Water-soluble pearl powder and preparation process thereof
By using lactate sparingly to convert calcium carbonate and employing it as an enzyme catalyst, the process addresses inefficiencies in existing methods, achieving reduced costs and faster protein hydrolysis for water-soluble pearl powder production.
Patent Information
- Application Number
- CN202510356111.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-03-25
- Publication Date
- 2025-07-15
AI Technical Summary
Excessive use of lactic acid in the existing water-soluble pearl powder preparation process leads to high process cost and low enzymatic efficiency, making it difficult to achieve efficient and low-cost preparation.
By combining lactic acid hydrolysis and enzymatic lysis, the amount of lactic acid is controlled to convert calcium carbonate into calcium lactate, and lactic acid solution is used as an enzymatic lysis promoter during the enzymatic lysis process, and calcium ions are used to catalyze the enzymatic lysis process to shorten the enzymatic lysis time.
Effectively save the dosage of lactic acid, shorten the enzymatic lysis time, improve the enzymatic lysis efficiency, and reduce the preparation cost.
Abstract
Description
Technical Field
[0001] The present invention belongs to the field of biotechnology, and particularly relates to a water-soluble pearl powder and a preparation process thereof. Background Art
[0002] Water-soluble pearl powder, also known as instant pearl powder and enzymatically hydrolyzed pearl powder, its active ingredients mainly include various amino acids, minerals (such as calcium, magnesium, zinc, manganese, iron, strontium, selenium, titanium, etc.), trace elements (such as selenium, zinc, germanium, vanadium, copper, phosphorus, potassium, sodium, etc.), active nutritional components (such as taurine, pearl polypeptide, etc.) and other components. Due to its good water solubility, it has a high absorption rate by the human body and is more favored than ordinary pearl powder.
[0003] Since the main components of pearls are calcium carbonate and scleroprotein, the existing preparation process of water-soluble pearl powder mainly adopts a combination of acid hydrolysis and enzymatic hydrolysis. That is, first, lactic acid reacts with calcium carbonate to convert insoluble calcium carbonate into water-soluble calcium lactate and free the scleroprotein therein; then the lactic acid solution is separated from the scleroprotein, and the scleroprotein is separately enzymatically hydrolyzed; finally, the lactic acid solution and the enzymatic hydrolysate are combined, concentrated and dried to obtain the water-soluble pearl powder.
[0004] The disadvantage of this preparation process is that in order to fully enzymatically hydrolyze the scleroprotein, generally an excessive amount of lactic acid is added. Part of this lactic acid converts calcium carbonate into calcium lactate, and part of it preliminarily hydrolyzes the scleroprotein to convert it into polypeptides with relatively small molecular weights; however, the hydrolysis of scleroprotein by lactic acid is very crude and has little impact on the subsequent enzymatic hydrolysis process, and it also causes excessive use of lactic acid, increasing the process cost. Summary of the Invention
[0005] The invention object of the present invention is to provide a water-soluble pearl powder and a preparation process thereof. The preparation process is simple and efficient, not only shortening the process flow time, but also saving costs.
[0006] To achieve the above invention object, the technical solution of the present invention is as follows: A preparation process of a water-soluble pearl powder, the preparation process includes the following steps: (1) Grinding and pulverizing pearls to make a slurry; (2) Hydrolyzing the slurry with lactic acid to obtain a lactic acid solution and a protein precipitate respectively; (3) Taking a part of the lactic acid solution as an enzymatic hydrolysis promoter, adding an enzyme and the enzymatic hydrolysis promoter to the protein precipitate for enzymatic hydrolysis to obtain an enzymatic hydrolysate; (4) Combining the lactic acid solution obtained in step (2) and the enzymatic hydrolysate obtained in step (3), concentrating and drying to obtain the water-soluble pearl powder.
[0007] The present invention also adopts a method combining lactic acid hydrolysis and enzymatic hydrolysis. However, the amount of lactic acid in step (2) is relatively small and is only used to convert calcium carbonate into calcium lactate. After separating the protein precipitate from the lactic acid solution, a part of the lactic acid solution is in-situ obtained to prepare an enzymatic hydrolysis promoter. When the protein precipitate is enzymatically hydrolyzed in the presence of the enzymatic hydrolysis promoter, the calcium ions contained in the enzymatic hydrolysis promoter play a catalytic role in the enzymatic hydrolysis process, enabling the enzymatic hydrolysis process to proceed more rapidly and shortening the enzymatic hydrolysis time.
[0008] In step (1) of the above preparation process, the pearls are crushed and then sieved through a 100-mesh sieve, and then made into a slurry with deionized water.
[0009] In step (2) of the above preparation process, after heating the slurry to 90 °C, lactic acid is added to the slurry according to the volume ratio of slurry: lactic acid of 1: (150 - 180), and then hydrolyzed at 90 - 100 °C for 100 - 120 min. In the present invention, the dosage of lactic acid can be saved by more than 16%, and the hydrolysis time can also be shortened by 17%.
[0010] Step (3) of the above preparation process includes: (a) The protein precipitate is washed with deionized water, then deionized water and an enzymatic hydrolysis promoter are added, and the pH of the reaction system is adjusted to 7.4 - 7.6 with Ca(OH)2; (b) The concentration of calcium ions in the reaction system is adjusted to 0.0008 - 0.001 mol / L with deionized water; (c) An enzyme is added to the reaction system for enzymatic hydrolysis.
[0011] In step (a), the protein precipitate is washed to remove the residual lactic acid solution in the protein, so as to better adjust the concentration of calcium ions in the reaction system subsequently; the filtrate after washing the protein precipitate can also be retained and merged with the lactic acid solution and the enzymatic hydrolysate in step (4). Of course, it is also feasible to directly adjust the calcium ion concentration in the protein precipitate without washing it.
[0012] In step (b), with the promotion of calcium ions at 0.0008 - 0.001 mol / L, the enzymatic hydrolysis process can be completed more quickly.
[0013] In step (b) of the above preparation process, the content of calcium ions in the reaction system is first measured by the EDTA titration method, and then the calcium ion concentration is adjusted. In addition to the EDTA titration method, a variety of known methods can also be used to measure the calcium ion concentration, and the present invention has no special limitation on this.
[0014] In step (c) of the above preparation process, the enzyme is neutral protease.
[0015] In step (c) of the above preparation process, the mass-volume ratio of the enzyme to the reaction system is (0.1 - 0.15 g): 100 mL.
[0016] In step (c) of the above preparation process, first heat the reaction system to 50 - 55 °C, then add two-thirds of the enzyme amount, and enzymolyze for 120 - 150 min; then continue to add the remaining one-third of the enzyme amount and enzymolyze for 100 - 120 min. Adding the enzyme in portions can enable the enzyme to fully participate; in the presence of the enzymatic hydrolysis promoter, the enzymatic hydrolysis time is shortened by more than 25%.
[0017] The present invention also provides a water-soluble pearl powder, which is prepared by the above preparation process.
[0018] Compared with the prior art, the technical effects of the present invention are reflected in: The present invention adopts a combination of lactic acid hydrolysis and enzymatic hydrolysis to prepare water-soluble pearl powder, but the amount of lactic acid used in the lactic acid hydrolysis step is relatively small, only used to convert calcium carbonate into calcium lactate; after separating the protein precipitate from the lactic acid solution, a part of the lactic acid solution is in-situ obtained to make an enzymatic hydrolysis promoter. When using the enzyme to enzymolyze the protein precipitate in the presence of the enzymatic hydrolysis promoter, the calcium ions contained in the enzymatic hydrolysis promoter play a catalytic role in the enzymatic hydrolysis process, which can promote the enzymatic hydrolysis process to proceed more rapidly and shorten the enzymatic hydrolysis time.
[0019] Example 1 The preparation process of a water-soluble pearl powder in this example includes the following steps: (1) Grind and crush pearls to make a slurry. Specifically, first wash and dry the pearls, then grind and crush them, pass through a 100-mesh sieve to obtain pearl powder, and then add deionized water to make a slurry (add in small amounts multiple times, and the less the amount of deionized water used, the better under the condition of ensuring the formation of the slurry). (2) Hydrolyze the slurry with lactic acid to obtain lactic acid solution and protein precipitate respectively. Specifically, first heat the slurry to 90 °C, then add lactic acid to the slurry according to the volume ratio of slurry: lactic acid of 1:150, and then hydrolyze in a 95 °C water bath for 100 min; after the hydrolysis is completed, separate the solution and the precipitate to obtain lactic acid solution and protein precipitate respectively. The protein precipitate is washed with deionized water and reserved for use, and the filtrate after washing the protein precipitate can also be reserved for use. (3) Take a part of the lactic acid solution as the enzymatic hydrolysis promoter, add the enzyme and the enzymatic hydrolysis promoter to the washed protein precipitate to carry out enzymatic hydrolysis to obtain an enzymatic hydrolysate. Specifically, first use the EDTA titration method to measure the calcium ion concentration in the lactic acid solution. Then, take a portion of the lactic acid solution as an enzymatic hydrolysis promoter, add it to the protein precipitate, and adjust the pH of the reaction system to 7.4 - 7.6 using Ca(OH)₂. Then, measure the calcium ion concentration in the reaction system again using the EDTA titration method, and adjust the calcium ion concentration in the reaction system to 0.0008 mol / L using deionized water. Then, raise the temperature of the reaction system to 50 °C, and weigh neutral protease (enzyme activity 200000 U / g) according to the mass-volume ratio of enzyme to reaction system of 0.1 g:100 mL. First, add two-thirds of the enzyme amount to the reaction system and perform enzymatic hydrolysis for 120 min. Then, continue to add the remaining one-third of the enzyme amount and perform enzymatic hydrolysis for 100 min. (4) Combine the lactic acid solution, filtrate obtained in step (2), and the enzymatic hydrolysate obtained in step (3), concentrate, and then vacuum dry to obtain the water-soluble pearl powder of this example.
[0020] Example 2 The preparation process of a water-soluble pearl powder in this example includes the following steps: (1) Grind and crush pearls to make a slurry. Specifically, first wash and dry the pearls, then grind and crush them, pass through a 100-mesh sieve to obtain pearl powder, and then add deionized water to make a slurry (add in small amounts multiple times, and use as little deionized water as possible while ensuring the formation of a slurry). (2) Hydrolyze the slurry with lactic acid to obtain a lactic acid solution and a protein precipitate respectively. Specifically, first heat the slurry to 90 °C, then add lactic acid to the slurry according to the volume ratio of slurry:lactic acid of 1:170, and then hydrolyze in a 100 °C water bath for 110 min. After hydrolysis, separate the solution and the precipitate to obtain a lactic acid solution and a protein precipitate respectively. The protein precipitate is washed with deionized water and reserved for use. The filtrate after washing the protein precipitate can also be reserved for use. (3) Take a portion of the lactic acid solution as an enzymatic hydrolysis promoter, add an enzyme and the enzymatic hydrolysis promoter to the washed protein precipitate to perform enzymatic hydrolysis to obtain an enzymatic hydrolysate. Specifically, first use the EDTA titration method to measure the calcium ion concentration in the lactic acid solution. Then, take a part of the lactic acid solution as an enzymatic hydrolysis promoter, add it to the protein precipitate, and adjust the pH of the reaction system to 7.4 - 7.6 using Ca(OH)₂. Then, use the EDTA titration method again to measure the calcium ion concentration in the reaction system, and adjust the calcium ion concentration in the reaction system to 0.0009 mol / L using deionized water. Then, raise the temperature of the reaction system to 53°C, and weigh neutral protease (enzyme activity 200000 U / g) according to the mass-volume ratio of enzyme to reaction system of 0.12 g:100 mL. First, add two-thirds of the enzyme amount to the reaction system and perform enzymatic hydrolysis for 140 min. Then, continue to add the remaining one-third of the enzyme amount and perform enzymatic hydrolysis for 110 min. (4) Combine the lactic acid solution, filtrate obtained in step (2), and the enzymatic hydrolysate obtained in step (3), concentrate and then dry in vacuum to obtain the water-soluble pearl powder of this example.
[0021] Example 3 The preparation process of a water-soluble pearl powder in this example includes the following steps: (1) Grind and crush pearls to make a slurry. Specifically, first wash and dry the pearls, then grind and crush them, pass through a 100-mesh sieve to obtain pearl powder, and then add deionized water to make a slurry (add in small amounts multiple times, and the less deionized water is used under the condition of ensuring the formation of the slurry, the better). (2) Hydrolyze the slurry with lactic acid to obtain a lactic acid solution and a protein precipitate respectively. Specifically, first heat the slurry to 90°C, then add lactic acid to the slurry according to the volume ratio of slurry:lactic acid of 1:180, and then hydrolyze in a 100°C water bath for 120 min. After hydrolysis, separate the solution and the precipitate to obtain a lactic acid solution and a protein precipitate respectively. The protein precipitate is washed with deionized water and reserved for use. The filtrate after washing the protein precipitate can also be reserved for use. (3) Take a part of the lactic acid solution as an enzymatic hydrolysis promoter, add an enzyme and the enzymatic hydrolysis promoter to the washed protein precipitate for enzymatic hydrolysis to obtain an enzymatic hydrolysate. Specifically, first use the EDTA titration method to measure the calcium ion concentration in the lactic acid solution. Then, take a portion of the lactic acid solution as an enzymatic hydrolysis promoter, add it to the protein precipitate, and adjust the pH of the reaction system to 7.4 - 7.6 using Ca(OH)₂. Then, measure the calcium ion concentration in the reaction system again using the EDTA titration method, and adjust the calcium ion concentration in the reaction system to 0.001 mol / L using deionized water. Then, raise the temperature of the reaction system to 55°C, and weigh neutral protease (enzyme activity 200000 U / g) according to the mass-to-volume ratio of enzyme to reaction system of 0.15 g : 100 mL. First, add two-thirds of the enzyme amount to the reaction system and perform enzymatic hydrolysis for 150 min. Then, continue to add the remaining one-third of the enzyme amount and perform enzymatic hydrolysis for 120 min. (4) Combine the lactic acid solution, filtrate obtained in step (2), and the enzymatic hydrolysate obtained in step (3), concentrate, and then vacuum dry to obtain the water-soluble pearl powder of this example.
[0022] Comparative Example 1 The preparation process of a water-soluble pearl powder in this example includes the following steps: (1) Grind and crush pearls to make a slurry. Specifically, first wash and dry the pearls, then grind and crush them, pass through a 100-mesh sieve to obtain pearl powder, and then add deionized water to make a slurry (add in small amounts multiple times, and use as little deionized water as possible while ensuring the formation of a slurry). (2) Hydrolyze the slurry with lactic acid to obtain a lactic acid solution and a protein precipitate respectively. Specifically, first heat the slurry to 90°C, then add lactic acid to the slurry according to the volume ratio of slurry : lactic acid of 1 : 220, and then hydrolyze in a 100°C water bath for 120 min. After hydrolysis, separate the solution and the precipitate to obtain a lactic acid solution and a protein precipitate respectively. The protein precipitate is washed with deionized water and set aside for later use. The filtrate after washing the protein precipitate can also be set aside for later use. (3) Add an enzyme and an enzymatic hydrolysis promoter to the washed protein precipitate for enzymatic hydrolysis to obtain an enzymatic hydrolysate. Specifically, resuspend the protein precipitate with deionized water and adjust the pH of the reaction system to 7.4 - 7.6 using Ca(OH)₂. Then, raise the temperature of the reaction system to 55°C, and weigh neutral protease (enzyme activity 200000 U / g) according to the mass-to-volume ratio of enzyme to reaction system of 0.3 g : 100 mL. First, add two-thirds of the enzyme amount to the reaction system and perform enzymatic hydrolysis for 180 min. Then, continue to add the remaining one-third of the enzyme amount and perform enzymatic hydrolysis for 180 min. (4) Combine the lactic acid solution, filtrate obtained in step (2), and the enzymatic hydrolysate obtained in step (3), concentrate, and then vacuum dry to obtain the water-soluble pearl powder of this comparative example.
[0023] Take the water-soluble pearl powder prepared in the above Examples 1-3 and Comparative Example 1, and use the nitrogen determination method in General Rules 0704 of the Third Part of the Chinese Pharmacopoeia 2020 Edition to test the nitrogen content of each water-soluble pearl powder. The results are shown in Table 1.
[0024] Table 1 Water-soluble pearl powder Nitrogen content (%) Example 1 0.205 Example 2 0.207 Example 3 0.206 Comparative Example 1 0.082 As can be seen from Table 1, after adding a part of lactic acid solution as an enzymatic hydrolysis promoter to the enzymatic hydrolysis process, not only is the enzymatic hydrolysis process more complete, but also the dosage of lactic acid can be saved in the early lactic acid hydrolysis stage, and at the same time, the time required for enzymatic hydrolysis can be shortened.
Claims
1. A preparation process of water-soluble pearl powder, characterized in that, It includes the following steps: (1) Grind and crush pearls to make a slurry; (2) Hydrolyze the slurry with lactic acid to obtain a lactic acid solution and a protein precipitate respectively; (3) Take a part of the lactic acid solution as an enzymatic hydrolysis promoter, add an enzyme and the enzymatic hydrolysis promoter to the protein precipitate for enzymatic hydrolysis to obtain an enzymatic hydrolysate; (4) Combine the lactic acid solution obtained in step (2) and the enzymatic hydrolysate obtained in step (3), concentrate and dry to obtain the water-soluble pearl powder.
2. The preparation process according to claim 1, characterized in that, In step (1), after crushing the pearls, pass them through a 100-mesh sieve, and then adjust them into a slurry with deionized water.
3. The preparation process according to claim 1, characterized in that, In step (2), after heating the slurry to 90 °C, add lactic acid to the slurry according to the volume ratio of slurry: lactic acid of 1: (150-180), and then hydrolyze at 90-100 °C for 100-120 min.
4. The preparation process according to claim 1, characterized in that, Step (3) includes: (a) Wash the protein precipitate with deionized water, then add deionized water and the enzymatic hydrolysis promoter, and adjust the pH of the reaction system to 7.4-7.6 with Ca(OH)2; (b) Adjust the concentration of calcium ions in the reaction system to 0.0008-0.001 mol / L with deionized water; (c) Add an enzyme to the reaction system for enzymatic hydrolysis.
5. The preparation process according to claim 4, characterized in that, In step (b), first measure the content of calcium ions in the reaction system by the EDTA titration method, and then adjust the calcium ion concentration.
6. The preparation process according to claim 4, characterized in that, In step (c), the enzyme is neutral protease.
7. The preparation process according to claim 4, characterized in that, In step (c), the mass-volume ratio of the enzyme to the reaction system is (0.1-0.15 g): 100 mL.
8. The preparation process according to claim 7, wherein In step (c), first heat the reaction system to 50-55 °C, then add two-thirds of the enzyme amount, and hydrolyze for 120-150 min; then continue to add the remaining one-third of the enzyme amount and hydrolyze for 100-120 min.
9. A water-soluble pearl powder, characterized in that, Prepared by the preparation process described in claims 1-8.