Targeted extraction method for flavor substances of Maotai-flavor liquor

Abstract

The invention relates to the technical field of food processing, in particular to a targeted extraction method for flavor substances of Maotai-flavor liquor, which adopts the following preparation method: S10, pretreatment and analysis; s20, carrying out primary reduced pressure rectification; s30, selective extraction with a secondary solvent; s40, molecular imprinting purification; S50, recombination callback; according to the method, target flavor substance components are extracted from Maotai-flavor liquor with high selectivity and high efficiency, irritant and bad flavor substances such as ethanol, higher alcohol and furfural are removed to the greatest extent, concentrated base liquor with mellow flavor and smooth taste is obtained, and a process capable of realizing industrial and standardized production is provided; the invention provides a core raw material for the high-quality Maotai-flavor pre-prepared cocktail, solves the problems of rough taste and unbalanced flavor of the traditional Maotai-flavor cocktail, realizes standardized and customizable production of the flavor of the base wine, improves the acceptability and re-purchase rate of consumers, and provides a core raw material technical support for pre-prepared wine products.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of food processing, in particular to the technology of liquor flavor chemistry and extraction, and especially to a method for targeted extraction of specific flavor components from Maotai-flavor liquor and its specific application in preparing base liquor for high-end cocktails. BACKGROUND

[0002] Maotai-flavor liquor is known for its complex flavor system (such as burnt smell, floral, fruity, and baked aroma), which is mainly derived from alcohols, esters, acids, aldehydes, ketones, and heterocyclic compounds such as pyrazine and furan. Traditional Maotai-flavor cocktails are usually prepared by direct blending, i.e., simply mixing Maotai-flavor liquor with fruit juice, syrup, etc., which has the following significant defects:

[0003] (1) Unbalanced flavor: Direct blending suppresses the aroma of other auxiliary materials due to the strong dominant flavor of Maotai-flavor liquor (such as burnt smell and astringency), resulting in a rough taste that is difficult for the general market, especially the Z generation, to accept.

[0004] (2) Low utilization rate of effective flavor substances: Some valuable and pleasant flavor substances in Maotai-flavor liquor (such as ethyl acetate, ethyl hexanoate, and tetramethylpyrazine (ligustilide)) are masked by a large amount of ethanol and irritating flavors, making it difficult to accurately serve the flavor design of cocktails.

[0005] (3) Poor stability: Direct mixing of liquor bodies can cause sedimentation and loss of luster, and the flavor changes greatly over time, resulting in low repurchase rate.

[0006] (4) Cannot be standardized: Relies on the personal experience of bartenders, with large batch differences, making it difficult to achieve industrialized mass production of pre-mixed drinks.

[0007] Existing extraction technologies (such as conventional distillation, solvent extraction, and supercritical CO2 extraction) have obvious shortcomings when applied to the extraction of Maotai-flavor flavor: conventional distillation can lead to the loss of low-boiling-point aromatic substances and the introduction of high-boiling-point fusel oil; organic solvent extraction has the risk of solvent residue and poor selectivity; supercritical CO2 extraction is relatively mild, but it cannot achieve "targeted" separation and enrichment of the many flavor components with large polarity differences in Maotai-flavor liquor, and the extracted substances are still complex and may contain undesirable flavors.

[0008] Therefore, there is an urgent need to develop a new targeted extraction process that can accurately separate and enrich specific pleasant flavor components in Maotai-flavor liquor while eliminating undesirable flavors and excessive ethanol, to solve the core problems in the application of innovative drinks. SUMMARY

[0009] The purpose of the present application is to overcome the defects and shortcomings of the prior art and provide a method for targeted extraction of Maotai-flavor liquor flavor substances.

[0010] The application discloses a targeting extraction method of flavor substances of Maotai-flavor liquor.

[0011] S10, pretreatment and analysis:

[0012] The flavor substances of base liquor of Maotai-flavor liquor are analyzed, a flavor substance fingerprint is established, a database is formed, and target flavor substance groups needing enrichment and undesirable flavor substance groups needing elimination are determined according to the database;

[0013] S20, primary vacuum rectification: base liquor is subjected to vacuum rectification under the condition that the temperature is 40-60 DEG C and the vacuum degree is-0.08 to-0.1 MPa, low-boiling-point substances are separated and eliminated, and a primary extraction liquid is obtained;

[0014] S30, secondary solvent selective leaching: the primary extraction liquid is mixed with a food-grade solvent with specific polarity, stirring extraction is carried out at 20-40 DEG C, the polarity of the solvent is configured to match the solubility parameter of the target flavor substance group, so that the target flavor substance group is selectively extracted, and a secondary initial extraction liquid is obtained;

[0015] S40, molecular imprinting purification: the secondary initial extraction liquid is subjected to solid-phase extraction column filled with molecular imprinting polymers, the molecular imprinting polymers are prepared by taking at least one key flavor molecule in the target flavor substance group as a template, the target flavor substance is specifically adsorbed and enriched, and a high-purity flavor concentrate is obtained through elution;

[0016] S50, recombination and adjustment: the high-purity flavor concentrate is mixed with edible alcohol and / or water, the ethanol content is adjusted to 20%-50%vol, and a final flavor base liquor is obtained.

[0017] Further, in step S10, headspace solid-phase microextraction-gas chromatography-mass spectrometry is used for flavor substance analysis.

[0018] Further, the target flavor substance group comprises at least one of esters and pyrazine compounds; and the undesirable flavor substance group comprises at least one of higher alcohols and aldehyde compounds.

[0019] Further, the low-boiling-point substances in step S20 comprise one or more of ethanol, acetaldehyde and hydrogen sulfide.

[0020] Further, the food-grade solvent with specific polarity in step S30 is one of an azeotropic mixture of ethyl acetate and water, an ethanol aqueous solution or a propylene glycol aqueous solution.

[0021] Further, the molecular imprinting polymer in step S40 is prepared by taking one of tetramethylpyrazine, ethyl hexanoate or phenethyl alcohol as a template molecule.

[0022] Further, the polarity of the solvent is adjusted by adjusting its composition ratio, so that the difference between its solubility parameter and the average solubility parameter of the target flavor group is within ±2.0 (J / cm 3 )^1 / 2.

[0023] Further, at the outlet of steps S2, S3 and / or S4, an online near-infrared spectroscopy (NIRS) monitoring system is integrated for real-time monitoring of the concentration of key flavor substances in the extraction products at each stage, and automatically adjusting the extraction parameters through a feedback system.

[0024] Further, the total content of target ester substances in the base liquor is more than 3 times that of the original Maotai-flavor base liquor, and the total content of higher alcohols is less than 20% of the original Maotai-flavor base liquor.

[0025] The method for targeted extraction of flavor substances of Maotai-flavor liquor according to the present application realizes high selectivity and high efficiency in extracting target flavor substance components from Maotai-flavor liquor, maximally removes stimulating and undesirable flavor substances such as ethanol, higher alcohols and furfural, obtains concentrated base liquor with smooth flavor and taste, provides a process that can be industrialized and standardized, provides core raw materials for high-quality Maotai-flavor pre-mixed cocktails, solves the problems of rough taste and unbalanced flavor of traditional Maotai-flavor cocktails, realizes standardized and customizable production of base liquor flavor, improves consumer acceptance and repeat purchase rate, and provides core raw material technical support for pre-mixed cocktail products. BRIEF DESCRIPTION OF DRAWINGS

[0026] The accompanying drawings, which are included to provide a further understanding of the present application and constitute a part of this application, do not limit the present application, and in the drawings:

[0027] Figure 1 is a process flow diagram of the present application;

[0028] Figure 2 is a left enlarged view of Figure 1 ;

[0029] Figure 3 is a middle enlarged view of Figure 1 ;

[0030] Figure 4 is a right enlarged view of Figure 1 . DETAILED DESCRIPTION

[0031] The present application will be described in detail below with reference to the accompanying drawings and specific examples, wherein the illustrative examples and descriptions are only used to explain the present application, but do not limit the present application.

[0032] The method for targeted extraction of flavor substances of Maotai-flavor liquor according to the present application is prepared by the following method:

[0033] S10, pretreatment and analysis:

[0034] Flavor substances of Jiangxiang base liquor are analyzed, a flavor substance fingerprint is established, and a database is formed;

[0035] Different rounds and years of Jiangxiang base liquor are selected, the composition of flavor substances is analyzed by using headspace solid-phase microextraction-gas chromatography-mass spectrometry, and a Jiangxiang flavor substance fingerprint database is established;

[0036] And according to this, the target flavor group that needs to be enriched and the undesirable flavor group that needs to be removed are determined;

[0037] According to the target cocktail flavor guide (if the aroma is dominant, the baking aroma is dominant, etc.), the target flavor group (group A) that needs to be enriched and the undesirable flavor group (group B) that needs to be removed are screened from the database;

[0038] S20, primary vacuum rectification: the base liquor is subjected to vacuum rectification under the conditions of a temperature of 40-60 DEG C and a vacuum degree of-0.08 to-0.1 MPa, low-boiling-point substances are separated and removed, and a primary extraction liquid is obtained;

[0039] In the present application, the primary extraction (vacuum rectification) is carried out under the conditions of a low temperature of 40-50 DEG C and a high vacuum of-0.09 to-0.1 MPa; under this condition, low-boiling-point substances such as ethanol, acetaldehyde and hydrogen sulfide are preferentially distilled out and collected, and by accurately controlling the temperature and the vacuum degree, the target flavor substances with medium and high boiling points are retained.

[0040] S30, secondary solvent selective leaching: the primary extraction liquid is mixed with a food-grade solvent with a specific polarity, and stirring extraction is carried out at 20-40 DEG C; the polarity of the solvent is configured to match the solubility parameter of the target flavor group, so that the target flavor group is selectively extracted, and a secondary initial extraction liquid is obtained;

[0041] In the present application, the secondary extraction (customized solvent selective leaching) is carried out by mixing the liquor body after the primary extraction with a food-grade solvent (such as an azeotropic mixture of ethyl acetate and water) with a specific polarity in a certain proportion; the polarity of the solvent is designed to match the solubility parameter of the target flavor group A, so that selective and efficient extraction is realized, while the solubility parameter of the undesirable flavor group B is mismatched, so that most of it is retained in the residual liquid.

[0042] S40, molecular imprinting purification: the secondary initial extraction liquid is passed through a solid-phase extraction column filled with molecular imprinting polymers, the molecular imprinting polymers are prepared by using at least one key flavor molecule in the target flavor group as a template, and are used to specifically adsorb and enrich the target flavor, and then a high-purity flavor concentrate is obtained by elution;

[0043] In the present application, the primary extract obtained by secondary extraction is passed through a device equipped with a molecular imprinting polymer solid-phase extraction column; the polymer of the extraction column is prepared by template polymerization for key marker molecules in group A target flavors (such as tetramethylpyrazine), and has high specific adsorption capacity, can further capture and enrich group A substances, while allowing a small amount of co-extracted group B impurities to flow through, achieving precise purification at the molecular level.

[0044] S50, recombination and readjustment: mixing the high-purity flavor concentrate with edible alcohol and / or water to adjust the ethanol content to 20%-50%vol to obtain the final flavor base liquor.

[0045] In the present application, the purified high-concentration flavor extract is diluted and recombined with high-purity edible alcohol and soft water; finally, the ethanol content is accurately readjusted to the ideal pre-mixed liquor base liquor concentration of 20%-30%vol, and the original liquor color can be retained or completely removed according to product requirements.

[0046] Further, in step S10, headspace solid-phase microextraction-gas chromatography-mass spectrometry (HS-SPME-GC-MS) technology is used for flavor substance analysis.

[0047] Further, the target flavor group includes at least one of esters and pyrazine compounds; the undesirable flavor group includes at least one of higher alcohols and aldehyde compounds.

[0048] Further, the low-boiling-point substance in step S20 includes one or more of ethanol, acetaldehyde, and hydrogen sulfide.

[0049] Further, the food-grade solvent of a specific polarity in step S30 is one of an azeotropic mixture of ethyl acetate and water, an ethanol aqueous solution, or a propylene glycol aqueous solution.

[0050] Further, the molecular imprinting polymer in step S40 is prepared using one of tetramethylpyrazine, ethyl hexanoate, or phenethyl alcohol as a template molecule.

[0051] Further, the polarity of the solvent is adjusted by adjusting its composition ratio, so that the difference between its solubility parameter and the average solubility parameter of the target flavor group is within ±2.0 (J / cm 3 )^1 / 2.

[0052] Further, an online near-infrared spectroscopy (NIRS) monitoring system is integrated at the outlet of steps S2, S3, and / or S4 for real-time monitoring of the concentration of key flavor substances in each extraction product, and automatically adjusting the extraction parameters through a feedback system.

[0053] Furthermore, the total content of target esters in the base liquor is more than three times that of the original sauce-flavored base liquor, and the total content of higher alcohols is less than 20% of that of the original sauce-flavored base liquor.

[0054] Specific examples are described below:

[0055] like Figures 1-2 As shown, the process of this invention is a continuous, multi-stage integrated system. In step S10, the base liquor is first transported from the raw liquor storage tank 1 to the primary extraction unit via the feed pump 2. The primary extraction unit is a vacuum distillation column 3.

[0056] Then, under the negative pressure created by the vacuum system 4, low-boiling-point substances (ethanol, acetaldehyde, etc.) are evaporated, liquefied by the condenser 5 and collected in the first temporary storage tank 6. The concentrate (residue) after removing light components is temporarily stored in the second temporary storage tank 7 (first-stage extraction temporary storage tank).

[0057] like Figure 3 As shown, the above-mentioned concentrate and a specific polar solvent precisely added by the metering system 8 are then simultaneously introduced into the secondary extraction unit (extraction vessel 9) for selective extraction; the mixture after extraction is introduced into the core purification unit, which is a molecularly imprinted polymer solid-phase extraction column 10.

[0058] Then, as it flows through the SPE column, the target flavor molecules in the initial extract are specifically adsorbed, while impurities are treated as waste liquid and enter the collector 12.

[0059] Next, the SPE column is eluted with an eluent to desorb the high-purity target flavor substances and collect them in tank 13, yielding a high-purity flavor concentrate S7, which is temporarily stored in a high-purity flavor concentrate tank. This unit is equipped with an online near-infrared spectroscopy monitoring probe 11 for real-time monitoring of the extraction and purification effect.

[0060] Finally, the mixture enters the recombination unit. The high-purity flavor concentrate S7 from the high-purity flavor concentrate tank is mixed with the high-purity edible alcohol and soft water S8 from the storage tanks (15, 16) in the precision blending tank 17 according to a preset ratio. The ethanol content is precisely adjusted to the required alcohol content and homogenized to finally obtain the finished targeted extraction sauce-flavored base liquor S9, which is stored in the finished base liquor storage tank 18 for later use.

[0061] To further illustrate, the preparation process for a "floral and fruity" flavored soy sauce-flavored cocktail base spirit is as follows:

[0062] Step 1: Preprocessing and Analysis

[0063] Select 3 years of aging Maotai-flavor base liquor, by HS-SPME-GC-MS analysis, determine the target enrichment group A (ethyl acetate, ethyl hexanoate, phenethyl alcohol, ethyl lactate) and eliminate group B (acetaldehyde, furfural, n-propanol, isobutyl alcohol).

[0064] Step two: primary extraction:

[0065] 100L base liquor is pumped into a vacuum distillation column, the temperature is controlled at 45℃, the vacuum degree is-0.095MPa, and the low-boiling-point substances (containing a large amount of ethanol and acetaldehyde) are collected, and the intermediate is obtained in the tower kettle, which is concentrated about 2 times.

[0066] Step three: secondary extraction: the intermediate is mixed with a specific proportion of ethyl acetate-water azeotropic solvent, and stirred at 25℃ for 1 hour. Ethyl acetate is preferentially extracted with A group of esters and alcohols.

[0067] Step four: purification: after solid-liquid separation, the extract is pumped into an MIP-SPE column with tetramethylpyrazine as a template molecule. A group of substances is specifically adsorbed, and then a small amount of ethanol is used for elution to obtain a high-purity flavor concentrate.

[0068] Step five: recombination:

[0069] The flavor substance content of the concentrate is analyzed, and it is diluted and recombined with 95% edible alcohol and pure water. Finally, the product is adjusted to be colorless and transparent, and the alcohol content is 25%vol.

[0070] Step six: effect:

[0071] After detection, the total content of target esters in the finished base liquor is 4.2 times that of the original liquor, and the content of undesirable aldehydes and alcohols is only 18% of that of the original liquor. When it is used to make "Maotai-flavor mojito", the blind test approval rate reaches 85%, which is significantly better than directly using Maotai-flavor liquor (approval rate 35%).

[0072] Compared with the prior art, the present application has the following remarkable beneficial effects:

[0073] 1. Flavor accuracy: precise intervention in the complex Maotai-flavor matrix is realized, and high-quality base liquor with clear flavor orientation and purity is obtained. Through the "database guidance-two-stage extraction-molecular imprinting" technical path, the "surgical operation" precise intervention in the complex Maotai-flavor matrix is realized, and high-quality base liquor with clear flavor orientation and purity is obtained.

[0074] 2. Revolutionary improvement of taste: the unpleasant taste such as pungency, astringency and bitterness is greatly reduced, the taste is smooth, and the pleasant flavor is prominent. The base liquor greatly reduces the unpleasant taste such as pungency, astringency and bitterness, the taste is extremely smooth, the pleasant flavor such as fruit flavor and baking flavor is prominent, and it is easy to be accepted by non-traditional Maotai-flavor liquor consumers. According to the preliminary blind test, the taste acceptance degree is improved by more than 60%.

[0075] 3. High standardization and stability: digital control of process parameters, minimal batch-to-batch difference (RSD of key flavor substances <5%), solving the core problem of industrial mass production.

[0076] 4. Flexibility of application: different flavor-focused base liquor can be produced according to different product requirements (such as fruit, tea, and spice cocktails), providing strong core raw material support for subsequent product development

[0077] 5. Building core technology barriers: this process integrates flavor chemistry, separation engineering, and polymer material technology, with high technical complexity and innovation, making it difficult to imitate.

[0078] The above is only the preferred embodiment of the present application, so any equivalent changes or modifications made in accordance with the characteristics and principles described in the scope of the present patent application are included in the scope of the present patent application.

Claims

1. A targeted extraction method of flavor substances in Maotai-flavor liquor, characterized in that: The preparation method is as follows: S10, pretreatment and analysis: The flavor substances of the Jiangxiang type liquor base liquor are analyzed, the flavor substance fingerprint is established, the database is formed, the target flavor substance group which needs to be enriched and the undesirable flavor substance group which needs to be removed are determined according to the database; S20, primary vacuum rectification: the base liquor is subjected to vacuum rectification under the conditions that the temperature is 40-60 DEG C and the vacuum degree is-0.08 to-0.1 MPa, low-boiling-point substances are separated and removed, and the primary extraction liquid is obtained; S30, secondary solvent selective extraction: the primary extraction liquid is mixed with a food-grade solvent with a specific polarity, and stirring extraction is carried out at 20-40 DEG C, the polarity of the solvent is configured to match the solubility parameter of the target flavor substance group, so that the target flavor substance group is selectively extracted, and the secondary initial extraction liquid is obtained; S40, molecular imprinting purification: the secondary initial extraction liquid is passed through a solid-phase extraction column filled with molecular imprinting polymers prepared by using at least one key flavor molecule in the target flavor substance group as a template, so as to specifically adsorb and enrich the target flavor substance, and then eluted to obtain a high-purity flavor concentrate; S50, recombination and adjustment: the high-purity flavor concentrate is mixed with edible alcohol and / or water, the ethanol content is adjusted to 20%-50%vol, and the final flavor base liquor is obtained.

2. The targeting extraction method of flavor substances of Maotai-flavor liquor according to claim 1, characterized in that: In step S10, headspace solid-phase microextraction-gas chromatography-mass spectrometry is used for flavor substance analysis.

3. The targeting extraction method of flavor substances of Maotai-flavor liquor according to claim 1, characterized in that: The target flavor substance group includes at least one of esters and pyrazine compounds; the undesirable flavor substance group includes at least one of higher alcohols and aldehyde compounds.

4. The method according to claim 1, wherein the method is characterized by: The low-boiling-point substances in step S20 include one or more of ethanol, acetaldehyde and hydrogen sulfide.

5. The method according to claim 1, wherein the method is characterized by: The food-grade solvent with a specific polarity in step S30 is one of an azeotropic mixture of ethyl acetate and water, an ethanol aqueous solution, or a propylene glycol aqueous solution.

6. The method according to claim 1, wherein the method is characterized by: The molecular imprinting polymer in step S40 is prepared by using one of tetramethylpyrazine, ethyl hexanoate or phenethyl alcohol as a template molecule.

7. The method according to claim 1, wherein the method is characterized by: The polarity of the solvent is adjusted by adjusting its composition ratio so that the difference between its solubility parameter and the average solubility parameter of the target flavor group is within ± 2.0 (J / cm 3 )^1 / 2.

8. The method according to claim 1, wherein the method is characterized by: At the outlet of steps S2, S3 and / or S4, an online near-infrared spectrum monitoring system is integrated for real-time monitoring of the concentration of key flavor substances in the extraction products at each stage, and the extraction parameters are automatically adjusted through a feedback system.

9. A Jiangxiang flavor concentrated base liquor prepared by the process of any one of claims 1-8.

10. Use of the Jiangxiang flavor concentrated base liquor of claim 9 in the preparation of a cocktail, a pre-mixed drink, a beverage or a foodstuff.

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