Preparation method for rosa roxburghii extract having high natural VC content

Abstract

A preparation method for a Rosa roxburghii extract having a high natural VC content, comprising the following steps: (1) adding water into frozen fresh Rosa roxburghii fruit for homogenization, and performing extraction when the homogenization is finished to obtain an extracted liquid; (2) adding a compound enzyme preparation into the extracted liquid for enzymolysis to obtain an enzymolyzed liquid; (3) carrying out solid-liquid separation on the enzymolyzed liquid to obtain a clear liquid and residues; (4) decolorizing the clear liquid by means of an adsorbent to obtain a decolorized liquid; (5) adding an encapsulated deodorant into the decolorized liquid to obtain a deodorized liquid; (6) directionally trapping a target substance from the deodorized liquid, and collecting the permeate and the retentate; and (7) drying the retentate and the permeate, and collecting dry powder. According to the preparation method, Rosa roxburghii is used as a raw material, and a Rosa roxburghii extract product having a high (≥40％) VC content, good taste, and good stability is prepared by means of the procedures such as cold pressing, enzymolysis, demineralization, decolorization, membrane-based separation, and drying.

Description

A preparation method of high-purity natural VC roxburghii extract

[0001] This application claims priority to a Chinese patent application filed with the Patent Office of China on September 4, 2023, with application number 2023111367418 and invention name “A method for preparing high-purity natural VC sea buckthorn extract”, the entire contents of which are incorporated by reference into this application. Technical Field

[0002] The invention relates to the technical field of food processing, and in particular to a method for preparing a high-purity natural VC roxburghii extract. Background Art

[0003] Rosa roxburghii, a member of the genus Rosa in the Rosaceae family, is a wild resource unique to the Yunnan-Guizhou Plateau and the western Sichuan Plateau. The "Book of Guizhou" records that "it tastes sweet and slightly sour, and can relieve stuffiness and eliminate stagnation." The "Supplement to Compendium of Materia Medica" states that "the roots, stems, leaves, fruits, and seeds of Rosa roxburghii can all be used as medicine, with stomachic, digestive, and nourishing properties, and the root bark has antidiarrheal properties." The "Guiyang Prefecture Chronicle" states that "wine made from Rosa roxburghii mixed with glutinous rice is sweet and helps with digestion." Recent research has revealed that Rosa roxburghii is rich in various nutrients and functional substances, including vitamin C, superoxide dismutase (SOD), flavonoids, and triterpenes, and possesses high nutritional and medicinal value.

[0004] Currently, commercialized sea buckthorn extracts typically use fresh sea buckthorn fruit as raw material, using extraction or adsorption separation to separate the natural VC present in them. The maximum VC content is 17%. Therefore, current sea buckthorn extracts have the following two defects: First, the main specification for VC content is 6%, with the highest specification being 17%. There are no sea buckthorn extract products with a VC content exceeding 40%. Second, due to lax production and processing controls and the oxidative properties of VC, the color of marketed products is too dark, mostly light brown. Third, sea buckthorn is rich in small molecules of secondary metabolites, and marketed products do not undergo special separation of impurities that affect taste, resulting in a poor taste and a strong sour and astringent flavor, which presents significant difficulties in back-end product application. The above three defects pose significant difficulties for the production and large-scale application of sea buckthorn products, and they urgently need to be resolved through breakthroughs in process technology.

[0005] Summary of the Invention

[0006] The present invention provides a method for preparing a high-purity natural VC (vitamin C) extract from roxburghii roxburghii. The method uses roxburghii as raw material and, through cold pressing, enzymatic hydrolysis, desalination, decolorization, membrane separation, and drying, produces a roxburghii roxburghii extract product with a high purity (≥40%) VC content. The product produced by this process has the advantages of high VC content, pure flavor, and light color, significantly improving product quality, reducing application difficulty, and achieving a high yield, making it very suitable for industrial production.

[0007] The present invention aims to provide a method for preparing a high-purity natural VC roxburghii extract, comprising the following steps:

[0008] (1) Cold pressing: Frozen fresh roxburghii fruit is added with water and homogenized under a nitrogen atmosphere. After the homogenization, the temperature is controlled below 40°C for extraction to obtain the extracted liquid;

[0009] (2) Enzymolysis: adding a composite enzyme preparation to the extracted liquid, wherein the composite enzyme preparation is selected from one or more of pectinase, cellulase, tannase, protease and lipase, and the amount of the composite enzyme preparation added is 0.1% to 2% by mass of the extracted liquid, and performing enzymatic hydrolysis on the liquid to obtain an enzymatically hydrolyzed liquid;

[0010] (3) Solid-liquid separation: The enzymatically hydrolyzed liquid is subjected to solid-liquid separation to obtain a clear liquid and a residue that meet the turbidity requirements;

[0011] (4) Decolorization: The clear liquid obtained in step (3) is decolorized by an adsorbent, and the color index of the liquid is controlled by the specific absorbance index to obtain a decolorized liquid;

[0012] (5) Deodorization: Add an embedded deodorizing agent to the decolorized liquid, and control the sensory index of the liquid through sensory control to obtain a deodorized liquid;

[0013] (6) Membrane separation: The deodorized liquid passes through a polymer membrane filtration system with a specific molecular weight cut-off to intercept the target substance, and the permeate and retentate are collected separately;

[0014] (7) Drying: The retentate and the permeate are dried, and the dry powder is collected to obtain a high-purity natural VC roxburghii extract.

[0015] The decolorized liquid in step (4) is required to meet the Brix 5% and the absorbance at 370 nm is not more than 3. The sensory index of the liquid is specifically controlled by sensory control in step (5): the test method of the triangular sensory test is carried out, the number of participants is not less than 12, and the number of correct answers is not more than 4.

[0016] Preferably, the mass ratio of the fresh roxburghii fruit to water in step (1) is 1:1-5. The freezing temperature of the fresh roxburghii fruit is -18°C-0°C. Preferably, the homogenization treatment in step (1) comprises the following steps: using a homogenizing colloid mill to perform homogenization treatment, so that the fresh roxburghii fruit is crushed to a particle size of 0.1-5 mm.

[0017] Preferably, the complex enzyme preparation in step (2) is pectinase, cellulase, tannase, protease and lipase, and the mass ratio of pectinase, cellulase, tannase, protease and lipase is 1:1:1:0.1:0.1.

[0018] Preferably, the temperature of the enzymatic hydrolysis treatment in step (2) is 50° C.-55° C., and the time is 10-60 minutes.

[0019] In step (3), a plate and frame filter, a horizontal screw centrifuge, a disc centrifuge, etc. are used to separate the solid and liquid, and the turbidity of the clear liquid is ≤3NTU, and there is no precipitate, suspended matter, or other impurities visible to the naked eye.

[0020] Preferably, the adsorbent in step (4) is activated carbon and / or diatomaceous earth, and the amount of the adsorbent added is 0.1%-1% by mass of the clear liquid.

[0021] Preferably, the embedding deodorizing agent in step (5) is cyclodextrin, and the amount of the embedding deodorizing agent added is 1.5%-3.0% by mass of the decolorized liquid.

[0022] Preferably, the specification of the polymer membrane filtration system in step (6) is 0.1-10KDa.

[0023] Preferably, the drying in step (7) is spray drying, with an air inlet temperature of 180°C-200°C and an air outlet temperature of 90°C-100°C.

[0024] The present invention also protects the roxburghii roxburghii extract obtained by the preparation method, wherein the vitamin C content of the roxburghii ... extract is greater than or equal to 40%.

[0025] Compared with the prior art, the present invention has the following beneficial effects:

[0026] 1. The preparation method proposed in the present invention uses roxburghii as raw material and prepares a roxburghii extract product with high purity (≥40%) VC content and sensory-friendly flavor through cold pressing, enzymatic hydrolysis, desalting, decolorization, deodorization, membrane separation, drying and other processes.

[0027] 2. The product prepared by the preparation method proposed in the present invention has the advantages of high content, friendly sensory flavor, and light color, which greatly improves the product quality, reduces the application difficulty, has a high yield, and is very suitable for industrial production. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] Figure 1 is a comparison of the appearance of the roxburghii powder prepared in Example 1 and commercially available roxburghii powder, wherein the top: the roxburghii powder prepared in Comparative Example 1; the middle: the roxburghii powder prepared in Comparative Example 2; and the bottom: the roxburghii powder prepared in Example 1. DETAILED DESCRIPTION

[0029] The present invention is described in further detail below with reference to the examples. These examples are only used to illustrate the present invention and are not intended to limit the scope of the invention. The experimental methods in the following examples where specific conditions are not specified are generally carried out in accordance with conventional conditions in the art or in accordance with the conditions recommended by the manufacturer; the raw materials, reagents, etc. used, unless otherwise specified, are deemed to be raw materials and reagents that can be obtained through commercial channels such as conventional markets. Any non-substantial changes and substitutions made by those skilled in the art on the basis of the present invention fall within the scope of protection claimed by the present invention. The specifications of the polymer membrane filtration system (nanofiltration membrane separation system) in the following examples are 0.1-10KDa. The freezing temperature of fresh sea buckthorn fruit is -18℃-0℃.

[0030] Example 1

[0031] 1000g of jelly sea buckthorn fruit is taken, 5L of purified water is added, and the mixture is homogenized by a colloid mill to crush the fresh sea buckthorn fruit to a particle size of 0.1-5mm. After the homogenization treatment is completed, the temperature is controlled below 40°C for extraction to obtain an extracted liquid. The extracted liquid is subjected to enzymatic hydrolysis, and a composite enzyme preparation (pectinase, cellulase, tannase, protease, and lipase in a mass ratio of 1:1:1:0.1:0.1) is added to the liquid, and the liquid is kept at 55°C for 30 minutes for enzymatic hydrolysis to obtain an enzymatically hydrolyzed liquid. The enzymatically hydrolyzed liquid is centrifuged in a disc centrifuge to obtain a supernatant and a residue that meet turbidity requirements. Activated carbon is added to the supernatant for decolorization, and the amount of activated carbon added is 0.5% by mass of the supernatant. β-cyclodextrin is added to the decolorized liquid for deodorization, and the amount of β-cyclodextrin added is 3.0% by mass of the decolorized liquid to obtain a deodorized liquid. The liquid is then passed through a nanofiltration membrane separation system, and the retentate and the permeate are spray-dried separately, with an inlet air temperature of 180°C and an outlet air temperature of 90°C. The spray-dried roxburghii extract powder has a VC content of up to 41.9% and is light yellow in color.

[0032] Comparative Example 1

[0033] 1000 g of jelly fruit of sea buckthorn was taken, 5 L of purified water was added, and the mixture was mixed and crushed to reduce the particle size of the jelly fruit of sea buckthorn to 0.1-5 mm. The jelly fruit was centrifuged to remove coarse residue, and the supernatant was transferred to a vacuum concentrator for concentration until the density of the concentrate reached 1 g / mL. The concentrate was spray-dried at an inlet air temperature of 180° C. and an outlet air temperature of 90° C. to obtain a light yellow powder with a VC content of 6.5%.

[0034] Comparative Example 2

[0035] 1000 g of jelly roxburghii fruit is taken, added with 5 L of purified water, mixed, and homogenized by a colloid mill to crush the roxburghii fruit to a particle size of 0.1-5 mm. After the homogenization treatment is completed, the temperature is controlled to be below 40 DEG C to perform extraction to obtain an extracted liquid. The extracted liquid is subjected to enzymolysis, and 0.1% of a composite enzyme preparation (pectinase: cellulase: tannase: protease: lipase = 1:1:1:0.1:0.1) based on the mass percentage of the liquid is added to the liquid. The liquid is kept warm at 55 DEG C for 30 minutes to perform an enzymolysis reaction to obtain an enzymolyzed liquid. The liquid is centrifuged by a disc centrifuge to obtain a supernatant and a residue that meet turbidity requirements. Activated carbon was added to the supernatant for decolorization, and the amount of activated carbon added was 0.5% of the mass percentage of the supernatant. The decolorized liquid was concentrated under reduced pressure, and the density of the concentrated liquid reached 1 g / mL. It was then spray-dried with an inlet air temperature of 180°C and an outlet air temperature of 90°C. The VC content of the sea buckthorn extract powder after spraying was 17.7%, and the yellow powder was dark in color.

[0036] As shown in FIG1 , the roxburghii roxburghii extract powder obtained in Comparative Example 1 is light yellow and slightly darker in color, the roxburghii roxburghii extract powder obtained in Comparative Example 2 is darker in yellow, and the roxburghii roxburghii extract powder obtained in Example 1 is light yellow.

[0037] Comparative Example 3

[0038] The method is the same as Example 1, except that the extracted liquid is subjected to enzymatic hydrolysis, 0.1% of the mass percentage of the extracted liquid pectinase is added to the extracted liquid, and spray drying is performed to obtain a light yellow powder with a VC content of 11.9%.

[0039] Comparative Example 4

[0040] The same as Example 1, except that: the extracted liquid was subjected to enzymatic hydrolysis, 0.1% of the mass percentage of the extracted liquid was added to the extracted liquid, and light yellow powder was obtained by spray drying with a VC content of 8.6%.

[0041] Comparative Example 5

[0042] The method is the same as Example 1, except that the extracted liquid is subjected to enzymatic hydrolysis, 0.1% of tannase by weight of the extracted liquid is added to the extracted liquid, and spray drying is performed to obtain a light yellow powder with a VC content of 6.9%.

[0043] Comparative Example 6

[0044] The same as Example 1, except that: the extracted liquid was subjected to enzymatic hydrolysis, and 0.1% of the mass percentage of the extracted liquid of protease and lipase (the mass ratio of protease to lipase was 1:1) was added to the extracted liquid. Spray drying gave a light yellow powder with a VC content of 7.3.

[0045] Comparative Example 7

[0046] The same method as Example 1, except that the extracted liquid was subjected to enzymatic hydrolysis, and 0.1% of the mass percentage of the extracted liquid, pectinase, cellulase, and tannase (the mass ratio of pectinase, cellulase, and tannase was 1:1:1) was added to the extracted liquid. Spray drying gave a light yellow powder with a VC content of 7.3%.

[0047] Comparative Example 8

[0048] The same as Example 1, except that: the extracted liquid was subjected to enzymatic hydrolysis, and 0.1% of the mass percentage of the extracted liquid, pectinase, protease and lipase were added to the extracted liquid (the mass ratio of pectinase, protease and lipase was 1:0.1:0.1). Spray drying gave a light yellow powder with a VC content of 15.8%.

[0049] Comparative Example 9

[0050] The same as Example 1, except that: the extracted liquid was subjected to enzymatic hydrolysis, and 0.1% of the mass percentage of the extracted liquid of cellulase, protease and lipase (the mass ratio of cellulase, protease and lipase was 1:0.1:0.1) was added to the extracted liquid. Spray drying gave a light yellow powder with a VC content of 14.9%.

[0051] Comparative Example 10

[0052] The same as Example 1, except that: the extracted liquid was subjected to enzymatic hydrolysis, and 0.1% of tannase, protease and lipase (the mass ratio of tannase, protease and lipase was 1:0.1:0.1) were added to the extracted liquid. Spray drying gave a light yellow powder with a VC content of 9.0%.

[0053] Example 2

[0054] The same as Example 1, except that the mass ratio of fresh roxburghii fruit to water was 1:1, the complex enzyme preparation was pectinase and cellulase in a mass ratio of 1:1, the addition amount of the complex enzyme preparation was 0.1% by mass of the clear solution, the reaction temperature of the enzymatic hydrolysis reaction was 50°C, the reaction time was 60 minutes, the adsorbent was diatomaceous earth, and the addition amount of the adsorbent was 0.1% by mass of the enzymatic hydrolysis solution. The spray drying air inlet temperature was 180°C, and the air outlet temperature was 90°C. Spray drying obtained a light yellow powder with a VC content of 15.5%.

[0055] Example 3

[0056] The same method as Example 1, except that the mass ratio of fresh roxburghii fruit to water was 1:5, the complex enzyme preparation comprised pectinase and tannase in a mass ratio of 1:1, and the amount of the complex enzyme preparation added was 2% by mass of the clear solution. The reaction temperature of the enzymatic hydrolysis reaction was 55°C, the reaction time was 10 minutes, and the adsorbent was diatomaceous earth, and the amount of the adsorbent added was 1% by mass of the enzymatic hydrolysis solution. The spray drying air inlet temperature was 200°C, and the air outlet temperature was 100°C. Spray drying yielded a light yellow powder with a VC content of 12.3%.

[0057] Example 4

[0058] The same as Example 1, except that the mass ratio of fresh roxburghii fruit to water was 1:5, the complex enzyme preparation comprised cellulase and tannase in a mass ratio of 1:1, and the amount of the complex enzyme preparation added was 1% by mass of the clear solution. The reaction temperature of the enzymatic hydrolysis reaction was 52°C, the reaction time was 30 minutes, the adsorbent was diatomaceous earth, and the amount of the adsorbent added was 0.5% by mass of the enzymatic hydrolysis solution. The spray drying air inlet temperature was 190°C, and the air outlet temperature was 100°C. Spray drying yielded a light yellow powder with a VC content of 11.1%.

[0059] The above are merely preferred embodiments of the present invention. It should be noted that the above preferred embodiments should not be construed as limiting the present invention, and the scope of protection of the present invention should be determined by the scope defined in the claims. Persons skilled in the art will appreciate that improvements and modifications may be made without departing from the spirit and scope of the present invention, and such improvements and modifications should also be considered within the scope of protection of the present invention.

Claims

1. A method for preparing a high-purity natural VC roxburghii extract, characterized in that: The steps include: (1) Cold pressing: Frozen fresh roxburghii fruit is added with water and homogenized under a nitrogen atmosphere. After the homogenization, the temperature is controlled below 40° C. to extract the extracted liquid; (2) enzymolysis: adding a composite enzyme preparation to the extracted liquid, wherein the composite enzyme preparation is selected from one or more of pectinase, cellulase, tannase, protease and lipase, and the amount of the composite enzyme preparation added is 0.1% to 2% of the mass percentage of the extracted liquid, and performing enzymolysis treatment on the liquid to obtain an enzymolyzed liquid; (3) solid-liquid separation: solid-liquid separation of the enzymatically hydrolyzed liquid to obtain a clear liquid and a residue that meet the turbidity requirements; (4) Decolorization: The clear liquid obtained in step (3) is decolorized by an adsorbent, and the decolorized liquid is obtained by controlling the color index of the liquid; (5) Deodorization: Adding an embedded deodorizing agent to the decolorized liquid, and obtaining a deodorized liquid by controlling the sensory indexes of the liquid; (6) Membrane separation: The deodorized liquid is filtered through a polymer membrane filtration system with a specific molecular weight cut-off to intercept the target substance, and the permeate and retentate are collected separately; (7) Drying: The retentate and permeate are dried separately and the dry powder is collected.

2. The preparation method according to claim 1, characterized in that: The mass ratio of the fresh roxburghii fruit to water in step (1) is 1:1-5.

3. The preparation method according to claim 1 or 2, characterized in that: The specific steps of the homogenization treatment in step (1) are: using a homogenizing colloid mill to perform homogenization treatment, so that the fresh roxburghii fruit is crushed to a particle size of 0.1-5 mm.

4. The preparation method according to claim 1, characterized in that: The composite enzyme preparation described in step (2) is pectinase, cellulase, tannase, protease and lipase, and the mass ratio of pectinase, cellulase, tannase, protease and lipase is 1:1:1:0.1:0.

1.

5. The preparation method according to claim 1 or 2, characterized in that: The temperature of the enzymatic hydrolysis treatment in step (2) is 50°C-55°C and the time is 10-60 minutes.

6. The preparation method according to claim 1 or 2, characterized in that: The adsorbent described in step (4) is activated carbon and / or diatomaceous earth, and the amount of the adsorbent added is 0.1%-1% by mass of the clear liquid.

7. The preparation method according to claim 1 or 2, characterized in that: The embedding deodorizing agent described in step (5) is cyclodextrin, and the added amount of the embedding deodorizing agent is 1.5%-3.0% of the mass percentage of the decolorized liquid.

8. The preparation method according to claim 1 or 2, characterized in that: The specification of the polymer membrane filtration system described in step (6) is 0.1-10KDa.

9. The preparation method according to claim 1 or 2, characterized in that: The drying described in step (7) is specifically spray drying, with an air inlet temperature of 180°C-200°C and an air outlet temperature of 90°C-100°C.

10. The roxburghii roxburghii extract obtained by the preparation method according to claim 1 or 2, characterized in that: The vitamin C content of the roxburghii extract is ≥40%.

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