

[0147] 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 method for preparing a pottery jar for increasing the woody flavor of liquor, characterized in that: The steps include: Mix the clay and wood fragrance regulator evenly, add mud to prepare mud cake; The mud cake is formed into a pottery jar body; The ceramic jar body is dried and then fired at high temperature to obtain a ceramic jar with woody flavor of liquor; Among them, the wood fragrance regulator is two or more of Pt-Pb@SiO2-Al2O3, SiO2, and Al2O3.

2. The method according to claim 1, characterized in that: The mass ratio of wood fragrance regulator, clay and mud is 5-30:100:80-120.

3. The method according to claim 1, characterized in that The wood fragrance regulator is a composition of Pt-Pb@SiO2-Al2O3, SiO2, and Al2O3 in a mass ratio of 1-3:1-3:1-3; more preferably, it is a composition of Pt-Pb@SiO2-Al2O3, SiO2, and Al2O3 in a mass ratio of 2:2:1; or The wood fragrance regulator is a composition of Pt-Pb@SiO2-Al2O3 and SiO2 in a mass ratio of 1-3:1-3; more preferably, it is a composition of Pt-Pb@SiO2-Al2O3 and SiO2 in a mass ratio of 2:1; or The wood fragrance regulator is a composition of Pt-Pb@SiO2-Al2O3 and Al2O3 in a mass ratio of 1-3:1-3; more preferably, it is a composition of Pt-Pb@SiO2-Al2O3 and Al2O3 in a mass ratio of 2:

1.

4. A ceramic jar for increasing the woody flavor of liquor prepared by the method described in any one of claims 1 to 3.

5. Application of the pottery jar for increasing the woody flavor of liquor as claimed in claim 4 in the field of liquor processing.

6. A method for regulating woody flavor in liquor, characterized in that: It adopts the pottery jar for increasing the woody flavor of liquor as described in claim 4.

7. The method according to claim 6, characterized in that The method for regulating the woody flavor in liquor comprises the following steps: The newly distilled liquor is put into a pottery jar to increase the woody flavor of the liquor, and stored at room temperature to mature, thereby obtaining a liquor with a woody flavor.

8. The method according to claim 7, characterized in that The liquor is one or more of the following: sauce-flavor liquor, light-flavor liquor, and strong-flavor liquor.

9. The woody-flavored liquor prepared by the method according to any one of claims 6 to 8.

10. A finished liquor, characterized in that: The liquor is obtained by blending with the woody-flavor liquor described in claim 9.

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