Preparation method and application of deodorized beet red
By centrifugation, fermentation, adsorption and microencapsulation of red beets, the finished product of deodorized beet red was prepared, which solved the problem of poor stability of beet red beet red, achieved high purity and stability of beet red, extended storage time, and no adverse odor.
Patent Information
- Application Number
- CN202411661187.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-20
- Publication Date
- 2025-02-25
AI Technical Summary
Beet red beet is poor in its stability in response to different situations such as light, heat, oxygen, pH changes, enzymes, and metal ions, resulting in yellowing and fading, limiting its application. The prior art methods for improving stability are complex and have poor results.
The red beet was peeled and crushed and centrifuged, and fermented with sugar and bacterial solution. Adhesive and remove impurities with macroporous adsorption resin, and then analyzed by ethanol solution and concentrated in nanofiltration membrane. Finally, microencapsulation treatment was performed to prepare the finished beet red product of deodorized beet.
It improves the purity and stability of beet red, extends its storage time, and has no adverse odor, increases color price and stable properties.
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Abstract
Description
Technical Field
[0001] The invention relates to the field of beetroot red preparation, in particular to a preparation method of deodorized beetroot red and application thereof. Background Art
[0002] Betanin, also known as beetroot red, is a natural pigment made from edible red beets through extraction, separation, concentration and drying. Its main components are betacyanins and betacyanins. It is a safe, brightly colored water-soluble natural food pigment that is red to purple-red in color and has good coloring ability, antioxidant and free radical scavenging functions. Betanin is a pigment derived from heterocyclic tyrosine, and the phenolic hydroxyl and cyclic amine parts make this type of compound reductive. In in vitro experiments, betanin showed antioxidant ability in both inorganic and organic systems, and had a good effect in inhibiting the oxidation of low-density lipoprotein. It has the effects of promoting the immune system, chemotherapy of cancer, and prevention of cardiovascular diseases and neurodegenerative diseases. Therefore, betanin can be used in the food, pharmaceutical and cosmetic industries. However, betalain is a highly environmentally sensitive pigment. It has poor stability in response to different situations such as light, heat, oxygen, pH changes, enzymes, and metal ions. It is prone to adverse reactions such as isomerization, dehydrogenation, decarboxylation, degradation, and oxidation, which manifests as yellowing and fading, limiting the application of betalain. At present, the method of improving the stability of betalain in the prior art is to start from the molecular structure of betalain, graft new groups on the pigment molecules through reactions such as glycosylation, acylation, and methylation, and change the structure and properties of the pigment. However, due to the complexity and instability of betalain components, glycosylation and acylation have the defects of complex operating procedures and unsatisfactory effects. Betalain is prepared using soybean lecithin and cholesterol as wall materials, and its stability is enhanced by embedding and encapsulation technology. Adding stabilizers to improve the color stability of pigments, protein fibers can be used as protective agents to improve the stability of betalain and reduce its degradation rate. However, whether it is synthesizing new products or preparing encapsulation systems, there are problems such as complex preparation processes, long time, and high costs. At the same time, betalain has poor stability, resulting in a short shelf life. The low purity and earthy smell of betalain currently available in the domestic market also limits its scope of application. Summary of the invention
[0003] In view of this, the present invention provides a preparation method of deodorized betaine and application thereof to solve the above problems.
[0004] The technical solution of the present invention is achieved in this way:
[0005] A method for preparing deodorized beetroot red comprises the following steps:
[0006] S1. Wash and peel the red beets, crush them, add water, separate them, and take the clear liquid;
[0007] S2, adding sugar to the separated red beet clear liquid, mixing and stirring, standing, adding the cultured bacterial liquid, mixing and stirring, fermenting, and obtaining fermented red beet slurry;
[0008] S3, using a macroporous adsorption resin to adsorb and remove impurities from the fermented red beet pulp, and then using an ethanol solution to resolve it to obtain a chromatographic solution, and concentrating and sterilizing the chromatographic solution through a nanofiltration membrane to obtain a deodorized beet red concentrate;
[0009] S4. Microencapsulate the beetroot red concentrate, add β-cyclodextrin, protein powder and maltodextrin to the deodorized beetroot red concentrate, adjust the pH value, homogenize, and dry by spray drying to obtain a deodorized beetroot red finished product.
[0010] Furthermore, in step S1, the centrifugal separation is performed by a disc separator, the separation speed is 5000-7000 rpm, the temperature is 15°C-35°C, the pressure is 0.8-1.0 MPa, and the mass of the added water is 4-5 times the weight of the red beet.
[0011] Further, in step S2, the bacterial liquid is composed of Bacillus subtilis and Candida oliveri in a mass ratio of 4-5:2-3, the fermentation temperature is 26-30°C, the fermentation pH is 4-6, and the fermentation time is 36-48h.
[0012] Furthermore, in step S2, the sugar is sucrose or brown sugar, the volume mass ratio of the clear liquid to the sugar is 30-40 mL:3-5 g, and the amount of the bacterial liquid added is 5%-10% of the volume of the mixed liquid.
[0013] Further, in step S3, the macroporous adsorption resin has a specific surface area of 1000-1200m 2 / g, the pore volume is 0.8-1.1mL / g, the mass fraction of the ethanol is 45-55%, the red beet concentrate is sterilized by pasteurization, the sterilization temperature is 62-65°C, and the time is 30-32min;
[0014] Furthermore, in step S4, the buffer solution for adjusting the pH value is one of a citric acid-sodium citrate solution or a sodium dihydrogen phosphate-citric acid solution, and the pH value adjustment range is 4-6.
[0015] Furthermore, in step S4, the spray drying has an air inlet temperature of 170-180°C and an air outlet temperature of 70-75°C.
[0016] Furthermore, in step S4, the mass ratio of the deodorized beetroot red concentrate, β-cyclodextrin, protein powder and maltodextrin is 70-90:6-10:5-8:2-3, and the protein powder is one of whey protein, ovalbumin and casein phosphopeptide.
[0017] Furthermore, in step S4, the particle size of the microcapsule particles is 100-150 μm, and the capsule wall is 2-10 μm.
[0018] Compared with the prior art, the present invention has the following beneficial effects:
[0019] According to the production steps of the present invention, the red beet is peeled, crushed and centrifuged, sugar and bacterial liquid are added for fermentation to obtain fermented red beet slurry, impurities are removed by adsorption with macroporous adsorption resin, ethanol solution is used for analysis, concentration is carried out through nanofiltration membrane, and sterilization is carried out to obtain deodorized beet red concentrated liquid. According to the production steps of the present invention, after adding sugar, the fermented red beet slurry is obtained by adding bacterial liquid for fermentation, so that the color value of the finished beet red product is increased; the impurities are removed by adsorption with macroporous adsorption resin, ethanol solution is used for analysis, and the production steps of concentration and sterilization through nanofiltration membrane are used to increase the impurity filtration amount, improve the purity of beet red, and the beet red concentrated liquid is microencapsulated again to increase the stability of beet red. The preparation method of the deodorized beet red of the present invention is simple, the color value of the finished beet red product is increased, and the properties are stable without irritating bad taste. DETAILED DESCRIPTION
[0020] In order to better understand the technical content of the present invention, specific embodiments are provided below to further illustrate the present invention.
[0021] Unless otherwise specified, the experimental methods used in the examples of the present invention are all conventional methods, and the reagents used in the examples are all available from commercial sources.
[0022] Bacillus subtilis, effective viable count greater than 1.5x10 6 cfu / g, moisture content less than 2.5%, manufacturer: Guangzhou Weiyuan Biotechnology Co., Ltd.; Candida oleophila, item number RN-67767, viable count greater than 2.0x10 6 cfu / g, the manufacturer is Noan Gene Technology (Wuhan) Co., Ltd.
[0023] Example 1
[0024] The preparation of deodorized beetroot red comprises the following steps:
[0025] Step (1): Wash and peel the red beets, crush them, add purified water 4 times the weight of the red beets, and perform disc centrifugal separation after adding water. The separation speed is 5000 rpm, the temperature is 15° C., and the pressure is 0.8 MPa. After separation, the clear liquid is collected;
[0026] Step (2): Add sucrose to the clear liquid of step (1) to obtain a mixed liquid, wherein the volume mass ratio of the clear liquid to the sucrose is 30 mL:3 g, and after stirring and standing after adding the sucrose, add 5% of the volume of the mixed liquid with a bacterial solution, wherein the bacterial solution is composed of Bacillus subtilis and Candida olive in a mass ratio of 5:2, the bacterial solution fermentation temperature is 26°C, the fermentation pH value is 4, and the fermentation time is 36 hours. Stir the above mixed liquid to obtain fermented red beet slurry;
[0027] Step (3): Fermented red beet pulp was placed in a 2 / g, a macroporous adsorption resin with a pore volume of 0.8mL / g was used for adsorption and impurity removal, and then a 45% ethanol solution was used for analysis to obtain a chromatographic solution, and the chromatographic solution was concentrated by a nanofiltration membrane and sterilized by pasteurization at a temperature of 62°C for 30min to obtain a deodorized beetroot red concentrate;
[0028] Step (4): microencapsulate the beetroot red concentrate, add β-cyclodextrin, whey protein and maltodextrin to the deodorized beetroot red concentrate, the mass ratio of beetroot red concentrate, β-cyclodextrin, whey protein and maltodextrin is 70:6:5:2, adjust the pH value with citric acid-sodium citrate buffer solution to pH 4, homogenize, and dry by spray drying, the air inlet temperature is 170°C, and the air outlet temperature is 70°C. The beetroot red microcapsule particles prepared by the above method have a particle size of 110±10μm and a capsule wall of 5±1μm.
[0029] Example 2
[0030] The preparation of deodorized beetroot red comprises the following steps:
[0031] Step (1): Wash and peel the red beets, crush them, add purified water 5 times the weight of the red beets, perform disc centrifugation after adding water, the separation speed is 7000 rpm, the temperature is 35° C., the pressure is 1.0 MPa, and take the clear liquid;
[0032] Step (2): adding brown sugar to the clear liquid to obtain a mixed liquid, wherein the volume mass ratio of the clear liquid to the brown sugar is 40 mL:5 g, stirring and standing after adding the brown sugar, adding the cultured bacterial liquid, wherein the amount of the bacterial liquid added is 10% of the volume of the mixed liquid, the bacterial liquid is composed of Bacillus subtilis and Candida olivelis in a mass ratio of 4:3, the bacterial liquid fermentation temperature is 30° C., the fermentation pH value is 6, the fermentation time is 48 hours, and the above mixed liquid is stirred to obtain fermented red beet slurry;
[0033] Step (3): The fermented red beet pulp is heated to 1200 m 2 / g, a macroporous adsorption resin with a pore volume of 1.1mL / g was used for adsorption and impurity removal, and then a chromatographic liquid was obtained by analysis with a mass fraction of 55% ethanol solution, and the chromatographic liquid was concentrated and sterilized through a nanofiltration membrane. The sterilization method was pasteurization, the sterilization temperature was 65℃, and the time was 32min. After sterilization, a deodorized beet red concentrate was obtained;
[0034] Step (4): microencapsulating the beetroot red concentrate, adding β-cyclodextrin, ovalbumin and maltodextrin to the deodorized beetroot red concentrate, wherein the mass ratio of the beetroot red concentrate, β-cyclodextrin, ovalbumin and maltodextrin is 90:10:8:3, adjusting the pH value to 6 with sodium dihydrogen phosphate-citric acid buffer solution, homogenizing, and drying by spray drying, wherein the air inlet temperature is 180° C. and the air outlet temperature is 75° C., and the obtained beetroot red microcapsule particles have a particle size of 120±15 μm and a capsule wall of 7±1.5 μm.
[0035] Example 3
[0036] The preparation of deodorized beetroot red comprises the following steps:
[0037] Step (1): Wash and peel the red beets, crush them, add 4.5 times the weight of the red beets of purified water, and perform disc centrifugation after adding the purified water. The separation speed is 6000 rpm, the temperature is 25° C., and the pressure is 1.0 MPa, and the clear liquid is collected;
[0038] Step (2): add sucrose to the clear liquid to obtain a mixed liquid, the volume mass ratio of the clear liquid to sucrose is 35mL:4g, after adding sucrose, stir and stand, add the cultured bacterial liquid, the amount of the bacterial liquid added is 7% of the volume of the mixed liquid, the bacterial liquid is composed of Bacillus subtilis and Candida olive in a mass ratio of 4.5:3, the bacterial liquid fermentation temperature is 28°C, the fermentation pH value is 5, and the fermentation time is 40h. Stir the above mixed liquid to obtain fermented red beet slurry;
[0039] Step (3): The fermented red beet pulp is adsorbed and impurities are removed by macroporous adsorption resin, and the specific surface area of the macroporous adsorption resin is 1100m 2 / g, pore volume of 1.0mL / g, and then 50% ethanol solution was used for analysis to obtain a chromatographic solution, and the chromatographic solution was concentrated by a nanofiltration membrane and sterilized by pasteurization at a temperature of 64°C for 31min to obtain a deodorized beetroot red concentrate;
[0040] Step (4): microencapsulate the beetroot red concentrate, add β-cyclodextrin, casein phosphopeptide and maltodextrin to the deodorized beetroot red concentrate, and the mass ratio of beetroot red concentrate, β-cyclodextrin, casein phosphopeptide and maltodextrin is 80:9:7:2. Use citric acid-sodium citrate buffer solution to adjust the pH value to 5, homogenize, and dry by spray drying. The air inlet temperature during drying is 175°C and the air outlet temperature is 73°C. The beetroot red microcapsule particles prepared by the above method have a particle size of 120±15μmμm and a capsule wall of 6±1.5μm.
[0041] Comparative Example 1
[0042] The main difference between Comparative Example 1 and Example 3 is that the bacterial liquid fermentation step is removed in step (2), and the other steps remain unchanged.
[0043] Step (2): Add sucrose to the clear liquid to obtain a mixed liquid, wherein the volume mass ratio of the clear liquid to sucrose is 35 mL:4 g. After adding the sucrose, stir and let stand, then stir to obtain fermented red beet slurry.
[0044] Comparative Example 2
[0045] The main difference between Comparative Example 2 and Example 3 is that the macroporous adsorption resin adsorption step is removed in step (3), the nanofiltration membrane concentration is changed to heating evaporation concentration, and the other steps remain unchanged.
[0046] Step (3): The fermented red beet pulp is resolved with a 50% ethanol solution to obtain a chromatographic solution, the chromatographic solution is heated and concentrated, and pasteurized at a temperature of 64° C. for 31 minutes to obtain a deodorized beet red concentrate.
[0047] Comparative Example 3
[0048] The main difference between Comparative Example 3 and Example 3 is that the microencapsulation treatment is removed in step (4), and the other steps remain unchanged.
[0049] Step (4): Dry the beet red concentrate by spray drying, with an air inlet temperature of 175° C. and an air outlet temperature of 73° C. during drying.
[0050] Comparison
[0051] Commercially available beetroot red was used, and the manufacturer was Henan Kangzhiwang Biotechnology Co., Ltd.
[0052] test
[0053] According to the method A.3 in Appendix A of GB 1886.111-2015 "Food Safety Standard Food Additive Beet Red", the color value of the beet red powder products prepared in Examples 1-3, Comparative Examples 1-3 and the control method was determined and calculated. The specific operation is to weigh 0.050g of beet red powder, dissolve it in pH 5.4 acetic acid-sodium acetate buffer to 100mL, draw 5ml of sample solution, and make it to 100mL, use a spectrophotometer, pH 5.4 acetic acid-sodium acetate buffer as a reference solution, measure its absorbance at 535nm in a 1cm cuvette, and then calculate the color value.
[0054] According to formula E 1%1cm535nm =A×f / (100×m), A is the absorbance of the actual test sample, f is the dilution factor, m is the sample mass, the calculation results are shown in Table 1, and the proportion of the residual amount of betaine in the photostability determination is shown in Table 2.
[0055] Table 1
[0056]
[0057]
[0058] Table 2
[0059]
[0060] The beetroot red prepared by Examples 1-3, Comparative Examples 1-3 and the control method was subjected to odor measurement by smell test scoring. 70 people with normal taste (random gender) were randomly selected, 10 people in each group, and divided into 7 groups to score the odor of beetroot red. The comprehensive scoring standard is shown in Table 3, and the scoring results are shown in Table 4.
[0061] Table 3
[0062] score 10-30 minutes 40-60 points 70-100 points odor There is a strong odor, bad smell Slightly peculiar smell, general smell No obvious odor
[0063] The odor measurement results of beetroot red prepared by Examples 1-3, Comparative Examples 1-3 and the control method show that the average odor score range of beetroot red prepared by the method of Examples 1-2 is 92-95 points, which is higher than that of Comparative Examples 1-3 and the control, indicating that the beetroot red prepared by the method of the present invention has no odor and no other unpleasant odor.
[0064] Table 4
[0065]
[0066]
[0067] In summary, the present invention peels and crushes red beets and then centrifuges them, adds sugar and cultured bacterial liquid for fermentation, adsorbs and removes impurities from the fermented red beet pulp with a macroporous adsorption resin, and then analyzes with an ethanol solution, concentrates through a nanofiltration membrane, and sterilizes to obtain a deodorized beet red concentrate. The color value of the deodorized beet red finished product prepared by the method increases, the remaining amount of deodorized beet red after 8 hours is greater than 90%, the stability of beet red increases, and there is no bad smell. After the bacterial liquid fermentation step is removed in Comparative Example 1, the stability of beet red decreases. After Comparative Example 2 removes the macroporous adsorption resin adsorption step and the nanofiltration membrane concentration is modified to the heating evaporation concentration step, the color value of the beet red finished product decreases, and the remaining amount of beet red decreases to less than 90%, that is, the amount of beet red decomposition increases, indicating that the instability of beet red is increased. After the microencapsulation treatment is removed in Comparative Example 3, the smell of the beet red finished product is poor and the stability is reduced. Therefore, the color value of the beet red finished product prepared by the method of the present invention increases, and the properties are stable and there is no bad smell.
[0068] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.
Claims
1. A method for preparing deodorized betaine, characterized in that: The following steps are involved: S1. Wash and peel the red beets, crush them, add water, separate them, and take the clear liquid; S2, adding sugar to the separated red beet clear liquid, mixing and stirring, standing, adding the cultured bacterial liquid, mixing and stirring, fermenting, and obtaining fermented red beet slurry; S3, using a macroporous adsorption resin to adsorb and remove impurities from the fermented red beet pulp, and then using an ethanol solution to resolve it to obtain a chromatographic solution, and concentrating and sterilizing the chromatographic solution through a nanofiltration membrane to obtain a deodorized beet red concentrate; S4. Microencapsulate the beetroot red concentrate, add β-cyclodextrin, protein powder and maltodextrin to the deodorized beetroot red concentrate, adjust the pH value, homogenize, and dry by spray drying to obtain a deodorized beetroot red finished product.
2. The method for preparing deodorized betaine according to claim 1, characterized in that: Step S1, the centrifugal separation is performed by a disc separator, the separation speed is 5000-7000 rpm, the temperature is 15°C-35°C, the pressure is 0.8-1.0 MPa, and the mass of the added water is 4-5 times the weight of the red beet.
3. The method for preparing deodorized betaine according to claim 1, characterized in that: Step S2, the bacterial liquid is composed of Bacillus subtilis and Candida oliveri in a mass ratio of 4-5:2-3, the fermentation temperature is 26-30°C, the fermentation pH value is 4-6, and the fermentation time is 36-48h.
4. The method for preparing deodorized betaine according to claim 1, characterized in that: Step S2, the sugar is sucrose or brown sugar, the volume mass ratio of the clear liquid to the sugar is 30-40 mL:3-5 g, and the amount of the bacterial liquid added is 5%-10% of the volume of the mixed liquid.
5. The method for preparing deodorized betaine according to claim 1, characterized in that: Step S3, the macroporous adsorption resin has a specific surface area of 1000-1200m 2 / g, the pore volume is 0.8-1.1mL / g, the mass fraction of the ethanol is 45-55%, the red beet concentrate is sterilized by pasteurization, the sterilization temperature is 62-65°C, and the time is 30-32min.
6. The method for preparing deodorized betaine according to claim 1, characterized in that: Step S4, the buffer solution for adjusting the pH value is one of a citric acid-sodium citrate solution or a sodium dihydrogen phosphate-citric acid solution, and the pH value adjustment range is 4-6.
7. The method for preparing deodorized betaine according to claim 1, characterized in that: Step S4, the spray drying, the inlet air temperature is 170-180°C, and the outlet air temperature is 70-75°C.
8. The method for preparing deodorized betaine according to claim 1, characterized in that: Step S4, the mass ratio of the deodorized beetroot red concentrate, β-cyclodextrin, protein powder and maltodextrin is 70-90:6-10:5-8:2-3, and the protein powder is one of whey protein, ovalbumin and casein phosphopeptide.
9. The method for preparing deodorized betaine according to claim 1, characterized in that: Step S4, the particle size of the microcapsule particles is 100-150 μm, and the capsule wall is 2-10 μm.
10. Application of betalain pigment obtained by the preparation method according to any one of claims 1 to 9 in the fields of food, medicine and cosmetics.
Citation Information
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