CN114634562B - Preparation method of protein iron succinate - Google Patents
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Abstract
The invention discloses a preparation method of protein iron succinate, which comprises the steps of carrying out ultrasonic treatment on 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 succinyl protein wet solid; then dissolving the succinyl protein wet solid in sodium hydroxide solution, wherein the pH value is 7-8; performing ultrasonic treatment, dropwise adding ferric trichloride solution and sodium hydroxide solution to maintain the pH value of the reaction solution at 6-9, stirring for reaction 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 with water to obtain a crude product of protein succinic acid iron; adding the crude product of the protein succinic acid into a sodium hydroxide solution, performing shearing control to the molecular weight range of 300-500kDa, and then adding a propping agent for spray drying to obtain a finished product. The molecular weight of the finally prepared protein iron succinate is still kept within the range of 300-500kDa, and the dissolution and re-dissolution effects are good when water is used, so that free iron can not be generated.
Description
Technical Field
The invention belongs to the technical field of medicines, and in particular relates to a preparation method of protein iron succinate.
Background
The protein iron succinate is prepared by acylating casein anhydride and then mixing with ferric salt (such as FeCl) 3 ) Chelating iron-supplementing medicine for treating Iron Deficiency Anemia (IDA) with main indication of various anemia symptoms and few adverse reactions of gastrointestinal tractAdvantages are achieved. The dosage form sold in the market at home and abroad at present is mainly protein iron succinate oral solution. Because of the unique characteristics, the protein iron succinate is protected by a protein film and is not damaged by gastric acid and is not hydrolyzed by pepsin, so that the gastric mucosa is not damaged. After entering the intestine, it redissolves and is digested by trypsin. After digestion of the protein protective film of the protein iron succinate, iron begins to be released in the duodenum.
Iron in the protein succinic acid iron molecule is tightly chelated with protein, no stimulation reaction of iron ions is generated after taking, and the bioavailability is high; the casein is not digested by pepsin in the stomach, can be hydrolyzed by trypsin at neutral pH value, and keeps the sensitivity characteristic of casein to pH value, so that the casein has intestinal targeting.
The iron protein succinate is chelated with ferric iron and casein, and the casein has no fixed molecular formula and molecular weight as a mixture, so the iron protein succinate also has no fixed chemical structural formula and molecular formula. The protein iron succinate prepared by the prior art has the advantages that most of the molecular weight is in the range of 300-2000kDa, the solubility of the protein iron succinate in water in the molecular weight range is poor, and the solution viscosity is high. In order to increase the solubility and stability of the protein iron succinate in water and facilitate the production and preparation of products such as oral liquid, the protein iron 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, chinese patent CN104402984B provides a method for preparing protein succinic acid with high iron content, by controlling the pH value of the environment when casein reacts with succinic anhydride, and controlling the method and time for dropping ferric trichloride solution containing sodium bicarbonate into succinic acid protein solution for reaction, the iron content of protein succinic acid is improved, and the iron content of prepared protein succinic acid is 5.1%.
For example, chinese patent CN102671189B provides a method for solubilising protein iron succinate, which comprises mixing and stirring protein iron succinate with solubilising agent (sodium dodecyl sulfate, poloxamer, PEG-400, beta-cyclodextrin), excipient (sorbitol) and latent solvent (propylene glycol) under alkaline condition, so as to improve solubility of protein iron succinate in water, and make the content of free iron in the prepared oral liquid not more than 0.1% of the total content.
For example, chinese patent CN102838667B provides a method for preparing protein iron succinate, which comprises the steps of adjusting and controlling the weight ratio of casein to succinic anhydride, the weight ratio of succinic acid protein to ferric trichloride, and the pH value in the reaction process, so as to prepare protein iron succinate with high acylation degree, large iron carrying capacity, good solubility, stable quality, low impurity content and remarkable curative effect.
However, none of the above methods for producing protein iron succinate is effective in controlling the molecular weight of the produced protein iron succinate.
For example, chinese patent application CN106589103a provides a method for preparing protein iron succinate, firstly, using ultrafiltration membrane with molecular weight cut-off of 500 kDa-1000 kDa to separate acylated liquid membrane to obtain filtrate, regulating pH value, then using ultrafiltration membrane with molecular weight of 100 kDa-300 kDa to make membrane separation of acylated liquid filtrate, removing permeate to obtain acylated casein solution, adding FeCl 3 Sequentially treating the reaction product by using ultrafiltration membranes with the molecular weight cut-off of 500 kDa-1000 kDa and 100 kDa-300 kDa, and adding acid to precipitate to obtain the protein iron succinate with the corresponding molecular weight. The method uses ultrafiltration membrane, which is complex, increases cost, and the prepared protein succinic acid iron has low resolubility and stability.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method of protein iron succinate, which is realized by the following technology.
The preparation method of the protein iron succinate comprises the following steps:
s1, acylation: preparing casein into aqueous solution, continuously performing first ultrasonic treatment, adding succinic anhydride into the casein solution for reaction, and continuously adding 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 succinyl protein wet solid;
s2, carrying out crude iron: adding sodium hydroxide solution into the succinyl protein wet solid obtained in the step S1 while stirring to completely dissolve the succinyl protein wet solid, wherein the pH value of the solution after dissolution is 7-8; continuously performing the second ultrasonic treatment on the solution system, dropwise adding ferric trichloride solution and 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 completed; after the reaction is finished, adding acid to adjust the pH value of the reaction solution to 2-3, separating out protein succinic acid iron, and stopping ultrasonic treatment; filtering and washing to obtain crude protein succinic acid iron with the iron content of 1-5%;
s3, refining: adding sodium hydroxide solution into the crude protein iron succinate product obtained in the step S2 while stirring to dissolve the crude protein iron succinate product completely, shearing a solution system, and controlling the molecular weight of the protein iron succinate to be 300-500kDa; adding a propping agent, uniformly stirring, and spray-drying to obtain a finished product of the protein iron succinate; the propping agent is lactose and/or fructose.
The preparation method of the protein iron succinate comprises three treatment stages of acylation, crude iron carrying and refining; the molecular weight of the protein succinic acid iron after the shearing treatment is controlled in the refining process by adopting ultrasonic treatment in the acylation and iron-carrying crude process, and the protein succinic acid iron with the molecular weight is matched with a propping agent, so that the molecular weight of the protein succinic acid iron prepared by final spray drying is still kept in the range of 300-500kDa, and the molecular weight of the protein succinic acid iron is not greatly changed compared with the molecular weight of the protein succinic acid iron controlled after the shearing treatment. The final prepared protein succinic acid iron finished product has good redissolution effect after being dissolved by water, and free iron is avoided. The acid solution can be common organic weak acid such as lactic acid, malic acid, etc. The propping agent can only play the role when lactose and fructose are selected, and the technical effect cannot be obtained when other saccharides such as sucrose are selected. Spray drying can be performed using parameters currently common in the industry.
The protein iron succinate prepared by the method can be used as a food additive to be applied to infant complementary foods and milk powder.
Preferably, the ultrasonic frequencies of the first ultrasonic treatment and the second ultrasonic treatment are sequentially reduced. The ultrasonic frequency of ultrasonic treatment adopts a mode of gradually decreasing, so that the molecular weight range of the prepared protein iron succinate can be initially controlled.
Preferably, the frequency of the first sonication is 35-45kHz and the power of the second sonication is 20-30kHz.
More preferably, the power of the first sonication is 40kHz and the power of the second sonication is 25kHz.
Preferably, in step S2, the iron carrying amount of the crude protein succinic acid iron product is 1-2%.
Preferably, in the step S3, the weight ratio of the propping agent to the crude product of the protein succinic acid is 4-5:1.
More preferably, in step S3, the weight ratio of the proppants to the crude protein succinic acid iron is 4.5:1.
Preferably, in step S3, the rate of shearing is 600-800rpm.
Compared with the prior art, the invention has the following advantages: the molecular weight of the protein iron succinate prepared by final spray drying is not greatly changed compared with the molecular weight of the protein iron succinate after shearing, and is still effectively controlled in a smaller range of 300-500kDa by respectively adopting ultrasonic treatment with specific frequency in two reaction stages of acylation and iron-carrying crude preparation and shearing treatment in a refining stage and matching with a propping agent, so that the prepared protein iron succinate has good solubility and stability when being used as products such as protein iron succinate oral liquid; free iron is not produced after redissolution.
Detailed Description
The following description of the present invention will be made clearly and fully, and it is apparent that the embodiments described are only some, but not all, of the embodiments of the present invention. All other embodiments, which can be made by one of ordinary skill in the art without undue burden on the person of ordinary skill in the art based on embodiments of the present invention, are within the scope of the present invention.
Example 1
This example prepares protein iron succinate according to the following method:
s1, acylation: preparing casein into an aqueous solution and continuously performing first ultrasonic treatment with ultrasonic frequency of 40kHz; 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 to be about 8.5; after the reaction is finished, dropwise adding a malic acid solution to adjust the pH value of the reaction solution to about 2.5, and stopping ultrasonic treatment; filtering to obtain precipitate to obtain succinyl protein wet solid;
s2, carrying out crude iron: adding sodium hydroxide solution into the succinyl protein wet solid obtained in the step S1 while stirring to completely dissolve the succinyl protein wet solid, wherein the pH value of the solution after dissolution is about 8.0; continuously performing second ultrasonic treatment on the solution system, wherein the ultrasonic frequency is 25kHz; dropwise adding ferric trichloride solution and sodium hydroxide solution to maintain the pH value of the reaction solution at about 6.5, and continuously stirring for reaction for 3 hours after the dropwise adding of the ferric trichloride solution is completed; after the reaction is finished, malic acid is dripped to adjust the pH value of the reaction solution to about 2.5, so that protein iron succinate is separated out, and the ultrasonic treatment is stopped; filtering and washing to obtain crude protein succinic acid iron with iron content of about 2%;
s3, refining: adding sodium hydroxide solution into the crude protein iron succinate product obtained in the step S2 while stirring to dissolve the crude protein iron succinate product completely, shearing the solution system at the shearing speed of 700rpm, and controlling the molecular weight of the protein iron succinate to be 300-500kDa; adding lactose (propping agent) and uniformly stirring, wherein the weight ratio of lactose to the crude product of protein succinic acid is 4.5:1; spray drying is carried out according to the mode that the air inlet temperature is 150-160 ℃ and the air outlet temperature is 90-100 ℃ to obtain the finished product of the protein iron succinate.
Example 2
The method for preparing protein iron succinate of this example differs from example 1 in that the frequency of the first ultrasonic treatment of step S1 is 35kHz; the frequency of the second sonication was 20kHz.
Example 3
The method for preparing protein iron succinate of this example differs from example 1 in that the frequency of the first ultrasonic treatment of step S1 is 45kHz; the frequency of the second sonication was 30kHz.
Example 4
The process for preparing iron protein succinate in this example differs from that in example 1 in that in step S3, the weight ratio of lactose to crude iron protein succinate is 5:1.
Example 5
The process for preparing iron protein succinate in this example differs from that in example 1 in that in step S3, the weight ratio of lactose to crude iron protein succinate is 4:1.
Example 6
The method for preparing protein iron succinate of this example is different from that of example 1 in that lactose is replaced with fructose in step S3, and the amount of fructose is the same as that of example 1.
Example 7
The difference between the method for preparing iron protein succinate in this example and the method in example 1 is that in step S3, lactose and fructose with the same weight are selected as the propping agent, 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
When the iron protein succinate is prepared in this comparative example, ultrasonic and shearing treatments are not performed, and the concrete steps are as follows:
s1, acylation: preparing casein into an aqueous solution, adding succinic anhydride for reaction 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 succinyl protein wet solid;
s2, carrying out crude iron: adding sodium hydroxide solution into the succinyl protein wet solid obtained in the step S1 while stirring to completely dissolve the succinyl protein wet solid, wherein the pH value of the solution after dissolution is about 8.0; dropwise adding ferric trichloride solution and sodium hydroxide solution to maintain the pH value of the reaction solution at about 6.5, and continuously stirring for reaction for 3 hours after the dropwise adding of the ferric trichloride solution is completed; after the reaction is finished, malic acid is dripped to adjust the pH value of the reaction solution to about 2.5, so that protein iron succinate is separated out; filtering and washing to obtain crude protein succinic acid iron with iron content of about 2%;
s3, refining: adding sodium hydroxide solution into the crude protein succinic acid iron product obtained in the step S2 while stirring to completely dissolve the crude protein succinic acid iron product; adding lactose (propping agent) and uniformly stirring, wherein the weight ratio of lactose to the crude product of protein succinic acid is 4.5:1; spray drying is carried out according to the mode that the air inlet temperature is 150-160 ℃ and the air outlet temperature is 90-100 ℃ to obtain the finished product of the protein iron succinate.
Comparative example 2
When the protein iron succinate is prepared in the comparative example, lactose (propping agent) is not added in the step S3, and malic acid is dropwise added as a pH value regulator, specifically as follows:
s1, acylation: preparing casein into an aqueous solution and continuously performing first ultrasonic treatment with ultrasonic frequency of 40kHz; 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 to be about 8.5; after the reaction is finished, dropwise adding a malic acid solution to adjust the pH value of the reaction solution to about 2.5, and stopping ultrasonic treatment; filtering to obtain precipitate to obtain succinyl protein wet solid;
s2, carrying out crude iron: adding sodium hydroxide solution into the succinyl protein wet solid obtained in the step S1 while stirring to completely dissolve the succinyl protein wet solid, wherein the pH value of the solution after dissolution is about 8.0; continuously performing second ultrasonic treatment on the solution system, wherein the ultrasonic frequency is 25kHz; dropwise adding ferric trichloride solution and sodium hydroxide solution to maintain the pH value of the reaction solution at about 6.5, and continuously stirring for reaction for 3 hours after the dropwise adding of the ferric trichloride solution is completed; after the reaction is finished, malic acid is dripped to adjust the pH value of the reaction solution to about 2.5, so that protein iron succinate is separated out, and the ultrasonic treatment is stopped; filtering and washing to obtain crude protein succinic acid iron with iron content of about 2%;
s3, refining: adding sodium hydroxide solution into the crude protein iron succinate product obtained in the step S2 while stirring to dissolve the crude protein iron succinate product completely, shearing the solution system at the shearing speed of 700rpm, and controlling the molecular weight of the protein iron succinate to be 300-500kDa; dripping malic acid to adjust pH value to 2-3 to precipitate protein succinic acid iron to form suspension, and spray drying at air inlet temperature of 150-160deg.C and air outlet temperature of 90-100deg.C to obtain protein succinic acid iron product.
Comparative example 3
When the comparative example is used for preparing protein iron succinate, lactose is not added, ultrasonic and shearing treatment is not carried out, and malic acid is dripped to serve as a pH value regulator, and the method specifically comprises the following steps:
s1, acylation: preparing casein into an aqueous solution, adding succinic anhydride for reaction 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 succinyl protein wet solid;
s2, carrying out crude iron: adding sodium hydroxide solution into the succinyl protein wet solid obtained in the step S1 while stirring to completely dissolve the succinyl protein wet solid, wherein the pH value of the solution after dissolution is about 8.0; dropwise adding ferric trichloride solution and sodium hydroxide solution to maintain the pH value of the reaction solution at about 6.5, and continuously stirring for reaction for 3 hours after the dropwise adding of the ferric trichloride solution is completed; after the reaction is finished, malic acid is dripped to adjust the pH value of the reaction solution to about 2.5, so that protein iron succinate is separated out; filtering and washing to obtain crude protein succinic acid iron with iron content of about 2%;
s3, refining: adding sodium hydroxide solution into the crude protein succinic acid iron product obtained in the step S2 while stirring to completely dissolve the crude protein succinic acid iron product; dripping malic acid to adjust pH value to 2-3 to precipitate protein succinic acid iron to form suspension, and spray drying at air inlet temperature of 150-160deg.C and air outlet temperature of 90-100deg.C to obtain protein succinic acid iron product.
Comparative example 4
The method for preparing protein iron succinate of this comparative example is different from example 1 in that the frequency of the first ultrasonic treatment of step S1 is 30kHz; in step S2, the second ultrasonic treatment is not performed.
Comparative example 5
The method for preparing protein iron succinate of this comparative example is different from example 1 in that the frequency of the first ultrasonic treatment of step S1 is 50kHz; the frequency of the second sonication of step S2 was 40kHz.
Comparative example 6
The method for preparing protein iron succinate of this comparative example is different 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 adjustor. The specific method comprises the following steps:
s1, acylation: preparing casein into an aqueous solution, adding succinic anhydride for reaction 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 succinyl protein wet solid;
s2, carrying out crude iron: adding sodium hydroxide solution into the succinyl protein wet solid obtained in the step S1 while stirring to completely dissolve the succinyl protein wet solid, wherein the pH value of the solution after dissolution is about 8.0; dropwise adding ferric trichloride solution and sodium hydroxide solution to maintain the pH value of the reaction solution at about 6.5, and continuously stirring for reaction for 3 hours after the dropwise adding of the ferric trichloride solution is completed; after the reaction is finished, malic acid is dripped to adjust the pH value of the reaction solution to about 2.5, so that protein iron succinate is separated out; filtering and washing to obtain crude protein succinic acid iron with iron content of about 2%;
s3, refining: adding sodium hydroxide solution into the crude protein iron succinate product obtained in the step S2 while stirring to dissolve the crude protein iron succinate product completely, shearing the solution system at the shearing speed of 700rpm, and controlling the molecular weight of the protein iron succinate to be 300-500kDa; adding sucrose and stirring uniformly, wherein the weight ratio of sucrose to the crude product of protein succinic acid iron is 4.5:1; dripping malic acid to regulate pH value to about 2.5 to separate out protein succinic acid iron to form suspension, and spray drying at 150-160 deg.c and 90-100 deg.c to obtain protein succinic acid iron product.
Application example:
1. the molecular weight of the prepared protein iron succinate is determined by adopting an SDS-polyacrylamide gel electrophoresis method, and the molecular weight range of the finished product of the protein iron succinate prepared in the embodiment 1 and the comparative example 1 comprises 300-500kDa and the distribution span is far more than 300-500kDa, namely the small end value of the molecular weight range is far less than 300kDa and the large end value is far more than 500kDa; 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 final iron protein succinate product prepared is similar to that of comparative example 1, and the distribution span is larger; the molecular weight range of the finished product of the protein succinic acid iron prepared in the comparative example 3 is larger than that of the comparative example 1; the molecular weight distribution range of the protein iron succinate of comparative example 4 has a small end value of more than 300kDa and a large end value of more than 500kDa; the molecular weight distribution range of the protein iron succinate of comparative example 5 has a small end value of less than 300kDa and a large end value of less than 500kDa; comparative example 6 in the preparation of iron protein succinate, although the molecular weight range after shearing was controlled within 300-500kDa, the molecular weight range of the final iron protein succinate product prepared was similar to that of comparative example 1, and the distribution span was relatively large.
2. At room temperature, 13 groups of 100mL of ultrapure water were taken, respectively, to which several weights of the iron protein succinate prepared in examples 1 to 7 and comparative examples 1 to 6 were added, and shaking was performed for 30 seconds every 5 minutes, and the dissolution of the iron protein succinate after 30 minutes was observed.
After testing, the solubility of the protein iron succinate of the examples 1-7 is better than that of the comparative examples 1-6; wherein, the solubility of the protein succinic acid iron in the examples 1, 6 and 7 is optimal and the three are not different, the solubility of the protein succinic acid iron in the examples 2 and 5 is slightly smaller than that in the example 1, and the solubility of the protein succinic acid iron in the examples 3 and 4 is slightly larger than that in the example 1; the solubility of the iron protein succinate of comparative example 3 was the smallest, the solubility of the iron protein succinate of comparative examples 1 to 4, 6 was smaller than that of example 1, and the solubility of the iron protein succinate of comparative example 5 was not much different from that of example 1.
3. The preparation method of the oral liquid by taking the protein iron succinate prepared in the examples 1-7 and the comparative examples 1-6 as raw materials comprises the following steps: adding 6g of protein iron succinate into purified water, adding sodium hydroxide solution to adjust the pH value to about 8.0, and stirring until the protein iron succinate is completely dissolved; adding sodium hydroxy phenyl propyl ester as antiseptic, stirring to dissolve, adding malic acid dropwise to adjust pH to 7.5, adding essence and saccharin sodium 0.1g each, and adding water to volume to 100mL to obtain the final product.
The free iron content of the oral liquid prepared by taking the protein succinic acid iron prepared in the examples 1-7 and the comparative examples 1-6 as raw materials is respectively measured, the free iron content of the oral liquid in the examples 1-7 is not detected, the free iron content of the oral liquid corresponding to the comparative examples 1 and 2 is 0.009% and 0.012%, the free iron content of the oral liquid corresponding to the comparative example 3 is 0.023%, the free iron content of the oral liquid corresponding to the comparative example 4 is 0.005%, the free iron content of the oral liquid corresponding to the comparative example 5 is 0.002%, and the free iron content of the oral liquid corresponding to the comparative example 6 is 0.003%.
The test results show that the molecular weight of the protein iron succinate can be effectively controlled within the range of 300-500kDa by carrying out proper ultrasonic and shearing treatment in the preparation process of the protein iron succinate and adding a proper amount of specific propping agent (lactose or fructose) in the final refining process, the prepared protein iron succinate product has better redissolution performance, and no free iron is produced in the preparation process of the oral liquid.
Claims (8)
1. The preparation method of the protein succinic acid iron is characterized by comprising the following steps:
s1, acylation: preparing casein into aqueous solution, continuously performing first ultrasonic treatment, adding succinic anhydride into the casein solution for reaction, and continuously adding 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 succinyl protein wet solid;
s2, carrying out crude iron: adding sodium hydroxide solution into the succinyl protein wet solid obtained in the step S1 while stirring to completely dissolve the succinyl protein wet solid, wherein the pH value of the solution after dissolution is 7-8; continuously performing the second ultrasonic treatment on the solution system, dropwise adding ferric trichloride solution and 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 completed; after the reaction is finished, adding acid to adjust the pH value of the reaction solution to 2-3, separating out protein succinic acid iron, and stopping ultrasonic treatment; filtering and washing to obtain crude protein succinic acid iron with the iron content of 1-5%;
s3, refining: adding sodium hydroxide solution into the crude protein iron succinate product obtained in the step S2 while stirring to dissolve the crude protein iron succinate product completely, shearing a solution system, and controlling the molecular weight of the protein iron succinate to be 300-500kDa; adding a propping agent, uniformly stirring, and spray-drying to obtain a finished product of the protein iron succinate; the propping agent is lactose and/or fructose.
2. The method for producing protein iron succinate according to claim 1, wherein the ultrasonic frequencies of the first ultrasonic treatment and the second ultrasonic treatment are sequentially decreased.
3. The method for preparing protein iron succinate according to claim 2, wherein the frequency of the first ultrasonic treatment is 35-45kHz and the power of the second ultrasonic treatment is 20-30kHz.
4. A method for preparing protein iron succinate according to claim 3, wherein the power of the first ultrasonic treatment is 40kHz and the power of the second ultrasonic treatment is 25kHz.
5. The method for producing iron protein succinate according to claim 1, wherein in step S2, the iron carrying amount of the crude iron protein succinate is 1-2%.
6. The method for preparing protein iron succinate according to claim 1, wherein in the step S3, the weight ratio of the propping agent to the crude protein iron succinate is 4-5:1.
7. The method of 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 for producing protein iron succinate according to claim 1, wherein in the step S3, the shearing rate is 600-800rpm.
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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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