CN113201078B - Preparation method and application of rice bran polysaccharide zinc chelate - Google Patents
Preparation method and application of rice bran polysaccharide zinc chelate Download PDFInfo
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- CN113201078B CN113201078B CN202110481443.7A CN202110481443A CN113201078B CN 113201078 B CN113201078 B CN 113201078B CN 202110481443 A CN202110481443 A CN 202110481443A CN 113201078 B CN113201078 B CN 113201078B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K20/00—Accessory food factors for animal feeding-stuffs
- A23K20/10—Organic substances
- A23K20/163—Sugars; Polysaccharides
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K20/00—Accessory food factors for animal feeding-stuffs
- A23K20/20—Inorganic substances, e.g. oligoelements
- A23K20/30—Oligoelements
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
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- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/16—Inorganic salts, minerals or trace elements
- A23L33/165—Complexes or chelates
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- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
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Abstract
The invention discloses a preparation method and application of rice bran polysaccharide zinc chelate, wherein a method for producing the polysaccharide zinc chelate by taking rice bran meal as a raw material is developed through the combination of a physical method and an enzyme method, the method has the characteristics of simple equipment and process, low cost, easiness in industrial large-scale production and application and the like, the high-purity rice bran polysaccharide can be obtained without adding a purification process, the prepared polysaccharide zinc chelate has high zinc content and obvious antioxidant effect, and the value-added utilization of the rice bran meal is realized at lower cost. The produced polysaccharide zinc chelate can be used as food additive, functional health product, feed additive and the like, and has good market prospect and social and environmental benefits.
Description
Technical Field
The invention relates to a preparation process of a polysaccharide zinc chelate with antioxidant activity, in particular to a preparation method and application of a rice bran polysaccharide zinc chelate.
Background
China is the main country of rice and rice bran resources are rich. The rice bran meal is a main byproduct of rice bran after oil extraction, is mainly used as animal feed at present, and has low product value. The rice bran polysaccharide is an important functional component in the rice bran meal, is heteroglycan with a complex structure, and has multiple effects of resisting oxidation, improving immunity, reducing blood sugar, reducing blood fat, resisting bacteria, resisting radiation, preserving freshness and the like. At present, the research on rice bran polysaccharide mostly focuses on the extraction and activity research of the polysaccharide, and the research on the related application of rice bran polysaccharide chelate is very little.
The invention patent CN107267571A of China's China in 2017 discloses an extraction method of rice bran polysaccharide, the preparation process of the polysaccharide comprises enzymolysis, primary extraction, secondary extraction, primary purification and secondary purification, the process is complex, and the yield of the polysaccharide can only reach 6.96%; the invention patent CN109608560A of China in 2019 discloses an extraction method of rice bran polysaccharide and a biscuit and a method for making the same. The polysaccharide preparation process comprises cellulase and protease enzymolysis and ultrasonic extraction, although the purity of the prepared polysaccharide is improved by 14 percent compared with that of the polysaccharide prepared in the patent CN107267571A, the polysaccharide yield is still 6.6 to 6.8 percent, and the ultrasonic technology has difficulty in industrial production and limits the application of the process.
The chelate of natural plant polysaccharide and metal ions is a novel high-efficiency nutrition enhancer widely applied clinically at present, the stable chelate is easily absorbed by small intestine mucous membrane cells, the stimulation of free metal ions to gastrointestinal mucous membranes can be reduced, and after the metal ions are released, the polysaccharide ligand can continuously exert the bioactivity function. Zinc, as one of the essential trace elements, is widely involved in processes such as energy metabolism, nucleic acid and protein synthesis, cellular and humoral immunity, and the like. The zinc deficiency of the body can cause the reduction of basal metabolism, the reduction of protein utilization rate, the low appetite and digestive function, the influence on growth and development and the like. Studies on polysaccharide-zinc chelates have been reported: 2014 Chinese national invention patent CN104031156A discloses prunella polysaccharide zinc chelate and its preparation method and application in anticancer drugs, but the chelate zinc content in the patent is only 1.5%; the invention patent CN109776694A of China's China in 2017 discloses a preparation method and application of copper, iron and zinc triple chelate of brown algae polysaccharide, wherein the content of the chelate zinc in the patent is increased to 8.5%; the invention relates to a water-soluble soybean polysaccharide zinc chelate of a zinc supplement agent, a preparation method and application thereof, and the national invention patent CN112048025A in 2020 discloses the water-soluble soybean polysaccharide zinc chelate of the zinc supplement agent, and the content of chelate zinc in the patent is only 2-3%. In conclusion, zinc chelation using rice bran polysaccharide as a ligand has not been reported, and there is a need to develop an organic chelating product having a higher zinc content.
Disclosure of Invention
The invention provides a preparation method of a rice bran polysaccharide zinc chelate compound capable of industrial production, which aims at the problem of low zinc content in the polysaccharide-zinc chelate compound, and has the advantages of high product yield, high polysaccharide content and high zinc ion content. On one hand, the problems of low yield, complex process and incapability of large-scale production in the preparation of the rice bran polysaccharide in the prior art are solved; on the other hand, an organic zinc chelate product which is easy to produce, low in cost, high in content and strong in antioxidant activity is developed.
The technical scheme adopted by the invention for solving the technical problem is as follows: a preparation method of rice bran polysaccharide zinc chelate comprises the following steps:
(1) Pretreatment of raw materials: crushing rice bran meal;
(2) Mixing materials: mixing rice bran meal with alpha-amylase and neutral protease;
(3) Hydraulic oscillation extraction: adding water into the mixed materials for proportioning, uniformly stirring, and performing oscillation treatment in hydraulic oscillation equipment;
(4) Enzymolysis: adjusting the pH value of the extraction mixture obtained in the step (3) to 4.5-5.5, respectively adding phytase, xylanase and cellulase, wherein the enzymolysis temperature is 45-55 ℃, and the enzymolysis time is 1.5-2.5 h;
(5) Enzyme deactivation: heating the enzymolysis mixed solution obtained in the step (4) to 90-100 ℃, and preserving the temperature for 5-10 min;
(6) Centrifuging: centrifuging the mixed solution after enzyme deactivation and collecting supernatant;
(7) Adding metal ions: adding zinc ion salt into the supernatant obtained in the step (6), wherein the mass ratio of the zinc ion to the rice bran meal raw material is (1-3): 100;
(8) Chelating: heating the polysaccharide extracting solution added with the metal salt to 60-80 ℃, stirring for 40-80 min, and after the chelation reaction is finished, concentrating the polysaccharide chelating solution at 70-85 ℃ under reduced pressure;
(9) Centrifuging: centrifuging the polysaccharide chelate concentrate and collecting the supernatant;
(10) Ethanol precipitation: adding absolute ethyl alcohol into the supernatant obtained in the step (9), and refrigerating at 4 ℃ for 8-12 h;
(11) Solid-liquid separation: precipitating the polysaccharide chelate concentrated clear solution with ethanol, layering, performing solid-liquid separation, and collecting precipitate;
(12) And (3) drying: and (4) drying the precipitate obtained in the step (11), crushing and sieving to obtain the rice bran polysaccharide zinc chelate.
Furthermore, the crushing granularity of the raw materials in the step (1) is 60-80 meshes.
Further, in the step (2), the addition amount of the alpha-amylase is 40-120U/g of the rice bran meal, and the addition amount of the neutral protease is 3000-5000U/g of the rice bran meal.
Further, the solid-liquid mass ratio in the step (3) is 1 (15-25), the hydraulic oscillation treatment time is 8-12 min, and the temperature is room temperature.
Further, the pH of the extraction mixture is adjusted with citric acid in the step (4).
Further, in the step (4), the adding amount of phytase is 120-180U/g rice bran meal, the adding amount of xylanase is 2000-4000U/g rice bran meal, and the adding amount of cellulase is 500-1000U/g rice bran meal.
Further, the centrifugation revolution number in the step (6) is 4000-5000 r/min, the centrifugation time is 5-10 min, the centrifugation revolution number in the step (9) is 4000-5000 r/min, and the centrifugation time is 10-20 min.
Further, the zinc ion salt in the step (7) is zinc chloride or zinc sulfate, and after enzymolysis and addition of metal salt, the pH value of the system is maintained at 4.0-6.0, and direct chelation can be performed.
Further, the ratio of the volume of the concentrated solution to the volume of the stock solution of the chelating solution in the step (8) is 1.
Further, the addition amount of the absolute ethyl alcohol in the step (10) is 2-4 times of the volume of the supernatant obtained in the step (9), the polysaccharide chelate concentrated supernatant is obviously layered after being precipitated by the ethyl alcohol, the precipitate is not aggregated and dispersed, and the polysaccharide zinc chelate exists in the precipitate.
Further, in the step (12), the drying temperature is 70-85 ℃, and the crushed materials are sieved by a 60-80-mesh sieve.
Further, the yield of the polysaccharide zinc chelate obtained in the step (12) is 10-16%, the polysaccharide content is 45-65%, and the zinc ion content is 8-15%.
The invention also provides application of the rice bran polysaccharide zinc chelate, and the rice bran polysaccharide zinc chelate prepared based on the preparation method is used for preparing any one of clinical medicines, health products, food additives and feed additives.
The method has the advantages that the cross-linking action between polysaccharide and protein, between polysaccharide and phytic acid, between phytic acid-protein-metal ions and between phytic acid and the protein can be broken by adopting the hydraulic oscillation technology and the enzymolysis treatment, so that the rice bran polysaccharide is greatly dissolved out in a short time, and a high-content organic zinc chelate product is produced by utilizing the strong chelation of the rice bran polysaccharide, and the method is simple in process, controllable in cost and remarkable in antioxidant activity.
When the hydraulic oscillation technology is used for extracting the rice bran polysaccharide, the processing time is strictly controlled, and the polysaccharide extraction rate is obviously reduced along with the prolonging of the processing time. Amylase is added while the hydraulic oscillation extraction is carried out, and the starch can be completely degraded even if the treatment time is short; the polysaccharide in the rice bran meal is crosslinked with phytic acid, cellulose, protein and the like, the polysaccharide can be further released under the combined action of phytase, xylanase and cellulase, and the content of the protein in a polysaccharide product can be obviously reduced under the combined action of hydraulic oscillation and protease, so that the yield and the purity of the product are improved.
The invention has the beneficial effects that:
the invention effectively combines the hydraulic oscillation technology and the enzymatic extraction, does not need a special purification process, can obviously improve the yield and the purity of the rice bran polysaccharide, and can directly carry out amplification production. The added zinc ions are effectively chelated in the polysaccharide by utilizing the super-strong chelating ability of the rice bran polysaccharide, and the chelated zinc ions are precipitated together with the polysaccharide through ethanol precipitation, so that the existing state of the zinc ions is changed from inorganic to organic. Finally provides a low-cost and high-content polysaccharide zinc chelate product. Before chelation, the yield of rice bran polysaccharide is more than 9%, and the purity of polysaccharide is more than 70%; after chelation, the polysaccharide zinc chelate yield is 10-16%, the polysaccharide content is 45-65%, and the zinc ion content is 8-15% with the change of the zinc ion addition.
Drawings
FIG. 1 shows the trend of the removal rate of DPPH free radicals by rice bran polysaccharides and rice bran polysaccharide zinc chelates;
FIG. 2 shows the variation of the OH radical scavenging rate of rice bran polysaccharides and rice bran polysaccharide zinc chelates.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and do not limit the invention.
Preparing rice bran polysaccharide zinc chelate:
example 1
(1) Crushing the rice bran meal, and sieving the crushed rice bran meal with a 60-mesh sieve;
(2) Weighing 2kg of sieved rice bran meal, and mixing with alpha-amylase and neutral protease, wherein the addition amount of the alpha-amylase is 40U/g of the rice bran meal, and the addition amount of the neutral protease is 3000U/g of the rice bran meal;
(3) Adding water into the mixed materials according to the solid-liquid mass ratio of 1;
(4) Adjusting the pH value of the extracted mixture to 5.5 by using citric acid, respectively adding phytase, xylanase and cellulase, carrying out enzymolysis at the temperature of 45 ℃ for 1.5h, wherein the addition amount of the phytase is 120U/g of rice bran meal, the addition amount of the xylanase is 2000U/g of rice bran meal, and the addition amount of the cellulase is 500U/g of rice bran meal;
(5) Heating the enzymolysis liquid to 100 deg.C, and keeping the temperature for 5min;
(6) Centrifuging the mixed solution after enzyme deactivation for 5min at the revolution of 4000r/min, and collecting supernatant;
(7) Adding zinc sulfate into the centrifugal supernatant, wherein the mass ratio of zinc ions to the raw material of the rice bran meal is 1;
(8) Heating the polysaccharide extracting solution added with the metal salt to 60 ℃, stirring for 40min, and after the reaction is finished, concentrating the chelating solution at 70 ℃ under reduced pressure, wherein the ratio of the volume of the concentrated solution to the volume of the stock solution is 1;
(9) Centrifuging the polysaccharide chelate concentrated solution at the revolution of 4000r/min for 10min, and collecting the supernatant;
(10) Adding anhydrous ethanol with the volume 4 times that of the polysaccharide chelate concentrated supernatant, and refrigerating at 4 ℃ for 8h;
(11) Pouring the refrigerated supernatant, and collecting the precipitate;
(12) And drying the precipitate at 70 ℃, crushing and sieving by a 60-mesh sieve to obtain the rice bran polysaccharide zinc chelate 1.
Example 2
(1) Crushing the rice bran meal, and sieving the crushed rice bran meal with a 80-mesh sieve;
(2) Weighing 2kg of sieved rice bran meal, and mixing with alpha-amylase and neutral protease, wherein the addition amount of the alpha-amylase is 80U/g of the rice bran meal, and the addition amount of the neutral protease is 4000U/g of the rice bran meal;
(3) Adding water into the mixed materials according to the solid-liquid mass ratio of 1;
(4) Adjusting the pH of the extracted mixture to 5.0 by using citric acid, respectively adding phytase, xylanase and cellulase, carrying out enzymolysis at 50 ℃ for 2.0h, wherein the addition amount of the phytase is 150U/g of rice bran meal, the addition amount of the xylanase is 3000U/g of rice bran meal, and the addition amount of the cellulase is 750U/g of rice bran meal;
(5) Heating the enzymolysis liquid to 95 ℃, and preserving the heat for 8min;
(6) Centrifuging the mixed solution after enzyme deactivation for 8min at the revolution of 5000r/min, and collecting supernatant;
(7) Adding zinc sulfate into the centrifugal supernatant, wherein the mass ratio of zinc ions to the raw material of the rice bran meal is 2;
(8) Heating the polysaccharide extracting solution added with the metal salt to 70 ℃, stirring for 60min, and after the reaction is finished, concentrating the chelating solution at 80 ℃ under reduced pressure, wherein the ratio of the volume of the concentrated solution to the volume of the stock solution is 1;
(9) Centrifuging the polysaccharide chelate concentrate for 15min at the speed of 5000r/min, and collecting the supernatant;
(10) Adding 3 times volume of absolute ethyl alcohol into the polysaccharide chelated concentrated supernatant, and refrigerating at 4 ℃ for 10 hours;
(11) Pouring the refrigerated supernatant, and collecting the precipitate;
(12) And drying the precipitate at 80 ℃, crushing and sieving by a 80-mesh sieve to obtain the rice bran polysaccharide zinc chelate 2.
Example 3
(1) Crushing the rice bran meal, and sieving the crushed rice bran meal with a 80-mesh sieve;
(2) Weighing 2kg of the sieved rice bran meal, and mixing the rice bran meal with alpha-amylase and neutral protease, wherein the addition amount of the alpha-amylase is 120U/g of the rice bran meal, and the addition amount of the neutral protease is 5000U/g of the rice bran meal;
(3) Adding water into the mixed materials according to the solid-liquid mass ratio of 1;
(4) Adjusting the pH value of the extracted mixture to 4.5 by using citric acid, respectively adding phytase, xylanase and cellulase, carrying out enzymolysis at 55 ℃ for 2.5h, wherein the addition amount of the phytase is 180U/g of rice bran meal, the addition amount of the xylanase is 4000U/g of rice bran meal, and the addition amount of the cellulase is 1000U/g of rice bran meal;
(5) Heating the enzymolysis liquid to 90 ℃, and preserving the temperature for 10min;
(6) Centrifuging the mixed solution after enzyme deactivation for 10min at the revolution of 4000r/min, and collecting supernatant;
(7) Adding zinc sulfate into the centrifugal supernatant, wherein the mass ratio of zinc ions to the raw material of the rice bran meal is 3;
(8) Heating the polysaccharide extracting solution added with the metal salt to 80 ℃, stirring for 80min, and after the reaction is finished, concentrating the chelating solution at 85 ℃ under reduced pressure, wherein the ratio of the volume of the concentrated solution to the volume of the stock solution is 1;
(9) Centrifuging the polysaccharide chelate concentrate for 20min at the revolution of 4000r/min, and collecting the supernatant;
(10) Adding 2 times volume of absolute ethyl alcohol into the polysaccharide chelate concentrated supernatant, and refrigerating at 4 ℃ for 12h;
(11) Pouring the refrigerated supernatant, and collecting the precipitate;
(12) And drying the precipitate at 85 ℃, crushing and sieving by a 80-mesh sieve to obtain the rice bran polysaccharide zinc chelate 3.
Preparation of rice bran polysaccharides without zinc chelation
Comparative example 1
(1) Crushing the rice bran meal, and sieving the crushed rice bran meal with a 60-mesh sieve;
(2) Weighing 2kg of the sieved rice bran meal, and mixing the rice bran meal with alpha-amylase and neutral protease, wherein the addition amount of the alpha-amylase is 40U/g of the rice bran meal, and the addition amount of the neutral protease is 3000U/g of the rice bran meal;
(3) Adding water into the mixed materials according to the solid-liquid mass ratio of 1;
(4) Adjusting the pH value of the extracted mixture to 5.5 by using citric acid, respectively adding phytase, xylanase and cellulase, carrying out enzymolysis at the temperature of 45 ℃ for 1.5h, wherein the addition amount of the phytase is 120U/g of rice bran meal, the addition amount of the xylanase is 2000U/g of rice bran meal, and the addition amount of the cellulase is 500U/g of rice bran meal;
(5) Heating the enzymolysis liquid to 100 deg.C, and keeping the temperature for 5min;
(6) Centrifuging the mixed solution after enzyme deactivation for 5min at the revolution of 4000r/min, and collecting supernatant;
(7) Concentrating the centrifugal supernatant at 70 ℃ under reduced pressure, wherein the ratio of the volume of the concentrated solution to the volume of the stock solution is 1;
(8) Centrifuging the polysaccharide concentrated solution at 4000r/min for 10min, and collecting supernatant;
(9) Adding absolute ethyl alcohol with the volume 4 times that of the polysaccharide concentrated supernatant, and refrigerating at 4 ℃ for 8h;
(10) Pouring the refrigerated supernatant, and collecting the precipitate;
(11) Drying the precipitate at 70 deg.C, pulverizing, and sieving with 60 mesh sieve to obtain testa oryzae polysaccharide 1.
Comparative example 2
(1) Crushing the rice bran meal, and sieving the crushed rice bran meal with a 80-mesh sieve;
(2) Weighing 2kg of sieved rice bran meal, and mixing with alpha-amylase and neutral protease, wherein the addition amount of the alpha-amylase is 80U/g of the rice bran meal, and the addition amount of the neutral protease is 4000U/g of the rice bran meal;
(3) Adding water into the mixed materials according to the solid-liquid mass ratio of 1;
(4) Adjusting the pH of the extracted mixture to 5.0 by using citric acid, respectively adding phytase, xylanase and cellulase, carrying out enzymolysis at 50 ℃ for 2.0h, wherein the addition amount of the phytase is 150U/g of rice bran meal, the addition amount of the xylanase is 3000U/g of rice bran meal, and the addition amount of the cellulase is 750U/g of rice bran meal;
(5) Heating the enzymolysis liquid to 95 ℃, and keeping the temperature for 8min;
(6) Centrifuging the mixed solution after enzyme deactivation for 8min at the speed of 5000r/min, and collecting supernatant;
(7) Concentrating the centrifugal supernatant at 80 ℃ under reduced pressure, wherein the ratio of the volume of the concentrated solution to the volume of the stock solution is 1;
(8) Centrifuging the polysaccharide concentrated solution at the speed of 5000r/min for 15min, and collecting the supernatant;
(9) Adding 3 times volume of anhydrous ethanol into the polysaccharide concentrated supernatant, and refrigerating at 4 ℃ for 10h;
(10) Pouring the refrigerated supernatant, and collecting the precipitate;
(11) Drying the precipitate at 80 deg.C, pulverizing, and sieving with 80 mesh sieve to obtain testa oryzae polysaccharide 2.
Comparative example 3
(1) Crushing the rice bran meal, and sieving the crushed rice bran meal with a 80-mesh sieve;
(2) Weighing 2kg of the sieved rice bran meal, and mixing the rice bran meal with alpha-amylase and neutral protease, wherein the addition amount of the alpha-amylase is 120U/g of the rice bran meal, and the addition amount of the neutral protease is 5000U/g of the rice bran meal;
(3) Adding water into the mixed materials according to the solid-liquid mass ratio of 1;
(4) Adjusting the pH value of the extracted mixture to 4.5 by using citric acid, respectively adding phytase, xylanase and cellulase, carrying out enzymolysis at 55 ℃ for 2.5h, wherein the addition amount of the phytase is 180U/g of rice bran meal, the addition amount of the xylanase is 4000U/g of rice bran meal, and the addition amount of the cellulase is 1000U/g of rice bran meal;
(5) Heating the enzymolysis liquid to 90 ℃, and preserving the temperature for 10min;
(6) Centrifuging the mixed solution after enzyme deactivation for 10min at the revolution of 4000r/min, and collecting supernatant;
(7) Concentrating the centrifugal supernatant at 85 ℃ under reduced pressure, wherein the ratio of the volume of the concentrated solution to the volume of the stock solution is 1;
(8) Centrifuging the polysaccharide concentrated solution at 4000r/min for 20min, and collecting supernatant;
(9) Adding 2 times volume of absolute ethyl alcohol into the polysaccharide concentrated supernatant, and refrigerating at 4 ℃ for 12h;
(10) Pouring the refrigerated supernatant, and collecting the precipitate;
(11) Drying the precipitate at 85 deg.C, pulverizing, and sieving with 80 mesh sieve to obtain testa oryzae polysaccharide 3.
The rice bran polysaccharide and the rice bran polysaccharide zinc chelate yield, the polysaccharide content and the zinc content which are prepared in the comparative example and the example are measured as follows:
according to the formula: yield/% = mass of rice bran polysaccharide (mass of zinc chelate of rice bran polysaccharide)/mass of rice bran meal x 100, and the yields of rice bran polysaccharide and zinc chelate of rice bran polysaccharide in comparative examples and examples were calculated.
According to the export-import inspection and quarantine industry standard SN/T4260-2015 of the people's republic of China: determination of crude polysaccharide in export plant source food (phenol-sulfuric acid method) determination of polysaccharide content in sample.
The zinc content of the sample was measured by an atomic absorption spectrophotometer, and the results are shown in table 1.
TABLE 1 Change in yield, polysaccharide content and Zinc content before and after chelation
Determination of antioxidant capacity of rice bran polysaccharide and rice bran polysaccharide zinc chelate prepared in comparative examples and examples
(1) Determination of DPPH radical scavenging Capacity:
preparing the rice bran polysaccharide and the rice bran polysaccharide zinc chelate compound prepared in the comparative example and the embodiment into a solution to be detected with the concentration gradient of 0.2, 0.4, 0.6, 0.8 and 1.0mg/mL, absorbing 1mL of the solution to be detected, respectively adding 3mL of 0.2mmol/L DPPH ethanol solution, mixing uniformly, placing in a dark place, reacting for 30min at room temperature, adjusting the zero point with distilled water, and measuring the light absorption value Ac of a blank tube and the light absorption value As of a sample tube at 517 nm. Vc was used as a positive control.
Semi-inhibitory concentration IC 50 And calculating according to the concentration value corresponding to the clearance rate of 50% read on the concentration-clearance two-dimensional curve.
According to the formula: clearance/% = (Ac-As)/Ac × 100, the clearance of DPPH radicals was calculated.
As can be seen from figure 1, the rice bran polysaccharide and the rice bran polysaccharide zinc chelate have a certain scavenging effect on DPPH, the scavenging rate is gradually increased along with the increase of the concentration in the concentration range of 0.2-1.0 mg/mL, the quantity-effect relationship is presented, when the Vc concentration is 0.2mg/mL, the scavenging rate on DPPH free radicals is over 90 percent, the rice bran polysaccharide zinc chelate 3 has the strongest capacity of scavenging DPPH free radicals, and when the concentration is 1.0mg/mL, the scavenging rate on DPPH free radicals is over 90 percent. Calculated IC of rice bran polysaccharide 1, rice bran polysaccharide 2 and rice bran polysaccharide 3 50 The value is close to 0.73mg/mL, and the IC of the rice bran polysaccharide zinc chelate 1, the rice bran polysaccharide zinc chelate 2 and the rice bran polysaccharide zinc chelate 3 50 Respectively as follows: 0.65mg/mL, 0.56mg/mL, 0.45mg/mL, show that the effect of the rice bran polysaccharide zinc chelate in removing DPPH is gradually enhanced with the increase of the zinc chelate amount in the rice bran polysaccharide.
(2) Measurement of hydroxyl radical (. OH) scavenging ability:
preparing the rice bran polysaccharide and the rice bran polysaccharide zinc chelate compound prepared in the comparative example and the example into the solution to be detected with the concentration gradient of 0.1, 0.2, 0.3, 0.4 and 0.5mg/mL, sucking 1mL of the solution to be detected, and respectively adding 10mmol/L of FeSO 4 1mL of 10mmol/L salicylic acid-ethanol solution, and finally 8.8mmol/L H 2 O 2 The reaction was started at 1mL, and the absorbance Ac in the blank tube and the absorbance As in the sample tube were measured at 510nm for 30min at 37 ℃. Vc was used as a positive control.
Semi-inhibitory concentration IC 50 And calculating according to the concentration value corresponding to the clearance rate of 50% read on the concentration-clearance two-dimensional curve.
According to the formula: clearance/% = (Ac-As)/Ac × 100, clearance of hydroxyl radical was calculated.
As can be seen from figure 2, the rice bran polysaccharide and the rice bran polysaccharide zinc chelate have certain effect of removing OH, the removal rate is gradually increased along with the increase of the concentration within the concentration range of 0.1-0.5 mg/mL, the quantity-effect relationship is presented, the rice bran polysaccharide zinc chelate 3 has the strongest capacity of removing OH free radicals, and when the concentration is 0.5mg/mL, the removal rate of the OH free radicals exceeds 85%. Calculated IC of rice bran polysaccharide 1, rice bran polysaccharide 2, rice bran polysaccharide 3 50 The value is close to 0.38mg/mL, and the IC of rice bran polysaccharide zinc chelate 1, rice bran polysaccharide zinc chelate 2, rice bran polysaccharide zinc chelate 3 and Vc 50 Respectively as follows: 0.33mg/mL, 0.28mg/mL, 0.24mg/mL, 0.20mg/mL, show that the effect of removing OH from the zinc chelate of the rice bran polysaccharide is gradually enhanced with the increase of the amount of the zinc chelate in the rice bran polysaccharide.
According to the invention, the novel extraction technology, namely the complex use of hydraulic oscillation and enzymolysis, is adopted to realize the short-time and high-efficiency extraction of the rice bran polysaccharide, the hydraulic oscillation treatment is carried out for 10min, the enzymolysis time is not more than 2.5h, the yield of the rice bran polysaccharide is higher than 9%, and the purity of the rice bran polysaccharide is higher than 70% before metal ions are chelated.
The invention applies the high-efficiency chelation of the rice bran polysaccharide to zinc ions to produce an organic zinc chelation product with high zinc ion content and strong antioxidant activity. The zinc ion content can be flexibly adjusted according to people with different requirements and animals of different types, and the product can be directly added into food and can also be used as a feed additive, so that the zinc ion-containing feed additive is nutritional, health-care, green and safe.
The technical solutions above illustrate the technical idea of the present invention, and the scope of the present invention should not be limited thereby, and any changes and modifications made to the above technical solutions according to the technical essence of the present invention are all within the scope of the technical solutions of the present invention.
Claims (7)
1. A preparation method of a rice bran polysaccharide zinc chelate is characterized by comprising the following steps:
(1) Pretreatment of raw materials: crushing rice bran meal;
(2) Mixing materials: mixing rice bran meal with alpha-amylase and neutral protease; the addition amount of the alpha-amylase is 40-120U/g rice bran meal, and the addition amount of the neutral protease is 3000-5000U/g rice bran meal;
(3) Hydraulic oscillation extraction: adding water into the mixed materials for batching, wherein the solid-liquid mass ratio is 1 (15-25), uniformly stirring, and then carrying out oscillation treatment in hydraulic oscillation equipment, wherein the hydraulic oscillation treatment time is 8-12min, and the temperature is room temperature;
(4) Enzymolysis: adjusting the pH value of the extraction mixture obtained in the step (3) to 4.5-5.5, respectively adding phytase, xylanase and cellulase, and carrying out enzymolysis at the temperature of 45-55 ℃ for 1.5-2.5 h; the adding amount of phytase is 120-180U/g rice bran meal, the adding amount of xylanase is 2000-4000U/g rice bran meal, and the adding amount of cellulase is 500-1000U/g rice bran meal;
(5) Enzyme deactivation: heating the enzymolysis mixed liquor obtained in the step (4) to 90-100 ℃, and preserving heat for 5-10 min;
(6) Centrifuging: centrifuging the mixed solution after enzyme deactivation and collecting supernatant;
(7) Adding metal ions: adding zinc ion salt into the supernatant obtained in the step (6), wherein the mass ratio of the zinc ion to the rice bran meal raw material is (1-3) to 100;
(8) Chelating: heating the polysaccharide extracting solution added with the zinc ion salt to 60 to 80 ℃, stirring for 40 to 80min, and after the chelation reaction is finished, concentrating the polysaccharide chelating solution at 70 to 85 ℃ under reduced pressure;
(9) Centrifuging: centrifuging the polysaccharide chelate concentrate and collecting the supernatant;
(10) Ethanol precipitation: adding absolute ethyl alcohol into the supernatant obtained in the step (9), and refrigerating at 4 ℃ for 8 to 12h;
(11) Solid-liquid separation: precipitating the polysaccharide chelate concentrated clear solution with ethanol, layering, performing solid-liquid separation, and collecting precipitate;
(12) And (3) drying: and (4) drying the precipitate obtained in the step (11), crushing and sieving to obtain the rice bran polysaccharide zinc chelate.
2. The preparation method of the rice bran polysaccharide zinc chelate complex as claimed in claim 1, wherein the crushing particle size of the raw material in the step (1) is 60 to 80 meshes.
3. The method for preparing zinc chelate of rice bran polysaccharide according to claim 1, wherein the centrifugation speed in step (6) is 4000 to 5000r/min and the centrifugation time is 5 to 10min, and the centrifugation speed in step (9) is 4000 to 5000r/min and the centrifugation time is 10 to 20min.
4. The method for preparing the rice bran polysaccharide zinc chelate complex as claimed in claim 1, wherein the ratio of the volume of the concentrated solution to the volume of the stock solution of the chelate solution in the step (8) is 1 to 10 to 1.
5. The preparation method of the rice bran polysaccharide zinc chelate complex as claimed in claim 1, wherein the addition amount of the absolute ethanol in the step (10) is 2 to 4 times of the volume of the supernatant obtained in the step (9), the polysaccharide chelate concentrated supernatant is separated into distinct layers after ethanol precipitation, the precipitate aggregation is not dispersed, and the polysaccharide zinc chelate complex exists in the precipitate.
6. The preparation method of the rice bran polysaccharide zinc chelate compound as claimed in claim 1, wherein the drying temperature in the step (12) is 70 to 85 ℃, the mixture is ground and sieved by using a sieve with 60 to 80 meshes, the yield of the polysaccharide zinc chelate compound obtained in the step (12) is 10 to 16 percent, the polysaccharide content is 45 to 65 percent, and the zinc ion content is 8 to 15 percent.
7. The application of the rice bran polysaccharide zinc chelate is characterized in that the rice bran polysaccharide zinc chelate prepared by the preparation method according to any one of claims 1 to 6 is used for preparing any one of products of clinical medicines, health products, food additives and feed additives.
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