High-stability white spirit and preparation method thereof
By adjusting the myristic acid content and alcohol content in baijiu, and combining distillation, electrodialysis, and preparative chromatography techniques, the problems of flavor and taste differences and unstable hops during baijiu storage have been solved, thus achieving stability and harmony in baijiu quality.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- QINGHAI SPRING MEDICINAL RESOURCES TECH CO LTD
- Filing Date
- 2026-01-15
- Publication Date
- 2026-04-14
AI Technical Summary
Existing baijiu exhibits significant differences in flavor and taste during storage, and the foam is unstable, leading to inconsistent product quality. Blending techniques are insufficient to completely resolve these differences.
By adjusting the myristic acid content in baijiu to 5-150 ppm and the alcohol content to 25-78% vol, and combining distillation, electrodialysis and preparative chromatography techniques, the stability of hops and flavor compounds in baijiu are precisely controlled, using pure natural raw materials and simple blending methods.
It achieves the stability of baijiu hops and the maximum stability of flavor substances, resulting in a unified and harmonious aroma and taste, maintaining the high-quality characteristics of the original liquor, and the preparation method is simple, safe and non-toxic.
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Abstract
Description
Technical Field
[0001] This invention belongs to the field of liquor brewing technology, specifically relating to a highly stable liquor and its preparation method. Background Technology
[0002] Baijiu refers to an alcoholic beverage made primarily from grains, using daqu, xiaoqu, or bran koji and yeast as saccharification and fermentation agents, through processes of cooking, saccharification, fermentation, and distillation. Throughout China's long history of winemaking, the varieties and flavors of baijiu have developed into distinct types and aromas depending on the region. Regardless of the aroma type, traditional baijiu undergoes varying degrees of change during storage, with most becoming smoother and more full-bodied over time.
[0003] The foam in baijiu (Chinese white liquor) is closely related to its quality. It's a layer of foam that forms on the surface of the liquor when it's vigorously shaken in the container or during distillation. By observing the size, dissipation rate, and particle state of the foam, one can infer the alcohol content and quality of the liquor. This method was historically used by distillers to select the best quality baijiu. Generally, high-quality baijiu has foam that is uniform in size, fine, and relatively stable in shape, not easily breaking off and disappearing immediately. Conversely, if the foam is uneven in size and unstable in shape, it indirectly indicates a problem with the quality of the baijiu.
[0004] The differences in flavor and taste resulting from the storage time of baijiu, as well as the instability of the foam, can lead to significant variations between different batches of finished baijiu produced at different times. Even blending techniques cannot completely eliminate this difference. This is a common problem and challenge faced by most baijiu companies. Summary of the Invention
[0005] To address the technical problems of significant flavor and taste variations and unstable foaming in existing batches of produced baijiu, making it difficult to maintain consistent flavor and taste, this invention provides a highly stable baijiu and its preparation method. The baijiu obtained through this method not only increases the stability of the foaming process during storage but also greatly stabilizes the flavor compounds, achieving a unified and harmonious aroma and taste without compromising the quality of the original spirit.
[0006] To solve the above-mentioned technical problems, the technical solution adopted in this application is as follows: In a first aspect, the present invention provides a highly stable spirit with a myristic acid content of 5-150 ppm and an alcohol content of 25-78% vol.
[0007] The myristic acid content in the liquor is 50-150 ppm.
[0008] The myristic acid content in the liquor is 40-80 ppm.
[0009] The alcohol content of the liquor is 39-53% vol.
[0010] The baijiu mentioned above refers to a distilled spirit made primarily from grains, using daqu, xiaoqu, bran koji, enzyme preparations, and yeast as saccharification and fermentation agents, and produced through processes such as cooking, saccharification, fermentation, distillation, aging, and blending.
[0011] The aroma type of the liquor is at least one of the following: soy sauce aroma, strong aroma, light aroma, phoenix aroma, rice aroma, soy sauce aroma, mixed aroma, sesame aroma, special aroma, old-fashioned liquor aroma, rich aroma, Dong aroma, or other aroma types.
[0012] The liquor, according to its production process, is at least one of solid-state fermented liquor, liquid-state fermented liquor, or solid-liquid fermented liquor.
[0013] The baijiu, according to the saccharification and fermentation agent, is at least one of daqu baijiu, xiaoqu baijiu, bran qu baijiu, or mixed qu baijiu.
[0014] Secondly, the present invention provides a method for preparing the above-mentioned high-stability liquor, wherein the myristic acid content in the liquor is adjusted to 5-150 ppm.
[0015] Furthermore, the alcohol content of the liquor is adjusted to 25-78% vol.
[0016] Furthermore, the method includes the following steps: first enriching and concentrating the myristic acid content in traditional baijiu or baijiu mash to 1-2% (W / V) and the alcohol content to 70-80% vol, then further concentrating it to over 90% through preparative chromatography or distillation, and finally obtaining it through blending.
[0017] The traditional baijiu is obtained by conventional solid-state distillation before the baijiu mash is enriched and concentrated.
[0018] The enrichment and concentration process refers to directly subjecting traditional baijiu to at least one of the following operations: membrane filtration, distillation, or electrodialysis.
[0019] Specifically, the method includes the following steps: S1. Traditional Baijiu is obtained by conventional solid-state distillation of Baijiu mash, or traditional Baijiu is directly concentrated by vacuum distillation, followed by electrodialysis until the solution pH ≥ 5. The vacuum distillation and / or electrodialysis operations are repeated until the tetradecanoic acid content is 1~2% (W / V) and the alcohol content is 70~80% vol. Then, flavoring wine with a tetradecanoic acid content of more than 90% is obtained by preparative chromatography or distillation. S2. Simply blend the flavoring wine from step S1 with traditional white wine to obtain the final product.
[0020] In step S1, the vacuum distillation concentration is achieved by at least one of the following methods: permeate membrane evaporation, thin-film rotary evaporation, or distillation.
[0021] Preferably, the evaporation and dehydration pressure of the permeation membrane is ≤500Pa, and the heating temperature is <50℃.
[0022] Preferably, the vacuum pressure of the thin-film rotary evaporation is ≤5000Pa and the heating temperature is <80℃.
[0023] In step S1, during the preparative chromatography, 85% ethanol is used as the eluting agent, and the fraction with a retention time RT between 18.0 and 19.5 min is collected.
[0024] The electrodialysis voltage is 1~15V and the current is 0.05~2A.
[0025] Beneficial Effects: This invention adjusts the myristic acid content in traditional baijiu to 5-150 ppm and the alcohol content to 25-78% vol, thereby making the changes in hops and flavor compounds during baijiu storage more stable, resulting in a higher-quality baijiu with a more pleasant flavor and taste. The high-stability baijiu of this invention is achieved through the following method: enrichment and concentration of myristic acid from traditional baijiu or baijiu mash, followed by simple blending to adjust the myristic acid content to 5-150 ppm and the alcohol content to 25-78% vol. This method greatly stabilizes the flavor compounds in the baijiu while also increasing the stability of the hops, resulting in a unified and harmonious aroma and flavor without compromising the advantages of the original spirit. Furthermore, the preparation method of this invention is simple, using all-natural, safe, and non-toxic raw materials, and can be widely applied in the baijiu production field. Detailed Implementation
[0026] To make the technical problems, solutions, and beneficial effects of this application clearer, the following detailed description is provided in conjunction with the embodiments. Unless otherwise defined, all technical terms used herein have the same meaning as understood by one of ordinary skill in the art.
[0027] Terminology definition: Unless otherwise defined herein, all technical and scientific terms used herein are intended to have the same meaning as commonly understood by one of ordinary skill in the art. The terms “comprising,” “including,” “having,” “containing,” or “involving,” and their other variations herein, are inclusive or open-ended and do not exclude other unlisted elements or method steps. One of one’s skill in the art will understand that the foregoing term “comprising” covers the meaning of “consisting of.”
[0028] In this invention, the terms "a," "an," "at least one," and "one or more" are used interchangeably. When a lower and upper limit of a numerical range is disclosed, any numerical value falling within that range and any included range are specifically disclosed. In particular, each range of values disclosed herein (in the form of "about a to b," or equivalently, "approximately a to b," or equivalently, "about ab") should be understood to represent each numerical value and range encompassed within a wider range.
[0029] In this invention, unless otherwise stated, the tetradecanoic acid described herein is also known as myristic acid, a long-chain saturated fatty acid with the molecular formula C1. 14 H 28 O2, with a molecular weight of 228.37 and CAS number 544-63-8, is typically present in traditional baijiu (Chinese liquor) at a concentration not exceeding 2 ppm.
[0030] In this invention, unless otherwise stated, the dodecanoic acid described herein is also known as lauric acid, with the molecular formula C1. 12 H 24 O2, with a molecular weight of 200.36 and CAS number 143-07-7.
[0031] In this invention, unless otherwise stated, the tridecanoic acid described herein is also an aliphatic carboxylic acid with a carbon number between that of dodecanoic acid (lauric acid) and tetradecanoic acid (myristic acid), and its molecular formula is C64-32 ... 13 H 26 O2, with a molecular weight of 214.35 and CAS number 638-53-9.
[0032] In this invention, unless otherwise stated, the pentadecanoic acid described herein has the molecular formula C5. 15 H 30 O2, with a molecular weight of 242.40 and CAS number 1002-84-2.
[0033] In this invention, unless otherwise stated, the hexadecanoic acid described herein is also known as palmitic acid or palmitic acid, and its molecular formula is C6H2O. 16 H 32 O2, with a molecular weight of 256.42 and CAS number 57-10-3.
[0034] In this invention, unless otherwise stated, the heptadecanoic acid described herein is also known as pearlitic acid, with the molecular formula Ch. 17 H 34 O2, with a molecular weight of 270.45 and CAS number 506-12-7.
[0035] In this invention, unless otherwise stated, the octadecanoic acid described herein is also called stearic acid, with the molecular formula C1. 18 H36 O2, with a molecular weight of 284.48 and CAS number 57-11-4.
[0036] The formation of baijiu (Chinese white liquor) bubbles is mainly due to the surface tension difference between alcohol and water, as well as the combined effects of trace components in the liquor, such as esters. According to existing literature, specifically, the formation of baijiu bubbles is related to the following factors: Alcohol content: The alcohol content directly affects the size of the hops. Generally speaking, the higher the alcohol content, the greater the surface tension of the liquid, and the larger the hops formed.
[0037] Temperature: Temperature has a significant effect on the surface tension of alcohol solutions. At lower temperatures, hops are relatively smaller but more persistent; while at higher temperatures, hops are relatively larger but shorter-lasting.
[0038] Age of the wine: The age of the wine also affects the formation of bubbles. For wines with the same alcohol content, the shorter the age, the larger the bubbles will be, but they will also dissipate faster and be more unevenly distributed.
[0039] Trace components: Flavor substances and trace components in liquor also have a certain impact on hops. If these components are abundant and complex in baijiu, the hops formed will be more numerous and more aesthetically pleasing. For example, esters in baijiu will polymerize at low temperatures to form dense foam, which is also a form of hop formation. Although hop formation is related to trace components, no literature or related reports have yet identified which type or specific trace component is responsible. Practice has also shown that a higher abundance or level of trace components does not necessarily result in better hop formation and foam accumulation.
[0040] In conclusion, the formation of hops in baijiu is a complex process influenced by multiple factors, and there is currently no clear mechanism.
[0041] Although baijiu (Chinese white liquor) is rich in trace components, their content is low, ranging from 1% to 2%. Existing literature reports (Zhou Qin et al., A review of the formation mechanism, influencing factors and characteristics of foam in beer and sparkling wine [J], Food Industry, 2022, Vol. 43, No. 7: 241-246) that the components that can increase foam in alcoholic beverages are all large molecular weight proteins and polysaccharides, such as in beer. However, baijiu is a distilled spirit, and its content of large molecular weight substances is extremely low, generally less than 1 ppm, which is insufficient to change the stability of hops. Although there are literature reports (Liu Jiangsheng et al., Discussion on Hops and Wine [J], Brewing, Vol. 41, No. 3, 2013: 36-41) that the formation of hops in baijiu is related to trace components and is the result of the combined action of various components, compared with fermented wines such as beer, the trace components in baijiu are affected by brewing technology, storage environment and various microorganisms. The trace components are constantly changing over time and there are many kinds. The conclusions reported in the existing literature are too general and are only inferences. At present, there are no reports or inventions of specific components or substances that can play a role in the stability of baijiu hops.
[0042] The applicant used common-aroma baijiu, such as sauce-aroma or strong-aroma baijiu, as a base to study the effects of common trace components in baijiu on the hops (or foaming) of baijiu. The content of these components in baijiu is mostly above 1 ppm. Trace components include: Alcohols: n-propanol, sec-butanol, isobutanol, n-butanol, isoamyl alcohol, n-pentanol, n-hexanol, 1,2-propanediol, 1,3-propanediol, β-phenylethanol, n-heptanol, n-octanol, benzyl alcohol, 2-heptanol, ethylene glycol, 2-hexanol, 2,3-butanediol, furfuryl alcohol, isooctanol, n-nonanol, 3-octanol, sec-pentanol, sec-octanol; the content of most alcohol components in baijiu does not exceed 500 ppm.
[0043] Esters: ethyl formate, ethyl acetate, ethyl lactate, ethyl propionate, ethyl butyrate, ethyl isobutyrate, ethyl valerate, ethyl isovalerate, ethyl hexanoate, ethyl heptanoate, ethyl octanoate, ethyl nonanoate, ethyl decanoate, n-propyl acetate, isobutyl acetate, isoamyl acetate, ethyl 3-methylbutyrate, diethyl succinate, propyl hexanoate, butyl acetate, ethyl undecanoate, ethyl laurate, ethyl tetradecanoate, ethyl pentadecanoate, ethyl palmitate, ethyl oleate, ethyl linoleate, ethyl phenylacetate; the content of most ester components in baijiu does not exceed 2500 ppm.
[0044] Acids: Acetic acid, lactic acid, propionic acid, butyric acid, isobutyric acid, valeric acid, isovaleric acid, hexanoic acid, heptanoic acid, octanoic acid, nonanoic acid, decanoic acid, undecanoic acid, dodecaic acid (lauric acid), tridecanoic acid, tetradecanoic acid (myristic acid), pentadecanoic acid, hexadecanoic acid (palmitic acid, palmitic acid), heptadecaic acid (pearlitic acid), oleic acid, linoleic acid, stearic acid (stearic acid), 2-furoic acid, maleic acid, succinic acid, 2-hydroxybutyric acid, azelaic acid, 2-hydroxyisovaleric acid, L-phenyllactic acid, benzoic acid; the content of most acid components in baijiu does not exceed 2000 ppm.
[0045] Ketones: 2-Pentanone, acetophenone, 2-nonanone, 2-heptanone, cyclopentanone, 2-hexanone, 2,3-butanedione (diacetyl), 2-octanone, 3-octanone, 2,3-pentanedione; the content of most ketone components in baijiu does not exceed 20 ppm.
[0046] Aldehydes: acetaldehyde, isobutyraldehyde, acetal, isovaleraldehyde, furfural. The content of most aldehyde components in baijiu does not exceed 1500 ppm.
[0047] The applicant dissolved the aforementioned trace components separately in 70-80 proof liquor to prepare a 1-10% concentration of baijiu mother liquor, or added it undiluted to base liquors of soy sauce aroma or strong aroma based on the flavor threshold of different flavor substances (flavor threshold refers to the lowest concentration of aroma and flavor substances that can be detected by sensory perception. The lower the threshold, the more sensitive the human body is to the taste or smell of the substance, and the greater its aroma and flavor effect). The selection criteria are that it promotes the flavor of different base liquors, does not affect the harmony of the liquor, and at the same time increases the fermentation and setting time of baijiu.
[0048] The screening experiments revealed that alcohols and esters in baijiu, regardless of their concentration or content, all have varying degrees of defoaming effects, especially large-molecule fatty acid esters such as ethyl heptanoate and higher-chain fatty acid esters, which make it difficult for the liquor to foam. Aldehydes and ketones, without affecting the flavor of the liquor, both reduce the persistence of the foam; however, 2,3-butanedione, furfural, and acetal have relatively smaller effects on foam persistence.
[0049] In the experiment on the effects of organic acids on the flavor of liquor, short-chain and medium-chain fatty acids, due to their low threshold, all affected the overall flavor of baijiu. In small amounts, they had varying degrees of defoaming effects or no effect at all. Among fatty acids with a dodecyl or higher concentration, it was discovered that only tetradecyl acid, at a certain concentration, could increase the foaming and settling time of baijiu, while also promoting the flavor of different types of baijiu. Other organic acids all had varying degrees of defoaming effects. Therefore, tetradecyl acid in baijiu plays a positive role in the stability of the foam and the stability of the flavor in baijiu. This is something that has not been discovered or reported in existing baijiu technology and is the main innovation of this invention.
[0050] Therefore, in one embodiment of the present invention, a highly stable spirit is first provided, which has a myristic acid content of 5-150 ppm and an alcohol content of 25-78% vol.
[0051] The myristic acid content mentioned is the content value detected immediately after the liquor is freshly prepared.
[0052] In addition, the foam that forms when baijiu is poured into a glass has been studied and reported to have a significant impact on the quality of baijiu. By observing the duration, aroma and taste of the foam, one can, to some extent, judge the quality information of baijiu, such as its flavor and alcohol content.
[0053] Duration of foam: The duration of foam can reflect the quality of baijiu. High-quality baijiu usually has dense and persistent foam, while inferior or blended baijiu usually has less foam that dissipates easily.
[0054] Aroma and taste: The aromatic components in baijiu are released as the bubbles disperse, so the aroma and taste of the bubbles can be used to make a preliminary judgment on the aroma type and quality of baijiu. For example, light aroma baijiu has a fresh bubble aroma, while strong aroma baijiu has a rich bubble aroma.
[0055] Therefore, good hop content can make baijiu (Chinese white liquor) more fragrant and mellow, increase its complexity and taste, and improve its overall quality. Furthermore, a good hop content helps promote the aging process of baijiu, enhancing its aged flavor and making it smoother and more mellow. Thus, the stability of hops can reflect the overall quality of baijiu; more stable hops indicate better quality.
[0056] Although screening experiments have shown that a certain concentration of tetradecanoic acid has a positive impact on the stability of hops in baijiu, controlling the concentration of tetradecanoic acid during the baijiu brewing process is quite difficult. The main difficulty lies in the complexity of its formation and control, which involves multiple brewing stages and factors.
[0057] First, tetradecanoic acid is not a regular or dominant acid in baijiu brewing; its formation can be influenced by various factors such as specific microbial activity, fermentation conditions, and raw material composition. Precisely controlling the amount of tetradecanoic acid produced during the brewing process requires a deep understanding and precise regulation of these factors, which is a major challenge in controlling tetradecanoic acid production.
[0058] Specifically, the difficulties include the following aspects: The complexity of microbial activity: The microbial community in the baijiu brewing process is diverse and complex, with different microorganisms having different requirements and responses to brewing conditions. Identifying and controlling the activity of specific microorganisms that produce myristic acid requires in-depth microbiological research and advanced brewing techniques.
[0059] Precise control of fermentation conditions: Temperature, pH, oxygen content and other conditions during fermentation will affect the metabolism of microorganisms. Precise control of microbial metabolism is a major challenge in the brewing process.
[0060] The influence of raw material composition: The raw material composition of baijiu also affects the formation of acids. For example, the fat content, types and amounts of fatty acids in the raw materials will affect the formation of acids during the brewing process. To control the formation of tetradecanoic acid, a deep understanding and precise control of the raw material composition are required.
[0061] Distillation and tail-cutting operations: During the distillation process, it is necessary to precisely control the heat and tail-cutting time to avoid other high-boiling-point substances affecting the quality of the liquor.
[0062] Concentration technology: Although concentration technology is becoming increasingly mature, it is necessary to consider the negative impact of other components in baijiu on the quality of the baijiu when it is applied. For example, if the content of dodecanoic acid is too high, it will affect the taste of the baijiu and produce a soapy taste, while if the content of hexadecanoic acid is too high, it will lead to the suppression of aroma and a dull taste. Therefore, precise control is needed during the concentration process to concentrate the hexadecanoic acid.
[0063] In summary, the main challenge in controlling tetradecanoic acid during baijiu brewing lies in the complexity of its formation and control, involving multiple aspects such as microbial activity, fermentation conditions, raw material components, distillation operations, and concentration techniques. Overcoming these challenges requires in-depth brewing techniques, microbiological research, and high-precision concentration technology. While other processes besides concentration are controllable, the results from their control are not as significant as those from concentration. For example, the raw materials and solid-state fermentation processes in traditional baijiu production are not significantly different, and it is difficult to precisely control the tetradecanoic acid content.
[0064] Therefore, in another embodiment of the present invention, a method for preparing high-stability baijiu is provided, comprising the following steps: first enriching and concentrating the myristic acid content in traditional baijiu or baijiu mash to 1-2% (W / V) and the alcohol content to 70-80% vol, then further concentrating it to more than 90% by preparative chromatography or distillation, and finally obtaining it by blending.
[0065] In the enrichment and concentration process of this invention, vacuum distillation is performed first, followed by electrodialysis, in order to remove other ionizable H+ ions. + Organic acids (such as acetic acid, lactic acid, etc.) are removed; then, other acidic impurities such as dodecanoic acid or hexadecanoic acid are removed by preparative chromatography.
[0066] The purpose of preparative chromatography is to obtain higher purity tetradecanoic acid, in order to avoid the defoaming effect of impurities such as dodecanoic acid and hexadecanoic acid, which would affect the stability of the liquor. This is because tetradecanoic acid can only be completely dissolved at an alcohol content of 70% vol or higher when its content is 1-2%, and only completely dissolved samples can be effectively separated during preparative chromatography.
[0067] The following specific embodiments will be provided to explain the solution of the present invention. Those skilled in the art will understand that the following embodiments are for illustrative purposes only and should not be considered as limiting the scope of the invention. Where specific techniques or conditions are not specified in the embodiments, they are performed according to the techniques or conditions described in the literature in the field or according to the product instructions. Reagents or instruments whose manufacturers are not specified are all conventional products that can be obtained commercially.
[0068] Screening experiment (1) Dissolve various components of alcohols, esters, acids, ketones and aldehydes in 70-80 degree high-proof liquor to prepare a mother liquor with a concentration of 1-10% (w / v); or (2) without dilution. According to the flavor threshold of different flavor substances, add the mother liquor or undiluted alcohols, esters, acids, ketones and aldehydes to commercially available 53° sauce aroma and 52° strong aroma base liquors respectively according to different dosages (since the dosage of each component such as alcohols, esters, acids, ketones and aldehydes is very small, the effect on the final alcohol content is small, and the final alcohol content is still 53° sauce aroma and 52° strong aroma). After sealing, place them together with the control group in a 35° constant temperature box for 7 days, take them out and place them in a 25° environment for 24 hours, and then conduct sensory tasting and hops test.
[0069] The selection criteria were that the experimental group's samples should enhance the flavor of different base spirits without affecting the harmony of the spirit, while also increasing the foaming and settling time of the baijiu. Samples from the experimental group with higher foaming height and settling time than the control group (base spirits) were considered to have improved foaming; samples with lower foaming height and settling time than the control group, or with no significant difference in foaming height or even higher than the control group, but with a shorter settling time, were considered to have poorer foaming.
[0070] The method for determining the height of the foam was as follows: 50 mL of wine was placed in a 150 mL Erlenmeyer flask with a ground glass stopper. The flask was first placed at room temperature (25℃) for 24 hours. The experimental group and the control group were then simultaneously shaken under the same force and angle, and placed on a table to observe the height of the foam. To avoid excessive error, each sample was tested 7 times, and the average value was taken.
[0071] The method for determining the blooming time is as follows: Take 50 mL of wine and place it in a 150 mL Erlenmeyer flask with a ground glass stopper. First, let it stand at room temperature (25℃) for 24 hours. Then, shake the flask to observe the blooming condition and record the blooming time in seconds. The time when the last bloom bursts is the end point. If a single bloom does not burst for a long time, it is not included in the count. To avoid excessive error, each sample is tested 7 times and the average value is taken.
[0072] The experimental results are shown in Tables A and B.
[0073] Table A: Screening Results of Acids
[0074] Table B shows the screening results for some other types of substances.
[0075] The results of the above screening tests show that alcohols and esters in baijiu, at certain concentrations or contents, all have varying degrees of defoaming effects, especially large-molecule fatty acid esters, such as ethyl heptanoate and most long-chain fatty acid esters, which make it difficult for the liquor to foam. Aldehydes and ketones, without affecting the flavor of the liquor, both reduce the persistence of the foam; however, 2,3-butanedione, furfural, and acetal have relatively smaller effects on the persistence of the foam.
[0076] In the experiment on the effects of organic acids on the flavor of liquor, short-chain and medium-chain fatty acids, due to their low threshold, all affected the overall flavor of baijiu. In small amounts, they had varying degrees of defoaming effect or no effect at all. Among fatty acids with a dodecanoic acid content or higher, it was accidentally discovered that only tetradecanoic acid, at a certain concentration, could increase the foaming and settling time of baijiu, while also promoting the flavor of baijiu with different body types. Other organic acids all had varying degrees of defoaming effect in the liquor. Therefore, the applicant further studied the foam stability and flavor stability of baijiu with different tetradecanoic acid contents, and conducted the following research on the preparation of baijiu and its foam and flavor stability.
[0077] The equipment used for detecting trace components in the following examples is: GC-FID (Agilent 8860). Chromatographic conditions: DB-Wax capillary column (0.25 mm x 0.25 μm x 30 m); Carrier gas: He; Flow rate: 1.2 mL / min; Column temperature: The injection port temperature was maintained at 260 ℃, the initial gas chromatography column temperature was 50 ℃, maintained for 2 min, increased to 145 ℃ at 3 ℃ / min, and then increased to 230 ℃ at 15 ℃ / min, and held for 15 min.
[0078] Selective reaction monitoring (SIM) mode was used to detect the main compounds in the wine samples. Quantitative analysis was performed using an external standard-standard curve method.
[0079] Example 1 S1, Preparation of high-tenthyl acetate flavoring wine Step 1: Take a 45% vol Maotai-flavor liquor with a myristic acid content of 1.61 ppm; Step 2: Concentration by vacuum distillation: A. First, the liquor is evaporated and dehydrated through a permeate membrane under a vacuum pressure of 500Pa and a material heating temperature of 45℃ to obtain a flavoring liquor with a tetradecanoic acid content of 11.25ppm and an alcohol content of 78%vol. B. The flavoring wine obtained in step A above is then subjected to thin-film rotary evaporation at a vacuum pressure of 5000 Pa and a material heating temperature of 70°C to obtain a flavoring wine with a tetradecanoic acid content of 194.64 ppm and an alcohol content of 18% vol. Step 3: The flavoring wine obtained in Step B above is subjected to electrodialysis until pH≥5, voltage 15V, current 1A, to remove some lactic acid, acetic acid and other short-chain organic acids that can ionize hydrogen ions, resulting in a flavoring wine with a tetradecanoic acid content of 206.78ppm and an alcohol content of 20%vol. Step 4: Repeat Step 2: A. Dehydrate the flavoring wine from Step 3 by permeate membrane evaporation under a vacuum pressure of 500 Pa and a material heating temperature of 45°C to obtain a flavoring wine with a tetradecanoic acid content of 1980.61 ppm and an alcohol content of 77% vol; B. Then, perform thin-film rotary evaporation on the flavoring wine obtained in Step A under a vacuum pressure of 5000 Pa and a material heating temperature of 70°C to obtain a flavoring wine with a tetradecanoic acid content of 6438.45 ppm and an alcohol content of 36% vol. Step 5: The flavoring wine obtained in Step 4 is subjected to permeate membrane evaporation and dehydration under a vacuum pressure of 500 Pa and a material heating temperature of 45°C, so that the myristic acid content in the flavoring wine reaches 1.04% and the alcohol content is 75% vol. Step Six: Preparative Chromatography: Using a C18 80*250 mm*30 μm stainless steel column, wash the column with 85% ethanol and equilibrate it. Then, load 100 mL of the flavored wine sample obtained in Step Five onto the column and elute with 85% ethanol at a flow rate of 150 mL / min. Collect the fraction with a retention time (RT) between 18.0 and 19.5 min, and distill it to dryness under vacuum to obtain a high-purity tetradecanoic acid sample. Gas chromatography analysis showed that its purity was 93.5%. Redissolve it in 75-degree high-proof liquor to obtain a flavored wine with a tetradecanoic acid content of 1% (this flavored wine has removed hexadecanoic acid and other impurities; the high-content component is only tetradecanoic acid. The 1% is used because 75-degree liquor can only dissolve a maximum of 1% of tetradecanoic acid).
[0080] S2, Mixing Select a commercially available 53% vol Maotai-flavor liquor and test its tetradecanoic acid content to be 0.59 ppm. Blend it with the flavoring liquor containing 1% tetradecanoic acid to obtain a 53% vol Maotai-flavor liquor with a tetradecanoic acid content of 150 ppm.
[0081] Example 2 S1, Preparation of high-tenthyl acetate flavoring wine Same as Example 1 S2, Mixing Select a commercially available 45% vol Maotai-flavor liquor and test its tetradecanoic acid content to be 0.62 ppm. Blend it with the flavoring liquor containing 1% tetradecanoic acid to obtain a 45% vol Maotai-flavor liquor with a tetradecanoic acid content of 5 ppm.
[0082] Example 3 S1, Preparation of high-tenthyl acetate flavoring wine Step 1: Take a 52% vol strong-aroma style baijiu, whose myristic acid content is 0.87 ppm; Step 2: Concentration by vacuum distillation: A. First, the liquor is evaporated and dehydrated through a permeate membrane under a vacuum pressure of 500 Pa and a heating temperature of 45°C to obtain a flavoring liquor with a tetradecanoic acid content of 21.25 ppm and an alcohol content of 78% vol. B. The flavoring wine obtained in step A above is then subjected to thin-film rotary evaporation at a vacuum pressure of 5000 Pa and a heating temperature of 70°C to obtain a flavoring wine with a tetradecanoic acid content of 294.15 ppm and an alcohol content of 18% vol. Step 3: The flavoring wine obtained in Step B above is subjected to electrodialysis until pH≥5, voltage 15V, current 1A, to remove most of the lactic acid, acetic acid and other short-chain organic acids that can ionize hydrogen ions, resulting in a flavoring wine with a tetradecanoic acid content of 243.16ppm and an alcohol content of 21%vol. Step 4: Repeat Step 2: A. Dehydrate the flavoring wine from Step 3 by permeate membrane evaporation under a vacuum pressure of 500 Pa and a material heating temperature of 45°C to obtain a flavoring wine with a tetradecanoic acid content of 2680.04 ppm and an alcohol content of 78% vol; B. Then, perform thin-film rotary evaporation on the flavoring wine obtained in Step A under a vacuum pressure of 5000 Pa and a material heating temperature of 70°C to obtain a flavoring wine with a tetradecanoic acid content of 6583.60 ppm and an alcohol content of 38% vol. Step 5: The flavoring wine obtained in Step 4 is subjected to permeate membrane evaporation and dehydration under a vacuum pressure of 500 Pa and a material heating temperature of 45°C, so that the myristic acid content in the flavoring wine reaches 1.01% and the alcohol content is 76% vol. Step Six: Preparative Chromatography: Using a C18 80*250mm*230um stainless steel column, first wash the column with 85% ethanol and equilibrate it. Then, load 100mL of the flavored wine sample obtained in Step Five onto the column, and elute with 85% ethanol at a flow rate of 150mL / min. Collect the fraction with a retention time (RT) between 18.0 and 19.5min, and distill it to dryness under vacuum to obtain a high-purity tetradecanoic acid sample. Gas chromatography analysis showed that its purity was 92.1%. Reconstitute with 75-degree high-proof liquor to obtain a flavored wine with a tetradecanoic acid content of 1%.
[0083] S2, Mixing Select a commercially available 39% vol strong-aroma baijiu and test its total tetradecanoic acid content to be 0.63 ppm. Blend it with the flavoring wine containing 1% tetradecanoic acid to obtain a 39% vol strong-aroma baijiu with a tetradecanoic acid content of 50 ppm.
[0084] Example 4 S1, Preparation of high-tenthyl acetate flavoring wine Same as Example 3 S2, Mixing Select a commercially available 52% vol strong-aroma baijiu (i.e., the baijiu in step one of Example 3), and test its tetradecanoic acid content to be 0.87 ppm. Blend it with the flavoring wine with a tetradecanoic acid content of 1% to obtain a 52% vol strong-aroma baijiu with a tetradecanoic acid content of 100 ppm.
[0085] Comparative Example 1 S1, Preparation of high-content dodecanoic acid flavoring wine Step 1: Take 45% vol Maotai-flavor liquor (i.e., the liquor in Step 1 of Example 1), whose dodecanoic acid content is 0.61 ppm; Step 2: Concentration by vacuum distillation: A. First, the liquor is evaporated and dehydrated through a permeation membrane under a vacuum pressure of 500 Pa and a heating temperature of 45℃ to obtain a flavoring liquor with a dodecanoic acid content of 9.40 ppm and an alcohol content of 78% vol. B. The flavoring wine obtained in step A above is then subjected to thin-film rotary evaporation at a vacuum pressure of 5000 Pa and a heating temperature of 70°C to obtain a flavoring wine with a dodecanoic acid content of 145.18 ppm and an alcohol content of 18% vol. Step 3: The flavoring wine obtained in Step B above is subjected to electrodialysis until pH≥5, voltage 15V, current 1A, to remove most of the lactic acid, acetic acid and other short-chain organic acids that can ionize hydrogen ions, resulting in a flavoring wine with a dodecanoic acid content of 160.04ppm and an alcohol content of 20%vol. Step 4: Repeat Step 2: A. Dehydrate the flavoring wine from Step 3 by permeate membrane evaporation under a vacuum pressure of 500 Pa and a material heating temperature of 45°C to obtain a flavoring wine with a dodecanoic acid content of 1253.25 ppm and an alcohol content of 77% vol; B. Then, perform thin-film rotary evaporation on the flavoring wine obtained in Step A under a vacuum pressure of 5000 Pa and a material heating temperature of 70°C to obtain a flavoring wine with a dodecanoic acid content of 5278.62 ppm and an alcohol content of 36% vol. Step 5: The flavoring wine obtained in Step 4 is subjected to permeate membrane evaporation and dehydration under a vacuum pressure of 500 Pa and a material heating temperature of 45°C, so that the dodecanoic acid content in the flavoring wine reaches 0.95% and the alcohol content is 75% vol. Step Six: Preparative Chromatography: Using a C18 80*250mm*30um stainless steel column, first wash the column with 85% ethanol and equilibrate it. Then, load 100mL of the flavored wine sample obtained in Step Five onto the column, and elute with 85% ethanol at a flow rate of 150mL / min. Collect the fraction with a retention time RT between 14.0 and 15.0min, and distill it to dryness under vacuum to obtain a high-purity dodecanoic acid sample. Gas chromatography analysis showed that its purity was 91.2%. Reconstitute with 75-degree high-proof liquor to obtain a flavored wine with a dodecanoic acid content of 1%.
[0086] S2, Mixing Select the same commercially available 45% vol Maotai-flavor liquor (i.e., the liquor in step one of Example 1), and test its dodecanoic acid content to be 0.61 ppm. Blend it with the flavoring liquor with 1% dodecanoic acid content mentioned above to obtain a 45% vol Maotai-flavor liquor with a dodecanoic acid content of 5 ppm.
[0087] Comparative Example 2 S1, Preparation of high-content triterpenoid flavoring wine Step 1: Take 45% vol Maotai-flavor liquor (i.e., the liquor in Step 1 of Example 1), whose triterpenoid content is 0.093 ppm; Step 2: Concentration by vacuum distillation: A. First, the liquor is evaporated and dehydrated through a permeation membrane under a vacuum pressure of 500Pa and a heating temperature of 45℃ to obtain a flavoring liquor with a triterpenoid content of 2.78ppm and an alcohol content of 78%vol. B. The flavoring wine obtained in step A above is then subjected to thin-film rotary evaporation at a vacuum pressure of 5000 Pa and a heating temperature of 70°C to obtain a flavoring wine with a triterpenoid content of 45.40 ppm and an alcohol content of 18% vol. Step 3: The flavoring wine obtained in Step B above is subjected to electrodialysis until pH≥5, voltage 15V, current 1A, to remove most of the lactic acid, acetic acid and other short-chain organic acids that can ionize hydrogen ions, resulting in a flavoring wine with a tridecanoic acid content of 43.82ppm and an alcohol content of 20%vol. Step 4: Repeat Step 2: A. Dehydrate the flavoring wine from Step 3 by permeate membrane evaporation under a vacuum pressure of 500 Pa and a material heating temperature of 45°C to obtain a flavoring wine with a triterpenoid content of 901.36 ppm and an alcohol content of 77% vol; B. Then, perform thin-film rotary evaporation on the flavoring wine obtained in Step A under a vacuum pressure of 5000 Pa and a material heating temperature of 70°C to obtain a flavoring wine with a triterpenoid content of 4527.88 ppm and an alcohol content of 36% vol. Step 5: The flavoring wine obtained in Step 4 is subjected to permeate membrane evaporation and dehydration under a vacuum pressure of 500 Pa and a material heating temperature of 45°C, so that the triterpenoid content in the flavoring wine reaches 0.92% and the alcohol content is 75% vol. Step Six: Preparative Chromatography: Using a C18 80*250mm*30um stainless steel column, first wash the column with 85% ethanol and equilibrate it. Then, load 100mL of the flavored wine sample obtained in Step Five onto the column, and elute with 85% ethanol at a flow rate of 150mL / min. Collect the fraction with a retention time (RT) between 15.7 and 16.8 min, and distill it to dryness under vacuum to obtain a high-purity tridecanoic acid sample. Gas chromatography analysis showed that its purity was 90.8%. Reconstitute with 75-degree high-proof liquor to obtain a flavored wine with a tridecanoic acid content of 1%.
[0088] S2, Mixing The same commercially available 53% vol Maotai-flavor liquor was selected, and its triterpenoid content was tested to be 0.058 ppm. It was then blended with the flavoring liquor with a triterpenoid content of 1% to obtain a 53% vol Maotai-flavor liquor with a triterpenoid content of 150 ppm.
[0089] Comparative Example 3 S1. Preparation of high-content 15-fifteen-acid flavoring wine Step 1: Take 52% vol strong-aroma baijiu (same as in Example 3), whose pentadecanoic acid content is 0.54 ppm; Step 2: Concentration by vacuum distillation: A. First, the liquor is evaporated and dehydrated through a permeation membrane under a vacuum pressure of 500Pa and a heating temperature of 45℃ to obtain a flavoring liquor with a pentadecanoic acid content of 8.52ppm and an alcohol content of 78%vol. B. The flavoring wine obtained in step A above is then subjected to thin-film rotary evaporation at a vacuum pressure of 5000 Pa and a heating temperature of 70°C to obtain a flavoring wine with a pentadecanoic acid content of 118.73 ppm and an alcohol content of 18% vol. Step 3: The flavoring wine obtained in Step B above is subjected to electrodialysis until pH ≥ 5, voltage 15V, current 1A, to remove most of the lactic acid, acetic acid and other short-chain organic acids that can ionize hydrogen ions. The resulting flavoring wine has a pentadecanoic acid content of 122.77ppm and an alcohol content of 20%vol. Step 4: Repeat Step 2. A) Dehydrate the flavoring wine from Step 3 by permeate membrane evaporation under a vacuum pressure of 500 Pa and a material heating temperature of 45°C to obtain a flavoring wine with a pentadecanoic acid content of 1201.36 ppm and an alcohol content of 77% vol; B) Then, dehydrate the flavoring wine obtained in Step A by thin-film rotary evaporation under a vacuum pressure of 5000 Pa and a material heating temperature of 70°C to obtain a flavoring wine with a pentadecanoic acid content of 5462.76 ppm and an alcohol content of 35% vol. Step 5: The flavoring wine obtained in Step 4 is subjected to permeate membrane evaporation and dehydration under a vacuum pressure of 500 Pa and a material heating temperature of 45°C, so that the content of pentadecanoic acid in the flavoring wine reaches 0.98% and the alcohol content is 76% vol.
[0090] Step Six: Preparative Chromatography: Using a C18 80*250mm 30um stainless steel column, first wash the column with 85% ethanol and equilibrate it. Then, load 100mL of the flavored wine sample obtained in Step Five onto the column, and elute with 85% ethanol at a flow rate of 150mL / min. Collect the fraction with a retention time RT between 20.5 and 21.5 min, and distill it to dryness under vacuum to obtain a high-purity pentadecanoic acid sample. Gas chromatography analysis showed that its purity was 92.1%. Reconstitute with 75-degree high-proof liquor to obtain a flavored wine with a pentadecanoic acid content of 1%.
[0091] S2, Mixing The same commercially available 39% vol strong-aroma style baijiu was selected, and its 15-fold acid content was tested to be 0.49 ppm. It was then blended with the flavoring wine containing 1% 13-fold acid to obtain a 39% vol strong-aroma style baijiu with a 15-fold acid content of 50 ppm.
[0092] Comparative Example 4 S1, Preparation of high-content hexadecanoic acid flavoring liquor Step 1: Take 52% vol strong-aroma baijiu (i.e., the baijiu in Step 1 of Example 3), whose hexadecanoic acid content is 17.79 ppm; Step 2: Concentration by vacuum distillation: A. First, the liquor is evaporated and dehydrated through a permeate membrane under a vacuum pressure of 500Pa and a heating temperature of 45℃ to obtain a flavoring liquor with a hexadecanoic acid content of 169.85ppm and an alcohol content of 78%vol. B. The flavoring wine obtained in step A above is then subjected to thin-film rotary evaporation at a vacuum pressure of 5000 Pa and a heating temperature of 70 °C to obtain a flavoring wine with a hexadecanoic acid content of 575.76 ppm and an alcohol content of 18% vol. Step 3: The flavoring wine obtained in Step B above is subjected to electrodialysis until pH ≥ 5, voltage 15V, current 1A, which removes most of the lactic acid, acetic acid and other short-chain organic acids that can ionize hydrogen ions. The resulting flavoring wine has a hexadecanoic acid content of 568.57ppm and an alcohol content of 21%vol. Step 4: Repeat Step 2: A. Dehydrate the flavoring wine from Step 3 by permeate membrane evaporation under a vacuum pressure of 500 Pa and a material heating temperature of 45°C to obtain a flavoring wine with a hexadecanoic acid content of 3527.50 ppm and an alcohol content of 78% vol; B. Then, perform thin-film rotary evaporation on the flavoring wine obtained in Step A under a vacuum pressure of 5000 Pa and a material heating temperature of 70°C to obtain a flavoring wine with a hexadecanoic acid content of 6325.64 ppm and an alcohol content of 38% vol. Step 5: The flavoring wine obtained in Step 4 is subjected to permeate membrane evaporation and dehydration under a vacuum pressure of 500 Pa and a material heating temperature of 45°C, so that the hexadecanoic acid content in the flavoring wine reaches 1.03% and the alcohol content is 76% vol. Step Six: Preparative Chromatography: Using a C18 80*250mm 30um stainless steel column, first wash the column with 85% ethanol and equilibrate it. Then, load 100mL of the flavored wine sample obtained in Step Five onto the column, and elute with 85% ethanol at a flow rate of 150mL / min. Collect the fraction with a retention time RT between 27.0 and 28.5min, and distill it to dryness under vacuum to obtain a high-purity hexadecanoic acid sample. Gas chromatography analysis showed that its purity was 87.8%. Reconstitute with 75-degree high-proof liquor to obtain a flavored wine with a hexadecanoic acid content of 1%.
[0093] S2, Mixing Select the same commercially available 52% vol strong-aroma style baijiu (i.e. the baijiu in step one of Example 3), and test its hexadecanoic acid content to be 17.45 ppm. Blend it with the flavoring wine with a hexadecanoic acid content of 1% to obtain a 52% vol strong-aroma style baijiu with a hexadecanoic acid content of 100 ppm.
[0094] Comparative Example 5 We selected the same commercially available 53% vol Maotai-flavor liquor, with a tetradecanoic acid content of 0.59 ppm, as a comparison for liquors with low tetradecanoic acid content.
[0095] Comparative Example 6 We selected the same commercially available 52% vol strong-aroma baijiu, with a tetradecanoic acid content of 0.87 ppm, as a comparison for baijiu with low tetradecanoic acid content.
[0096] Comparative Example 7 S1, Preparation of high-tenthyl acetate flavoring wine Same as Example 1 S2, Mixing Select a 53% vol Maotai-flavor liquor and test its tetradecanoic acid content to be 0.59 ppm. Blend it with the flavoring liquor containing 1% tetradecanoic acid to obtain a 53% vol Maotai-flavor liquor with a tetradecanoic acid content of 160 ppm.
[0097] Comparative Example 8 S1, Preparation of low-content tetradecanoic acid flavoring wine Same as Example 3 S2, Mixing Select a commercially available 39% vol strong-aroma baijiu and test its total tetradecanoic acid content to be 0.63 ppm. Blend it with the flavoring wine containing 1% tetradecanoic acid to obtain a 39% vol strong-aroma baijiu with a tetradecanoic acid content of 2 ppm.
[0098] Table C: Summary of Experimental Examples
[0099] Effect verification 1. Hop stability test The baijiu prepared in the experimental examples in Table C was evaluated for its foaming and settling time. All samples were placed in a 45°C oven and evaluated every 30 days. The foaming status and settling time were recorded on days 0, 60, 120, and 240.
[0100] The method for testing hop stability (i.e., hop settling time) is as follows: Take 50 mL of hops and place them in a 150 mL Erlenmeyer flask with a ground glass stopper. First, place the flask at room temperature (25℃) for 24 hours. Then, shake the flask to observe the quality of the hops and record the hop settling time in seconds. The hop settling time is considered the end of the test, and any individual hops that do not break are not included in the count. To avoid excessive error, each sample is tested 7 times and the average value is taken. The test results are shown in Tables 1-4, and the data are expressed as X±S. Hop thickness refers to the thickness of the foam surface; more than 1 cm is considered thick, and less than 0.5 cm is considered thin.
[0101] Table 1. Hop stability test results (0 days) for different embodiments and comparative examples
[0102] Table 2. Hop stability test results (60 days) for different examples and comparative examples
[0103] Table 3. Hop stability test results (120 days) for different examples and comparative examples
[0104] Table 4. Hop stability test results (240 days) for different examples and comparative examples
[0105] As shown in Tables 1-4, the baijiu from Examples 1-4, whether freshly prepared or during storage, exhibited thicker foam and a longer settling time compared to Comparative Examples 1-8, generally remaining above 50 seconds. The settling time for the other comparative baijiu was generally below 35 seconds, especially for Comparative Examples 1-4, which contained added long-chain fatty acids, which had a certain impact on foam formation and resulted in a shorter settling time. This indicates that when the myristic acid content in baijiu is within a certain range, it can stably increase foam formation and settling time during storage.
[0106] 2. Stability test of Baijiu flavor Sensory evaluation was conducted on the baijiu prepared in the experimental examples in Table C. The specific procedures for sensory evaluation were carried out in accordance with GB / T10345.2. Twelve professionals with sensitive sensory organs, who had undergone specialized training and met the requirements for sensory analysis, were selected to score the aroma, taste, and harmony of the baijiu. The scoring criteria are shown in Table D below, and the data are expressed as X±S.
[0107] Table D: Scoring Standards for Baijiu (Chinese liquor)
[0108] The prepared liquor and raw liquor were scored according to the scoring criteria in Table D. The results are shown in Tables 5-8 below.
[0109] Table 5 Sensory evaluation scores of the baijiu from different embodiments and the original spirit from the comparative example (0 days)
[0110] Table 6 Sensory evaluation scores of the baijiu from different embodiments and the original spirits from the comparative example (60 days)
[0111] Table 7 Sensory evaluation scores of the baijiu from different embodiments and the original spirits from the comparative example (120 days)
[0112] Table 8 Sensory evaluation scores of the baijiu from different embodiments and the original spirits from the comparative example (240 days)
[0113] As shown in Tables 5-8, the aroma, flavor, and harmony of Examples 1-4 were all better than those of the comparative examples. Whether freshly made or during storage, the baijiu (Chinese liquor) scored higher than those of Comparative Examples 1-8. This indicates that when the myristotropic acid content of baijiu is within a certain range, the aroma, flavor, and harmony of aroma and flavor can be stabilized during storage.
[0114] 3. Detection of flavor components in baijiu Flavor components of the baijiu prepared in the experimental examples in Table C were detected using the methods described above.
[0115] Table 9. Detection of wine components in different embodiments (day 0) Unit: ppb
[0116] Table 10 Component Detection of Different Comparative Samples of Wine (Day 0) Unit: ppb
[0117] Table 11. Detection of wine components in different embodiments (120 days) Unit: ppb
[0118] Table 12 Component Detection of Wines from Different Comparative Examples (120 days) Unit: ppb
[0119] Table 13 Detection of wine components in different embodiments (240 days) Unit: ppb
[0120] Table 14 Component Detection of Different Comparative Wines (240 Days) Unit: ppb
[0121] As shown in Tables 9-14, the content of compounds in the wine samples exhibited a certain regularity throughout the storage process. Esters mainly showed a decreasing trend, especially short-chain fatty acid ethyl esters. In addition, alcohols and aldehydes also decreased to some extent. Although flavor compounds showed a certain trend during storage, and after adjustments to the content of long-chain organic acids such as myristic acid, they eventually formed corresponding long-chain fatty acid ethyl esters with ethanol during storage, thus reducing the myristic acid content in the wine, the slight changes in these substances did not affect the overall stability of the wine, based on sensory evaluation results and hop stability. This is likely because myristic acid can form stable chemical bonds in the wine, resulting in a stable associated structure, which greatly enhances the flavor and hop stability of the wine.
Claims
1. A highly stable spirit, characterized in that: The myristic acid content is 5~150ppm, and the alcohol content is 25~78%vol.
2. The high-stability liquor according to claim 1, characterized in that: The baijiu is at least one of the following: soy sauce aroma, strong aroma, light aroma, phoenix aroma, rice aroma, soy sauce aroma, mixed aroma, sesame aroma, special aroma, Laobaigan aroma, rich aroma, Dong aroma, other aroma types, daqu baijiu, xiaoqu baijiu, bran qu baijiu, mixed qu baijiu, solid-state baijiu, liquid-state baijiu, or solid-liquid baijiu.
3. The method for preparing high-stability baijiu according to claim 1 or 2, characterized in that: The goal is to adjust the myristic acid content in baijiu to 5-150 ppm.
4. The method for preparing high-stability baijiu according to claim 3, characterized in that: It involves adjusting the alcohol content of the liquor to 25-78% vol.
5. The method for preparing high-stability baijiu according to claim 3 or 4, characterized in that: Includes the following steps: The myristic acid content in traditional baijiu or baijiu mash is first enriched and concentrated to 1-2% (W / V), with an alcohol content of 70-80% vol. Then, it is further concentrated to over 90% through preparative chromatography or distillation, and finally blended to obtain the final product.
6. The method for preparing high-stability baijiu according to claim 5, characterized in that: The enrichment and concentration refers to directly subjecting traditional baijiu to at least one of the following operations: membrane filtration, distillation, or electrodialysis.
7. The method for preparing high-stability baijiu according to claim 5 or 6, characterized in that: The method includes the following steps: S1. Traditional Baijiu is obtained by conventional solid-state distillation of Baijiu mash, or traditional Baijiu is directly concentrated by vacuum distillation, followed by electrodialysis until the solution pH ≥ 5. The vacuum distillation and / or electrodialysis operations are repeated until the tetradecanoic acid content is 1~2% (W / V) and the alcohol content is 70~80% vol. Then, flavoring wine with a tetradecanoic acid content of more than 90% is obtained by preparative chromatography or distillation. S2. Simply blend the flavoring wine from step S1 with traditional white wine to obtain the final product.
8. The method for preparing high-stability baijiu according to claim 7, characterized in that: In step S1, the vacuum distillation concentration is achieved by at least one of permeate membrane evaporation, thin-film rotary evaporation, or distillation; preferably, the permeate membrane evaporation dehydration pressure is ≤500Pa and the heating temperature is <50℃; preferably, the thin-film rotary evaporation vacuum pressure is ≤5000Pa and the heating temperature is <80℃.
9. The method for preparing high-stability baijiu according to claim 7 or 8, characterized in that: In step S1, the preparative chromatogram is eluted with 85% ethanol, and the fraction with a retention time RT between 18.0 and 19.5 min is collected.
10. The method for preparing high-stability baijiu according to any one of claims 7 to 9, characterized in that: The electrodialysis voltage is 1~15V and the current is 0.05~2A.