CN114634562A - Preparation method of iron protein succinate - Google Patents
Preparation method of iron protein succinate Download PDFInfo
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Abstract
The invention discloses a preparation method of iron protein succinate, which comprises the steps of carrying out ultrasonic treatment on a casein solution, adding succinic anhydride, and adjusting the pH value to 8.0-10.0; dropwise adding an acid solution to adjust the pH value to 2-3; filtering to obtain precipitate to obtain wet succinyl protein solid; then dissolving the wet succinyl protein solid in a sodium hydroxide solution, wherein the pH value is 7-8; carrying out ultrasonic treatment, dropwise adding a ferric trichloride solution and a sodium hydroxide solution to maintain the pH value of the reaction solution at 6-9, stirring and reacting for 3 hours after the dropwise adding is finished, adding acid to adjust the pH value of the reaction solution to 2-3, filtering and washing to obtain a crude product of the ferric protein succinate; adding the crude product of the iron protein succinate into a sodium hydroxide solution, shearing to control the molecular weight range to be 300-500kDa, and then adding a propping agent for spray drying to obtain a finished product. The molecular weight of the finally prepared iron protein succinate is still kept within the range of 300-500kDa, the dissolution and redissolution effects with water are good, and free iron can not be generated.
Description
Technical Field
The invention belongs to the technical field of medicines, and particularly relates to a preparation method of iron protein succinate.
Background
The iron protein succinate is prepared by acylating casein anhydride and mixing with trivalent iron salt (such as FeCl)3) The novel iron-supplementing medicament for treating iron-deficiency anemia (IDA) is chelated, and has the advantages of various anemia symptoms as main indications, few gastrointestinal adverse reactions and the like. The current dosage form sold in the market at home and abroad is mainly ferric protein succinate oral solution. Because of its unique properties, iron proteinsuccinate is protected from the destruction of gastric acid and the enzymatic hydrolysis by pepsin, without causing damage to the gastric mucosa. After entering the intestine, it is redissolved and digested by trypsin. After digestion of the protein protective membrane of iron protein succinate, iron release begins in the duodenum.
Iron in the iron protein succinate molecules is tightly chelated with protein, and the iron ion does not have stimulation reaction after being taken, so that the bioavailability is high; and the casein is not digested by pepsin in the stomach and can be hydrolyzed by trypsin at a neutral pH value, so that the sensitivity of the casein to the pH value is kept, and the casein has intestinal targeting property.
The iron protein succinate is formed by chelating casein and ferric iron, and the casein as a mixture has no fixed molecular formula and molecular weight, so the iron protein succinate also has no fixed chemical structural formula and molecular formula. The iron protein succinate prepared by the prior art is mostly in the range of 300-2000kDa in molecular weight, the solubility of the iron protein succinate in water is poor, and the solution viscosity is high. In order to increase the solubility and stability of the iron protein succinate in water so as to be convenient for producing products such as oral liquid and the like, the iron protein succinate solution needs to be treated, and the conventional shearing emulsifying and dispersing mode is easy to destroy the molecular structure and lose the functionality.
In the prior art, for example, the chinese granted patent CN104402984B provides a method for preparing iron protein succinate with high iron loading, which increases the iron loading of iron protein succinate by controlling the environmental pH value of casein during the reaction with succinic anhydride and controlling the method and time for dropping the iron trichloride solution containing sodium bicarbonate into the succinic acid protein solution for reaction, and the iron content of the prepared iron protein succinate is 5.1%.
For another example, CN102671189B, granted to china patent, provides a method for solubilizing iron protein succinate, which comprises mixing and stirring iron protein succinate with solubilizing agents (sodium dodecyl sulfate, poloxamer, PEG-400, β -cyclodextrin), excipient (sorbitol), and cosolvent (propylene glycol) under alkaline conditions, thereby increasing the solubility of iron protein succinate in water, and making the content of free iron in the prepared oral liquid not more than 0.1% of the total content.
For example, the chinese granted patent CN102838667B provides a method for preparing iron protein succinate, which is characterized by adjusting and controlling the weight ratio of casein to succinic anhydride, the weight ratio of succinic protein to ferric trichloride, and the pH value during the reaction process, so as to prepare iron protein succinate with high acylation degree, large iron-carrying capacity, good solubility, stable quality, low impurity content, and significant efficacy.
However, none of the above-mentioned methods for preparing iron protein succinate can effectively control the molecular weight of the prepared iron protein succinate.
For example, the Chinese patent application CN106589103A provides a method for preparing iron succinate protein, firstly, an ultrafiltration membrane with the molecular weight cutoff of 500 kDa-1000 kDa is utilized to separate an acylated liquid membrane to obtain a filtrate, the ultrafiltration membrane with the molecular weight of 100 kDa-300 kDa is utilized to carry out membrane separation on the acylated liquid filtrate after the pH value is adjusted, the permeate is removed to obtain an acylated casein solution, FeCl is added into the acylated casein solution3After the reaction, ultrafiltration membranes with the molecular weight cutoff of 500 kDa-1000 kDa and 100 kDa-300 kDa are used for treatment in sequence, and then acid is added for precipitation to obtain the protein iron succinate with the corresponding molecular weight. The method utilizes an ultrafiltration membrane, which is tedious and increases the cost, and the prepared iron protein succinate has poor redissolution property and stability.
Disclosure of Invention
In view of the above disadvantages of the prior art, the present invention provides a method for preparing iron protein succinate, which is specifically realized by the following techniques.
A preparation method of iron protein succinate comprises the following steps:
s1, acylation: preparing casein into an aqueous solution, continuously performing first ultrasonic treatment, adding succinic anhydride into the casein solution for reaction, and continuously adding a sodium hydroxide solution to keep the pH value of the reaction solution at 8.0-10.0; after the reaction is finished, dropwise adding an acid solution to adjust the pH value of the reaction solution to 2-3, and stopping ultrasonic treatment; filtering to obtain precipitate to obtain wet succinyl protein solid;
s2, crude iron loading: adding a sodium hydroxide solution into the wet succinyl protein solid obtained in the step S1 while stirring to completely dissolve the wet succinyl protein solid, wherein the pH value of the solution after dissolution is 7-8; continuously carrying out secondary ultrasonic treatment on the solution system, dropwise adding a ferric trichloride solution and a sodium hydroxide solution to maintain the pH value of the reaction solution at 6-9, and continuously stirring for reacting for 3 hours after the dropwise adding of the ferric trichloride solution is finished; after the reaction is finished, adding acid to adjust the pH value of the reaction solution to 2-3, precipitating iron protein succinate, and stopping ultrasonic treatment; filtering and washing to obtain a crude product of the iron protein succinate with the iron loading of 1-5%;
s3, refining: adding sodium hydroxide solution into the crude product of the iron protein succinate obtained in the step S2 while stirring to completely dissolve the iron protein succinate, and shearing the solution system to control the molecular weight range of the iron protein succinate to be 300-500 kDa; adding a propping agent, uniformly stirring, and spray-drying to obtain a finished product of the iron protein succinate; the proppant is lactose and/or fructose.
The preparation method of the iron protein succinate comprises three treatment stages of acylation, iron-carrying rough preparation and refining; ultrasonic treatment is adopted in the acylation and iron-carrying crude process, the molecular weight of the iron protein succinate after shearing treatment is controlled in the refining process, and the iron protein succinate with the molecular weight is matched with a propping agent, so that the molecular weight of the iron protein succinate prepared by final spray drying is still kept in the range of 300-500kDa and is not changed greatly compared with the molecular weight of the iron protein succinate controlled after shearing treatment. The finally prepared iron protein succinate finished product has good redissolution effect after being dissolved by water, and the generation of free iron is avoided. The acid solution can be selected from common organic weak acids such as lactic acid, malic acid, etc. The proppant used can only play the role when lactose and fructose are selected, and the technical effect cannot be obtained when other sugars such as sucrose are selected. Spray drying may be carried out using the parameters customary in the art at the present time.
The iron protein succinate prepared by the method can be used as a food additive to be applied to infant supplementary food and milk powder.
Preferably, the ultrasonic frequency of the first ultrasonic treatment and the ultrasonic frequency of the second ultrasonic treatment are sequentially reduced. The ultrasonic frequency of the ultrasonic treatment adopts a sequentially decreasing mode, and the molecular weight range of the prepared iron protein succinate can be preliminarily controlled.
Preferably, the frequency of the first sonication is between 35 and 45kHz and the power of the second sonication is between 20 and 30 kHz.
More preferably, the power of the first sonication is 40kHz and the power of the second sonication is 25 kHz.
Preferably, in step S2, the iron loading amount of the crude iron protein succinate is 1-2%.
Preferably, in step S3, the weight ratio of the proppant to the crude iron protein succinate is 4-5: 1.
More preferably, in step S3, the weight ratio of the proppant to the crude iron protein succinate is 4.5: 1.
Preferably, in step S3, the shearing rate is 600-800 rpm.
Compared with the prior art, the invention has the advantages that: when the iron protein succinate is prepared, ultrasonic treatment with specific frequency is respectively adopted in two reaction stages of acylation and iron-carrying rough preparation, the molecular weight of the iron protein succinate is controlled by shearing treatment in a refining stage, and the molecular weight of the iron protein succinate prepared by spray drying is enabled to be not greatly changed compared with the molecular weight of the iron protein succinate after shearing by matching with a propping agent and still be effectively controlled within a smaller range of 300-500kDa, so that the prepared iron protein succinate oral liquid and other products have good solubility and stability; free iron is not generated after re-dissolution.
Detailed Description
The technical solutions of the present invention will be described clearly and completely below, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
This example prepared iron protein succinate as follows:
s1, acylation: preparing casein into an aqueous solution and continuously performing first ultrasonic treatment, wherein the ultrasonic frequency is 40 kHz; adding succinic anhydride into the casein solution for reacting for 1 hour, and continuously adding sodium hydroxide solution to keep the pH value of the reaction solution at about 8.5; after the reaction is finished, malic acid solution is dripped to adjust the pH value of the reaction solution to be about 2.5, and the ultrasonic treatment is stopped; filtering to obtain precipitate to obtain wet succinyl protein solid;
s2, crude iron loading: adding a sodium hydroxide solution into the wet succinyl protein solid obtained in the step S1 while stirring to completely dissolve the wet succinyl protein solid, wherein the pH value of the solution after dissolution is about 8.0; continuously carrying out secondary ultrasonic treatment on the solution system, wherein the ultrasonic frequency is 25 kHz; dropwise adding a ferric trichloride solution and a sodium hydroxide solution to maintain the pH value of the reaction solution at about 6.5, and continuously stirring for reacting for 3 hours after the dropwise adding of the ferric trichloride solution is finished; after the reaction is finished, malic acid is dripped to adjust the pH value of the reaction solution to be about 2.5, so that the iron protein succinate is precipitated, and the ultrasonic treatment is stopped; filtering and washing to obtain a crude iron protein succinate product with iron loading of about 2%;
s3, refining: adding sodium hydroxide solution into the crude product of the iron protein succinate obtained in the step S2 while stirring to completely dissolve the iron protein succinate, shearing the solution system at the shearing rate of 700rpm, and controlling the molecular weight range of the iron protein succinate to be 300-500 kDa; adding lactose (propping agent) and stirring uniformly, wherein the weight ratio of lactose to the crude iron protein succinate is 4.5: 1; spray drying is carried out according to the air inlet temperature of 150-.
Example 2
The method for preparing iron protein succinate of the present example differs from example 1 in that the frequency of the first ultrasonic treatment of step S1 is 35 kHz; the frequency of the second sonication was 20 kHz.
Example 3
The method for preparing iron protein succinate of the present example differs from example 1 in that the frequency of the first ultrasonic treatment of step S1 is 45 kHz; the frequency of the second sonication was 30 kHz.
Example 4
The method for preparing iron protein succinate in this example is different from example 1 in that the weight ratio of lactose to crude iron protein succinate in step S3 is 5: 1.
Example 5
The method for preparing iron protein succinate in this example is different from example 1 in that the weight ratio of lactose to crude iron protein succinate in step S3 is 4: 1.
Example 6
The present example differs from example 1 in that, in step S3, lactose is replaced with fructose, and the amount of fructose used is the same as in example 1.
Example 7
The method for preparing iron protein succinate in this embodiment is different from that in embodiment 1 in that in step S3, the same weight of lactose and fructose is used as the proppant, and the weight ratio of the total weight of lactose and fructose to the crude iron protein succinate is 4.5: 1.
Comparative example 1
The comparative example, in which the iron protein succinate was prepared, did not undergo the ultrasonic treatment and the shearing treatment, specifically includes the following steps:
s1, acylation: preparing casein into aqueous solution, adding succinic anhydride to react for 1 hour, and continuously adding sodium hydroxide solution to keep the pH value of the reaction solution at about 8.5; after the reaction is finished, malic acid solution is dripped to adjust the pH value of the reaction solution to about 2.5; filtering to obtain precipitate to obtain wet succinyl protein solid;
s2, crude iron loading: adding a sodium hydroxide solution into the wet succinyl protein solid obtained in the step S1 while stirring to completely dissolve the wet succinyl protein solid, wherein the pH value of the solution after dissolution is about 8.0; dropwise adding a ferric trichloride solution and a sodium hydroxide solution to maintain the pH value of the reaction solution at about 6.5, and continuously stirring for reacting for 3 hours after the dropwise adding of the ferric trichloride solution is finished; after the reaction is finished, malic acid is dripped to adjust the pH value of the reaction solution to about 2.5, so that the iron protein succinate is precipitated; filtering and washing to obtain a crude product of the iron protein succinate with iron loading of about 2 percent;
s3, refining: adding a sodium hydroxide solution into the crude iron protein succinate product obtained in the step S2 while stirring to completely dissolve the crude iron protein succinate product; adding lactose (propping agent) and stirring uniformly, wherein the weight ratio of the lactose to the crude iron protein succinate is 4.5: 1; spray drying is carried out according to the air inlet temperature of 150-.
Comparative example 2
When the iron protein succinate is prepared according to the comparative example, lactose (a propping agent) is not added in the step S3, and malic acid is added as a pH value regulator, specifically as follows:
s1, acylation: preparing casein into an aqueous solution and continuously carrying out first ultrasonic treatment, wherein the ultrasonic frequency is 40 kHz; adding succinic anhydride into the casein solution to react for 1 hour, and continuously adding sodium hydroxide solution to keep the pH value of the reaction solution at about 8.5; after the reaction is finished, malic acid solution is dripped to adjust the pH value of the reaction solution to be about 2.5, and the ultrasonic treatment is stopped; filtering to obtain precipitate to obtain wet succinyl protein solid;
s2, crude iron loading: adding a sodium hydroxide solution into the wet succinyl protein solid obtained in the step S1 while stirring to completely dissolve the wet succinyl protein solid, wherein the pH value of the solution after dissolution is about 8.0; continuously carrying out secondary ultrasonic treatment on the solution system, wherein the ultrasonic frequency is 25 kHz; dropwise adding a ferric trichloride solution and a sodium hydroxide solution to maintain the pH value of the reaction solution at about 6.5, and continuously stirring for reacting for 3 hours after the dropwise adding of the ferric trichloride solution is finished; after the reaction is finished, malic acid is dripped to adjust the pH value of the reaction solution to be about 2.5, so that the iron protein succinate is precipitated, and the ultrasonic treatment is stopped; filtering and washing to obtain a crude product of the iron protein succinate with iron loading of about 2 percent;
s3, refining: adding sodium hydroxide solution into the crude product of the iron protein succinate obtained in the step S2 while stirring to completely dissolve the iron protein succinate, shearing the solution system at the shearing rate of 700rpm, and controlling the molecular weight range of the iron protein succinate to be 300-500 kDa; dropping malic acid to adjust the pH value to 2-3 to precipitate the iron protein succinate to form a suspension, and then performing spray drying at the air inlet temperature of 150-160 ℃ and the air outlet temperature of 90-100 ℃ to obtain the iron protein succinate finished product.
Comparative example 3
When the iron protein succinate is prepared according to the comparative example, no lactose is added, ultrasonic and shearing treatment is not carried out, and malic acid is dripped to be used as a pH value regulator, which comprises the following steps:
s1, acylation: preparing casein into aqueous solution, adding succinic anhydride for reacting for 1 hour, and continuously adding sodium hydroxide solution to keep the pH value of the reaction solution at about 8.5; after the reaction is finished, malic acid solution is dripped to adjust the pH value of the reaction solution to about 2.5; filtering to obtain precipitate to obtain wet succinyl protein solid;
s2, crude iron loading: adding a sodium hydroxide solution into the wet succinyl protein solid obtained in the step S1 while stirring to completely dissolve the wet succinyl protein solid, wherein the pH value of the solution after dissolution is about 8.0; dropwise adding a ferric trichloride solution and a sodium hydroxide solution to maintain the pH value of the reaction solution at about 6.5, and continuously stirring for reacting for 3 hours after the dropwise adding of the ferric trichloride solution is finished; after the reaction is finished, malic acid is dripped to adjust the pH value of the reaction solution to be about 2.5, so that the iron protein succinate is precipitated; filtering and washing to obtain a crude product of the iron protein succinate with iron loading of about 2 percent;
s3, refining: adding a sodium hydroxide solution into the crude iron protein succinate product obtained in the step S2 while stirring to completely dissolve the crude iron protein succinate product; dropping malic acid to adjust the pH value to 2-3 to precipitate the iron protein succinate to form a suspension, and then performing spray drying at the air inlet temperature of 150-160 ℃ and the air outlet temperature of 90-100 ℃ to obtain the iron protein succinate finished product.
Comparative example 4
The present comparative example method for preparing iron-protein succinate differs from example 1 in that the frequency of the first ultrasonic treatment of step S1 is 30 kHz; the second ultrasonic processing is not performed in step S2.
Comparative example 5
The present comparative example method for preparing iron-protein succinate differs from example 1 in that the frequency of the first ultrasonic treatment of step S1 is 50 kHz; the frequency of the second ultrasonic treatment of step S2 was 40 kHz.
Comparative example 6
The method for preparing iron proteinsuccinate according to this comparative example differs from example 1 in that lactose is replaced with sucrose in step S3, the amount of sucrose is the same as in example 1, and malic acid is added dropwise as a pH adjuster. The specific method comprises the following steps:
s1, acylation: preparing casein into aqueous solution, adding succinic anhydride for reacting for 1 hour, and continuously adding sodium hydroxide solution to keep the pH value of the reaction solution at about 8.5; after the reaction is finished, malic acid solution is dripped to adjust the pH value of the reaction solution to about 2.5; filtering to obtain precipitate to obtain wet succinyl protein solid;
s2, crude iron loading: adding a sodium hydroxide solution into the wet succinyl protein solid obtained in the step S1 while stirring to completely dissolve the wet succinyl protein solid, wherein the pH value of the solution after dissolution is about 8.0; dropwise adding a ferric trichloride solution and a sodium hydroxide solution to maintain the pH value of the reaction solution at about 6.5, and continuously stirring for reacting for 3 hours after the dropwise adding of the ferric trichloride solution is finished; after the reaction is finished, malic acid is dripped to adjust the pH value of the reaction solution to be about 2.5, so that the iron protein succinate is precipitated; filtering and washing to obtain a crude product of the iron protein succinate with iron loading of about 2 percent;
s3, refining: adding sodium hydroxide solution into the crude product of the iron protein succinate obtained in the step S2 while stirring to completely dissolve the iron protein succinate, and shearing the solution system at the shearing rate of 700rpm, wherein the molecular weight range of the iron protein succinate is controlled to be 300-500 kDa; adding sucrose, and stirring uniformly, wherein the weight ratio of the sucrose to the crude product of the iron protein succinate is 4.5: 1; dropping malic acid to regulate pH value to 2.5 to separate out iron protein succinate to form suspension, and spray drying at 150-160 deg.c and 90-100 deg.c to obtain iron protein succinate product.
Application example:
1. through the determination of the molecular weight of the prepared iron protein succinate by SDS-polyacrylamide gel electrophoresis, in examples 1-7, the molecular weight range of the finished iron protein succinate prepared in comparative example 1 comprises 300-500kDa and the distribution span is far larger than 300-500kDa, i.e. the small end of the molecular weight range is far smaller than 300kDa and the large end is far larger than 500 kDa; in the case of the iron protein succinate prepared in comparative example 2, although the molecular weight range can be controlled within 300-500kDa after shearing, the molecular weight range of the finally prepared iron protein succinate finished product is similar to that of comparative example 1, and the distribution span is large; the molecular weight range of the finished iron protein succinate prepared in the comparative example 3 is larger than that of the finished iron protein succinate prepared in the comparative example 1; the small end of the molecular weight distribution range of the iron protein succinate of comparative example 4 is greater than 300kDa, and the large end is greater than 500 kDa; the iron protein succinate of comparative example 5 has a molecular weight distribution range with a small end of less than 300kDa and a large end of less than 500 kDa; comparative example 6 in the preparation of iron protein succinate, although the molecular weight range after cleavage was controlled within 300-500kDa, the molecular weight range of the final iron protein succinate product was similar to that of comparative example 1, and the distribution span was relatively large.
2. At room temperature, 13 groups of 100mL ultrapure water were taken, and a plurality of weight of iron protein succinate prepared in examples 1 to 7 and comparative examples 1 to 6 were added thereto, and shaken every 5min for 30s, and the dissolution of iron protein succinate after 30min was observed.
After testing, the solubility of the iron protein succinates of examples 1-7 is better than that of comparative examples 1-6; wherein, the solubility of the iron protein succinates of the examples 1, 6 and 7 is the best and the three are not different, the solubility of the iron protein succinates of the examples 2 and 5 is slightly less than that of the example 1, and the solubility of the iron protein succinates of the examples 3 and 4 is slightly more than that of the example 1; the solubility of iron protein succinate of comparative example 3 was minimal, the solubility of iron protein succinate of comparative examples 1-4, 6 was less than that of example 1, and the solubility of iron protein succinate of comparative example 5 was comparable to that of example 1.
3. The iron protein succinate prepared in the examples 1-7 and the comparative examples 1-6 is used as a raw material to prepare the oral liquid, and the preparation method comprises the following steps: adding 6g of iron protein succinate into purified water, adding a sodium hydroxide solution to adjust the pH value to be about 8.0, and stirring until the iron protein succinate is completely dissolved; adding sodium hydroxy phenylpropionate as antiseptic, stirring to dissolve, adding malic acid dropwise to adjust pH to about 7.5, adding essence and saccharin sodium 0.1g each, adding water to desired volume of 100mL to obtain oral liquid.
The content of free iron in oral liquids prepared from the iron proteinsuccinates prepared in examples 1-7 and comparative examples 1-6 was determined, the content of free iron in oral liquids in examples 1-7 was not detected, the content of free iron in oral liquids in comparative examples 1 and 2 was 0.009% and 0.012%, respectively, the content of free iron in oral liquids in comparative example 3 was 0.023%, the content of free iron in oral liquids in comparative example 4 was 0.005%, the content of free iron in oral liquids in comparative example 5 was 0.002%, and the content of free iron in oral liquids in comparative example 6 was 0.003%.
The test results show that proper ultrasonic treatment and shearing treatment are carried out in the preparation process of the iron protein succinate, and a proper amount of specific propping agent (lactose or fructose) is added during final refining, so that the molecular weight of the iron protein succinate can be effectively controlled within the range of 300-500kDa, the redissolution performance of the prepared iron protein succinate product is better, and no free iron is generated when the iron protein succinate product is prepared into oral liquid.
Claims (8)
1. The preparation method of the iron protein succinate is characterized by comprising the following steps of:
s1, acylation: preparing casein into an aqueous solution, continuously performing first ultrasonic treatment, adding succinic anhydride into the casein solution for reaction, and continuously adding a sodium hydroxide solution to keep the pH value of the reaction solution at 8.0-10.0; after the reaction is finished, dropwise adding an acid solution to adjust the pH value of the reaction solution to 2-3, and stopping ultrasonic treatment; filtering to obtain precipitate to obtain wet succinyl protein solid;
s2, crude iron loading: adding a sodium hydroxide solution into the wet succinyl protein solid obtained in the step S1 while stirring to completely dissolve the wet succinyl protein solid, wherein the pH value of the solution after dissolution is 7-8; continuously carrying out secondary ultrasonic treatment on the solution system, dropwise adding a ferric trichloride solution and a sodium hydroxide solution to maintain the pH value of the reaction solution at 6-9, and continuously stirring for reacting for 3 hours after the dropwise adding of the ferric trichloride solution is finished; after the reaction is finished, adding acid to adjust the pH value of the reaction solution to 2-3, precipitating iron protein succinate, and stopping ultrasonic treatment; filtering and washing to obtain a crude product of the iron protein succinate with the iron loading of 1-5%;
s3, refining: adding sodium hydroxide solution into the crude product of the iron protein succinate obtained in the step S2 while stirring to completely dissolve the iron protein succinate, and shearing the solution system to control the molecular weight range of the iron protein succinate to be 300-500 kDa; adding a propping agent, uniformly stirring, and spray-drying to obtain a finished product of the iron protein succinate; the proppant is lactose and/or fructose.
2. The method according to claim 1, wherein the ultrasonic frequencies of the first ultrasonic treatment and the second ultrasonic treatment are sequentially decreased.
3. The method of preparing iron proteinsuccinate according to claim 2, wherein the frequency of the first sonication is 35-45kHz and the power of the second sonication is 20-30 kHz.
4. The method of preparing iron protein succinate according to claim 3, wherein the power of the first sonication is 40kHz and the power of the second sonication is 25 kHz.
5. The method according to claim 1, wherein in step S2, the iron loading of the crude iron protein succinate product is 1-2%.
6. The method according to claim 1, wherein in step S3, the weight ratio of the proppant to the crude iron protein succinate is 4-5: 1.
7. The method according to claim 6, wherein in step S3, the weight ratio of the proppant to the crude iron protein succinate is 4.5: 1.
8. The method as claimed in claim 1, wherein the shearing rate in step S3 is 600-800 rpm.
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| CN112063676A (en) * | 2020-09-02 | 2020-12-11 | 杭州汉库医药科技有限公司 | Casein purification method and preparation method of iron protein succinate |
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