Method for improving content of health functional ingredients of vinegar and reducing precipitation

Abstract

The present application relates to the technical field of vinegar processing, and specifically discloses a method for improving functional components of vinegar and reducing precipitation by high-pressure homogenization, gradient membrane filtration and low-temperature concentration. The method comprises the following steps: S1, preparation and selection of vinegar stock solution; S2, high-pressure homogenization pretreatment of the vinegar stock solution; S3, gradient membrane filtration separation of target components; and S4, low-temperature vacuum concentration of functional substances. The vinegar stock solution is subjected to high-pressure homogenization, and pectinase is added to synergistically decompose polysaccharides, break up colloidal clumps, and release the wrapped functional components. Then, the target components are precisely separated through gradient membrane filtration, and finally, low-temperature vacuum concentration is performed to achieve the purpose of enriching functional components. The present application can not only significantly improve the extraction rate and stability of functional components of vinegar, but also reduce energy consumption and precipitation, and is suitable for industrialized production of high-quality vinegar and can be extended to the development of high-value-added products such as health vinegar and medicinal vinegar.

Description

Technical Field

[0001] This invention relates to the field of vinegar processing technology, specifically to a method for increasing the content of health-promoting functional components in vinegar and reducing precipitation. Background Technology

[0002] Vinegar, a liquid acidic condiment made alone or in combination with various starchy, sugary, and edible alcohol fermented by microorganisms, contains a variety of functional components, such as polyphenols, flavonoids, and tetramethylpyrazine. These components possess physiological activities such as antioxidation, lowering blood lipids, and anti-aging. The content of these components directly affects the health benefits and market positioning of vinegar. However, due to impurities such as colloids and large protein molecules interfering with the encapsulation of functional components, the retention rate of functional components in traditionally fermented vinegar is low.

[0003] Current technologies for extracting and enriching functional components in vinegar mainly focus on conventional filtration and high-temperature concentration processes. For example, diatomaceous earth pre-coated filtration for concentration suffers from several drawbacks: it cannot accurately retain target components and has low concentration efficiency, requiring frequent filter media replacement. Single-membrane filtration technology, on the other hand, can cause membrane pore blockage and small molecule retention. Traditional high-temperature evaporation concentration, typically at temperatures ≥80℃, can cause degradation of heat-sensitive components, damage to functional active substances and product nutrients, and is also energy-intensive. Existing methods do not optimize the filtration and concentration processes in a coordinated manner, making continuous production impossible.

[0004] Therefore, a vinegar production process that can effectively increase the content of health-promoting functional components in vinegar and has a simple preparation process that can be adapted to continuous production is a technical problem that urgently needs to be solved in this field. Summary of the Invention

[0005] To overcome the above-mentioned technical defects, the present invention adopts the following technical solution: The first aspect of this invention provides a method for increasing the content of health-promoting functional components in vinegar and reducing precipitation, comprising the following steps: S1: Preparation and selection of vinegar stock solution; S2: High-pressure homogenization of vinegar concentrate to break down colloids and large molecular aggregates in the concentrate; S3: Separate the target components by filtration of the homogenized vinegar liquid through a gradient membrane; S4: The filtrate after membrane filtration is concentrated under low temperature and vacuum to enrich functional substances; Furthermore, in S1, the vinegar stock solution is any one or more of solid-state fermented vinegar, liquid-state fermented vinegar, and compound fermented vinegar; Furthermore, in S2, the homogenization pressure is 50~150MPa, and the high-pressure homogenization is performed 2~3 times; Furthermore, in S2, pectinase with a mass concentration of 0.1% to 0.5% of the original vinegar solution is added before homogenization; Furthermore, in S2, the homogenization temperature is 40~45℃, and the pH is 3.5-4.5; Furthermore, in S3, the gradient membrane filtration includes primary filtration and secondary filtration, wherein the primary filtration uses a membrane with a pore size of 0.1~0.2 mm. m The secondary filtration includes filtration using a ceramic microfiltration membrane with a molecular weight cutoff of 5-10 kDa; Furthermore, in S3, the gradient membrane is also cleaned using a pulse backwashing method, with a backwashing pressure of 0.2~0.4 MPa and a rinsing interval of 20~40 minutes. Furthermore, in S4, the conditions for low-temperature vacuum concentration are: concentration temperature 35-45℃, vacuum degree -0.095~-0.08MPa, and concentration to 20-40% of the original volume of the filtrate; Furthermore, in S4, the low-temperature vacuum concentration also includes adding 0.01~0.05% of ascorbic acid by mass of the filtrate as an antioxidant; A second aspect of the present invention provides a system for any of the above-mentioned methods for increasing the content of health-promoting functional components in vinegar and reducing precipitation, comprising: a high-pressure homogenizing device, a gradient membrane filtration device, a low-temperature vacuum concentration device, and a control system; A third aspect of the present invention provides a vinegar with health-promoting functions, wherein the vinegar is made by any of the methods described above; Furthermore, the vinegar contains ≥2500 mg / L of polyphenols, ≥1200 mg / L of flavonoids, and ≥50 mg / L of tetramethylpyrazine. The fourth aspect of the present invention provides the use of any of the above-mentioned health-promoting vinegars in the preparation of high value-added products; Furthermore, the high value-added product is a vinegar health product or a medicinal vinegar; Beneficial effects

[0006] Compared with the prior art, the beneficial effects of the present invention are: 1. Process Synergy: For the first time, high-pressure homogenization technology is introduced into the vinegar pretreatment process to solve the problem of colloidal encapsulation; a gradient membrane filtration method of "microfiltration + ultrafiltration" is adopted to achieve graded removal of impurities; pulse backwashing technology is used to remove particulate impurities remaining on the filter membrane, reducing the load on subsequent ultrafiltration; and low-temperature concentration and antioxidants are used in combination to protect heat-sensitive components.

[0007] 2. Precise Parameter Control: By exploring the effects of homogenization pressure (30-200 MPa) on membrane flux and concentration temperature (30-80℃) on browning index, the effects of different parameters on functional components were verified. The optimal parameters for high-pressure homogenization combined with gradient membrane filtration and low-temperature concentration were determined, identifying the optimal homogenization pressure range as 50-150 MPa and membrane pore size (0.1~0.2 mm for microfiltration). m The best results are achieved with ultrafiltration (5-10 kDa) and a concentration temperature ≤45℃.

[0008] 3. Experiments have shown that, compared with existing technologies, the polyphenol retention rate of this invention is higher than that of traditional processes, and the polyphenol content of the final product is increased by more than 50%; the membrane operating flux after homogenization treatment is increased by more than 150% compared with traditional processes; the combination of high-pressure homogenization synergistic gradient membrane filtration and low-temperature concentration process reduces unit energy consumption by more than 50% compared with traditional processes; the high-functionality vinegar produced by this invention has good stability, with no obvious precipitation after 18 months of storage, compared with the obvious precipitation after 6 months of traditional solid-state fermentation process, extending the shelf life by 200%. Attached Figure Description

[0009] Figure 1 This is a flowchart of the core process of this invention. Detailed Implementation

[0010] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present application will be clearly and completely described below with reference to the accompanying drawings. Obviously, the embodiments described below are only some embodiments of the present application, not all embodiments. Therefore, based on the embodiments of the present application, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present application. Example

[0011] Example 1 A method for enhancing the functional components of vinegar and reducing precipitation includes the following steps: S1 Vinegar stock solution preparation and selection, wherein the stock solution is Zhenjiang vinegar fermentation liquid with a total acidity of 6.00g / 100mL; S2 high-pressure homogenization treatment breaks down colloids and macromolecular aggregates in the original vinegar solution. The homogenization pressure is 110 MPa, the number of cycles is 2, and 0.3% pectinase is added (operation conditions: pH 4.0, 42℃ water bath for 30 min). S3 separates the target components from the homogenized liquid through gradient membrane filtration. The membrane filtration system includes primary filtration: using a ceramic microfiltration membrane with a pore size of 0.2 μm; secondary filtration: using a PES ultrafiltration membrane with a molecular weight cutoff of 10 kDa; and pulse backwashing technology with a backwashing pressure of 0.3 MPa and an interval of 30 min. The filtrate after membrane filtration in S4 was concentrated and enriched with functional substances under low-temperature vacuum. A rotary evaporator with a matching low-temperature cooling system was used, with a concentration temperature of 42℃, a vacuum degree of -0.09MPa, a concentration volume of 30% of the original volume, and the addition of 0.02% ascorbic acid.

[0012] Example 2 Based on Example 1, the differences from Example 1 are as follows: the vinegar stock in S1 is Shanxi aged vinegar fermentation liquid with a total acid of 6.00g / 100mL; the high-pressure homogenization pressure in S2 is 100MPa; the primary filtration in S3 uses a ceramic microfiltration membrane with a pore size of 0.1μm, and the secondary filtration uses a PES ultrafiltration membrane with a molecular weight cutoff of 5kDa; the concentration temperature in S4 is 40℃.

[0013] Example 3 Based on Example 1, the difference from Example 1 is that the homogenization pressure in S2 is 30 MPa.

[0014] Example 4 Based on Example 1, the difference from Example 1 is that the homogenization pressure in S2 is 50 MPa.

[0015] Example 5 Based on Example 1, the difference from Example 1 is that the homogenization pressure in S2 is 150 MPa.

[0016] Example 6 Based on Example 1, the difference from Example 1 is that the homogenization pressure in S2 is 200 MPa.

[0017] Example 7 Based on Example 1, the difference from Example 1 is that the concentration temperature in S4 is 35°C.

[0018] Example 8 Based on Example 1, the difference from Example 1 is that the concentration temperature in S4 is 45°C.

[0019] Example 9 Based on Example 1, the difference from Example 1 is that the concentration temperature in S4 is 60°C.

[0020] Example 10 Based on Example 1, the difference from Example 1 is that the concentration temperature in S4 is 80°C.

[0021] II. Comparative Example Comparative Example 1 S1 Preparation and selection of vinegar stock solution, wherein the stock solution is the same batch of Zhenjiang vinegar fermentation liquid as in Example 1; S2 Filtering the vinegar stock solution with diatomaceous earth with a pore size of 20μm; S3 Concentrating the filtered stock solution three times at 80℃ and normal pressure to obtain concentrated solution.

[0022] Comparative Example 2 S1 Preparation and selection of vinegar stock solution, wherein the stock solution is the same batch of Zhenjiang vinegar fermentation liquid as in Example 1; S2 After filtering the vinegar stock solution with diatomaceous earth to obtain a pore size of 20 μm, it is then filtered with a membrane to obtain a pore size of 200 nm; S3 The filtered stock solution is concentrated three times at 80°C and normal pressure to obtain a concentrated solution.

[0023] Comparative Example 3 S1 Preparation and selection of vinegar stock solution, wherein the stock solution is the same batch of Zhenjiang vinegar fermentation liquid as in Example 1; S2 Centrifuge the vinegar stock solution at 6000 rpm for 15 min, and then filter it through a membrane with a pore size of 200 nm; S3 Concentrate the concentrated stock solution at 80℃ and normal pressure by 3 times to obtain concentrated liquid.

[0024] Comparative Example 4 S1 Preparation and selection of vinegar stock solution, wherein the stock solution is the same batch of Zhenjiang vinegar fermentation liquid as in Example 1; S2 The vinegar stock solution is concentrated by freezing at low temperature by 3 times to obtain concentrated solution. The freezing concentration temperature is -10℃ and the freezing concentration treatment time is 12h. The freezing treatment is to precipitate water in the form of ice crystals to obtain frozen concentrated vinegar solution.

[0025] Comparative Example 5 S1 Preparation and selection of vinegar stock solution, wherein the stock solution is the same batch of Zhenjiang vinegar fermentation liquid as in Example 1; S2 Concentrate the vinegar stock solution by vacuum rotary evaporation three times to obtain concentrated liquid.

[0026] Comparative Example 6: Commercially available vinegar No. 1 Comparative Example 7: Commercially available vinegar No. 2 Comparative Example 8: Commercially available vinegar No. 3 Comparative Example 9: Commercially available vinegar No. 4 III. Experimental Examples 3.1 Measurement Method Total acid content: Refer to GB 18187-2000 "Brewn Vinegar" Total flavonoids and tetramethylpyrazine content: Refer to GB / T 19777-2013 Geographical Indication Product "Shanxi Aged Vinegar" Polyphenol content: Refer to T / AHFIA 005-2018 Folin-Ciocalteu spectrophotometric method Particle size distribution: Detected using a laser particle size analyzer. Membrane flux decay rate: refers to the rate or proportion at which membrane flux (the volume of fluid passing through a unit membrane area per unit time) gradually decreases over time. Browning Index (BI): The absorbance values ​​of vinegar diluted with distilled water at 420 nm and 520 nm were measured, which were A... 420nm and A 520nm , BI=(A 520nm -A 420nm ) / Dilution factor 3.2 Test Results The indicators of vinegar and vinegar concentrate in the above embodiments and comparative examples were tested, and the results are shown in Tables 1-5. The results show that the method of using high-pressure homogenization combined with gradient membrane filtration and low-temperature concentration to enhance the functional components of vinegar, compared with traditional methods of single membrane concentration or vacuum / freeze concentration, significantly increases the content of functional active ingredients such as flavonoids, polyphenols, and ligustrazine, far exceeding that of commercially available vinegar. The membrane throughput after homogenization is more than 150% higher than that of traditional processes. The combination of high-pressure homogenization combined with gradient membrane filtration and low-temperature concentration reduces unit energy consumption by more than 50% compared to traditional processes. The high-functionality vinegar produced using this invention exhibits good stability, with no significant precipitation after 18 months of storage, compared to significant precipitation after 6 months in traditional solid-state fermentation processes, extending the shelf life by 200%.

[0027]

[0028] Note: D10 refers to the particle size corresponding to 10% of the cumulative distribution, D50 refers to the particle size corresponding to 50% of the cumulative distribution, and D90 refers to the particle size corresponding to 90% of the cumulative distribution.

[0029]

[0030]

[0031]

[0032] The above description is merely the preferred embodiment of this application, but the scope of protection of this application is not limited thereto. Any variations or substitutions within the technical scope disclosed in this application should be included within the scope of protection of this application. Therefore, the scope of protection of this application should be determined by the scope of the claims.

Claims

1. A method for increasing the content of health-promoting functional components and reducing precipitation in vinegar, characterized in that, Includes the following steps: S1: Preparation and selection of vinegar stock solution; S2: High-pressure homogenization of vinegar concentrate to break down colloids and large molecular aggregates in the concentrate; S3: Separate the target components by filtration of the homogenized vinegar liquid through a gradient membrane; S4: The filtrate after membrane filtration is concentrated under low temperature and vacuum to enrich functional substances.

2. The method for increasing the content of health-promoting functional components and reducing precipitation in vinegar according to claim 1, characterized in that, In S1, the vinegar stock solution is any one or more of solid-state fermented vinegar, liquid-state fermented vinegar, and compound fermented vinegar.

3. The method for increasing the content of health-promoting functional components and reducing precipitation in vinegar according to claim 1, characterized in that, In S2, the homogenization pressure is 50~150MPa, and the high-pressure homogenization is performed 2~3 times; Furthermore, in S2, the homogenization temperature is 40~45℃ and the pH is 3.5-4.

5.

4. The method for increasing the content of health-promoting functional components and reducing precipitation in vinegar according to claim 1, characterized in that, In step S2, pectinase with a mass concentration of 0.1% to 0.5% of the original vinegar solution is added before homogenization.

5. The method for increasing the content of health-promoting functional components and reducing precipitation in vinegar according to claim 1, characterized in that, In S3, the gradient membrane filtration includes primary filtration and secondary filtration, wherein the primary filtration uses a membrane with a pore size of 0.1~0.2 mm. μ The secondary filtration includes filtration using a ceramic microfiltration membrane with a molecular weight cutoff of 5-10 kDa; the secondary filtration includes filtration using a polyether sulfone (PES) ultrafiltration membrane with a molecular weight cutoff of 5-10 kDa.

6. The method for increasing the content of health-promoting functional components and reducing precipitation in vinegar according to claim 1, characterized in that, In S3, the gradient membrane is also cleaned using a pulse backwashing method, with a backwashing pressure of 0.2~0.4 MPa and a rinsing interval of 20~40 minutes.

7. The method for increasing the content of health-promoting functional components and reducing precipitation in vinegar according to claim 1, characterized in that, In S4, the conditions for low-temperature vacuum concentration are: concentration temperature 35-45℃, vacuum degree -0.095~-0.08MPa, and concentration to 20-40% of the original volume of the filtrate.

8. The method for increasing the content of health-promoting functional components and reducing precipitation in vinegar according to claim 1, characterized in that, In S4, the low-temperature vacuum concentration further includes adding 0.01~0.05% of ascorbic acid by mass of the filtrate as an antioxidant.

9. A system for increasing the content of health-promoting functional components and reducing precipitation in vinegar as described in any one of claims 1 to 8, comprising: High-pressure homogenizing device, gradient membrane filtration device, low-temperature vacuum concentration device and control system.

10. A type of vinegar with health benefits, characterized in that, The vinegar is made by the method described in any one of claims 1 to 8; further, the vinegar contains ≥2500 mg / L of polyphenols, ≥1200 mg / L of flavonoids, and ≥50 mg / L of ligustrazine.

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