Wolfberry amino acid essence tablet and production method thereof

Abstract

The invention relates to the technical field of natural substance extraction, in particular to a Chinese wolfberry fruit amino acid essence tablet and a production method thereof. The production method comprises the steps of (1) degreasing, (2) enzymolysis, (3) alcohol precipitation, (4) pretreatment, (5) hydrolysis and (6) tabletting. Through proper pretreatment and enzymolysis technologies, the functional characteristics of the wolfberry amino acid powder can be remarkably improved, and the wolfberry amino acid powder is pressed into tablets and can be used as an additive to be added into products such as beverages and health-care foods, so that the nutritional value of the products is improved.

Description

Technical Field

[0001] The invention relates to the technical field of natural substance extraction, in particular to a wolfberry amino acid essence tablet and a production method thereof. Background Art

[0002] Lycium barbarum is a traditional Chinese medicinal material widely used in food and health products. Its main active ingredients include polysaccharides, carotenoids, flavonoids and amino acids. Among them, Lycium barbarum polysaccharides have attracted widespread attention due to their significant biological activities and health benefits, and many studies have focused on their extraction and application. However, there are relatively few studies on the extraction technology of amino acids in Lycium barbarum, and the existing technology mainly focuses on the extraction of polysaccharides.

[0003] Amino acids are the basic building blocks of proteins and have important physiological functions, such as promoting cell growth, repairing tissues and enhancing immunity. Although wolfberry contains a variety of amino acids, the current research on its amino acid extraction methods and technologies is still insufficient, resulting in its potential nutritional value not being fully utilized. Summary of the invention

[0004] In view of this, the purpose of the present invention is to provide a wolfberry amino acid essence tablet and a production method thereof, so as to improve the extraction efficiency, optimize the extraction conditions, and protect the active ingredients, thereby promoting the widespread application of wolfberry amino acids in the field of food and health products.

[0005] Based on the above purpose, the present invention provides a method for producing wolfberry amino acid essence tablets, comprising the following steps:

[0006] (1) defatting: defatting the wolfberry powder with n-hexane to obtain defatted wolfberry powder;

[0007] (2) Enzymatic hydrolysis: using composite enzyme 1 to enzymatically hydrolyze the defatted wolfberry powder to obtain an enzymatic hydrolyzate;

[0008] (3) Alcohol precipitation: using ethanol to precipitate the enzymatic hydrolysate to obtain enzymatic hydrolysate powder;

[0009] (4) Pretreatment: Add the enzymatic hydrolyzed powder to deionized water, adjust the pH to 7.5-8 with sodium hydroxide, raise the temperature to 80-85° C., stir and react for 48-72 hours, then adjust the pH to 4-5 with hydrochloric acid, centrifuge and vacuum dry to obtain wolfberry essence powder;

[0010] (5) hydrolysis: using compound enzyme 2 to hydrolyze the wolfberry essence powder to obtain wolfberry amino acid powder;

[0011] (6) Tablet pressing: The wolfberry amino acid powder is pressed into tablets by a tablet press to obtain wolfberry amino acid essence tablets.

[0012] Furthermore, in step (2), the compound enzyme 1 is a mixture of cellulase and pectinase in a weight ratio of 10-20:3-6.

[0013] Furthermore, in step (5), the compound enzyme 2 is a mixture of alkaline protease and alkaline amylase in a weight ratio of 2-4:0.5-1.5.

[0014] Preferably, in step (1), the weight ratio of wolfberry powder to n-hexane is 2:3-6.

[0015] Preferably, the degreasing temperature in step (1) is 55-60° C. and the degreasing time is 4-6 hours.

[0016] Preferably, the temperature of the enzymatic hydrolysis in step (2) is 50-60° C. and the time is 2-3 h.

[0017] Preferably, the temperature of the alcohol precipitation in step (3) is 2-5°C and the time is 24-36h.

[0018] Preferably, in step (4), the weight ratio of the enzymatic hydrolysis powder to deionized water is 1:10-20.

[0019] Preferably, the hydrolysis temperature in step (5) is 60-65° C. and the time is 4-6 h.

[0020] Furthermore, the present invention also provides a wolfberry amino acid essence tablet, which is obtained by the production method of the wolfberry amino acid essence tablet.

[0021] Furthermore, the present invention also provides an application of wolfberry amino acid essence tablets, which can be used as an additive to be added to beverages, health foods and other products to enhance their nutritional value.

[0022] Beneficial effects of the present invention:

[0023] The present invention uses cellulase and pectinase to process defatted wolfberry powder. Cellulase and pectinase effectively decompose cell walls and other biomacromolecules, promote the release of polysaccharides and proteins, greatly improve the extraction efficiency of amino acids, and lay a foundation for subsequent applications.

[0024] The present invention performs pretreatment before hydrolyzing and extracting amino acids, and the pretreatment effectively promotes the occurrence of the Maillard reaction, which not only improves the hydrolysis degree of the amino acids, but also generates more antioxidant components, thereby enhancing the overall antioxidant capacity.

[0025] The invention processes the wolfberry essence powder by compounding alkaline protease and alkaline amylase. The addition of alkaline amylase effectively improves the antioxidant property and hydrolysis degree of the wolfberry amino acid powder. Meanwhile, alkaline amylase adjusts the molecular chain structure and exposes more hydrophobic surfaces, thereby promoting the formation of a three-dimensional network structure through hydrophobic interaction, thereby further improving the emulsification activity and stability.

[0026] The present invention can significantly improve the functional properties of wolfberry amino acid powder through appropriate pretreatment and enzymolysis technology. These findings provide new technical support for the development and application of wolfberry amino acid, and also provide valuable reference for research in related fields. DETAILED DESCRIPTION

[0027] In order to make the objectives, technical solutions and advantages of the present invention more clearly understood, the present invention is further described in detail below in conjunction with specific embodiments.

[0028] The specification of cellulase in the specific embodiment of the present invention is 100,000 u / g, the specification of pectinase is 150,000 u / g, the specification of alkaline protease is 250,000 u / g, and the specification of alkaline amylase is 120,000 u / g. The above enzymes are all purchased from Shanghai Huashang Xiangyang Biotechnology Co., Ltd. The wolfberry powder comes from Zhongning County and is picked in early July with a moisture content of 12.5%.

[0029] Embodiment 1:

[0030] (1) Defatting: Add 10 g of wolfberry powder to 25 g of n-hexane, heat to 60° C., stir for 5 h, centrifuge, air-dry and sieve through an 80-mesh sieve to obtain defatted wolfberry powder;

[0031] (2) Enzymatic hydrolysis: Add 5 g defatted wolfberry powder to 100 g deionized water, then add 15 mg cellulase and 4.5 mg pectinase, adjust the pH to 5.6 with 0.1 mol / L hydrochloric acid, seal the cup with plastic wrap, heat to 55 °C, extract for 2.5 h, then heat to 100 °C, inactivate the enzyme for 5 min, filter, and obtain the enzymatic solution.

[0032] (3) Alcohol precipitation: add 50 g of the enzymatic hydrolysate to 250 g of 95% ethanol solution, cool to 4°C, let stand for 32 h, centrifuge, and vacuum dry to obtain enzymatic hydrolysate powder;

[0033] (4) Pretreatment: add 1 g of enzymatic hydrolysis powder to 15 g of deionized water, adjust the pH to 7.8 with 0.1 mol / L sodium hydroxide, raise the temperature to 80-85°C, stir and react for 60 h, then adjust the pH to 4.4 with 0.1 mol / L hydrochloric acid, centrifuge and vacuum dry to obtain wolfberry essence powder;

[0034] (5) Hydrolysis: 0.5 g of wolfberry essence powder was added to 15 g of deionized water, and then 3 mg of alkaline protease and 1 mg of alkaline amylase were added. The pH was adjusted to 8.2 with 0.1 mol / L sodium hydroxide, and the temperature was raised to 65° C., and the hydrolysis was carried out for 5 h. The temperature was then raised to 100° C., and the enzyme was inactivated for 5 min. The mixture was centrifuged, and the supernatant was freeze-dried to obtain wolfberry amino acid powder.

[0035] (6) Tablet pressing: The wolfberry amino acid powder is pressed into tablets by a tablet press to obtain wolfberry amino acid essence tablets.

[0036] Embodiment 2:

[0037] (1) Defatting: 10 g of wolfberry powder was added to 15 g of n-hexane, heated to 55°C, stirred for 4 h, centrifuged, air-dried, and sieved through an 80-mesh sieve to obtain defatted wolfberry powder;

[0038] (2) Enzymatic hydrolysis: Add 5 g defatted wolfberry powder to 80 g deionized water, then add 10 mg cellulase and 3 mg pectinase, adjust the pH to 5.2 with 0.1 mol / L hydrochloric acid, seal the cup with plastic wrap, heat to 50 °C, extract for 2 h, then heat to 100 °C, inactivate the enzyme for 3 min, filter, and obtain the enzymatic solution.

[0039] (3) Alcohol precipitation: add 50 g of enzymatic hydrolysate to 200 g of 95% ethanol solution, cool to 2°C, let stand for 24 h, centrifuge, and vacuum dry to obtain enzymatic hydrolysate powder;

[0040] (4) Pretreatment: 1 g of enzymatic hydrolysis powder was added to 10 g of deionized water, the pH was adjusted to 7.6 with 0.1 mol / L sodium hydroxide, the temperature was raised to 80°C, the reaction was stirred for 48 h, and the pH was adjusted to 4.1 with 0.1 mol / L hydrochloric acid, centrifuged, and vacuum dried to obtain wolfberry essence powder;

[0041] (5) Hydrolysis: add 0.5 g of wolfberry essence powder to 10-20 g of deionized water, then add 2 mg of alkaline protease and 0.5 mg of alkaline amylase, adjust the pH to 7.9 with 0.1 mol / L sodium hydroxide, heat to 60°C, hydrolyze for 4 h, then heat to 100°C, inactivate the enzyme for 3 min, centrifuge, and freeze-dry the supernatant to obtain wolfberry amino acid powder;

[0042] (6) Tablet pressing: The wolfberry amino acid powder is pressed into tablets by a tablet press to obtain wolfberry amino acid essence tablets.

[0043] Embodiment 3:

[0044] (1) Defatting: Add 10 g of wolfberry powder to 30 g of n-hexane, heat to 60° C., stir for 6 h, centrifuge, air-dry and sieve through an 80-mesh sieve to obtain defatted wolfberry powder;

[0045] (2) Enzymatic hydrolysis: Add 5 g defatted wolfberry powder to 120 g deionized water, then add 20 mg cellulase and 6 mg pectinase, adjust the pH to 6 with 0.1 mol / L hydrochloric acid, seal the cup with plastic wrap, heat to 60 °C, extract for 3 h, then heat to 100 °C, inactivate the enzyme for 5 min, filter, and obtain the enzymatic solution.

[0046] (3) Alcohol precipitation: add 50 g of the enzymatic hydrolysate into 300 g of 95% ethanol solution, cool to 5°C, let stand for 36 h, centrifuge, and vacuum dry to obtain enzymatic hydrolysate powder;

[0047] (4) Pretreatment: 1 g of enzymatic hydrolysis powder was added to 20 g of deionized water, the pH was adjusted to 8 with 0.1 mol / L sodium hydroxide, the temperature was raised to 85°C, the reaction was stirred for 72 h, and the pH was adjusted to 4.9 with 0.1 mol / L hydrochloric acid, centrifuged, and vacuum dried to obtain wolfberry essence powder;

[0048] (5) Hydrolysis: 0.5 g of wolfberry essence powder was added to 20 g of deionized water, and then 4 mg of alkaline protease and 1.5 mg of alkaline amylase were added, and the pH was adjusted to 8.4 with 0.1 mol / L sodium hydroxide, and the temperature was raised to 65°C, and the hydrolysis was carried out for 6 h, and then the temperature was raised to 100°C, and the enzyme was inactivated for 5 min, and the supernatant was taken for centrifugation and freeze-dried to obtain wolfberry amino acid powder;

[0049] (6) Tablet pressing: The wolfberry amino acid powder is pressed into tablets by a tablet press to obtain wolfberry amino acid essence tablets.

[0050] Comparative Example 1:

[0051] The difference between Comparative Example 1 and Example 1 is that: there is no pretreatment;

[0052] The specific steps are as follows:

[0053] (1) Defatting: Add 10 g of wolfberry powder to 25 g of n-hexane, heat to 60° C., stir for 5 h, centrifuge, air-dry and sieve through an 80-mesh sieve to obtain defatted wolfberry powder;

[0054] (2) Enzymatic hydrolysis: Add 5 g defatted wolfberry powder to 100 g deionized water, then add 15 mg cellulase and 4.5 mg pectinase, adjust the pH to 5.6 with 0.1 mol / L hydrochloric acid, seal the cup with plastic wrap, heat to 55 °C, extract for 2.5 h, then heat to 100 °C, inactivate the enzyme for 5 min, filter, and obtain the enzymatic solution.

[0055] (3) Alcohol precipitation: add 50 g of the enzymatic hydrolysate to 250 g of 95% ethanol solution, cool to 4°C, let stand for 32 h, centrifuge, and vacuum dry to obtain enzymatic hydrolysate powder;

[0056] (4) Hydrolysis: add 0.5 g of enzymatic hydrolysis powder to 15 g of deionized water, then add 3 mg of alkaline protease and 1 mg of alkaline amylase, adjust the pH to 8.2 with 0.1 mol / L sodium hydroxide, heat to 65°C, hydrolyze for 5 h, then heat to 100°C, inactivate the enzyme for 5 min, centrifuge, and freeze-dry the supernatant to obtain wolfberry amino acid powder;

[0057] (5) Tablet pressing: The wolfberry amino acid powder is pressed into tablets by a tablet press to obtain wolfberry amino acid essence tablets.

[0058] Comparative Example 2:

[0059] The difference between Comparative Example 2 and Example 1 is that alkaline amylase is not added in step (5);

[0060] The specific steps are as follows:

[0061] (1) Defatting: Add 10 g of wolfberry powder to 25 g of n-hexane, heat to 60° C., stir for 5 h, centrifuge, air-dry and sieve through an 80-mesh sieve to obtain defatted wolfberry powder;

[0062] (2) Enzymatic hydrolysis: Add 5 g defatted wolfberry powder to 100 g deionized water, then add 15 mg cellulase and 4.5 mg pectinase, adjust the pH to 5.5 with 0.1 mol / L hydrochloric acid, seal the cup with plastic wrap, heat to 55 °C, extract for 2.5 h, then heat to 100 °C, inactivate the enzyme for 5 min, filter, and obtain the enzymatic solution.

[0063] (3) Alcohol precipitation: add 50 g of the enzymatic hydrolysate to 250 g of 95% ethanol solution, cool to 4°C, let stand for 32 h, centrifuge, and vacuum dry to obtain enzymatic hydrolysate powder;

[0064] (4) Pretreatment: add 1 g of enzymatic hydrolysis powder to 15 g of deionized water, adjust the pH to 7.7 with 0.1 mol / L sodium hydroxide, raise the temperature to 80-85°C, stir and react for 60 h, then adjust the pH to 4.5 with 0.1 mol / L hydrochloric acid, centrifuge and vacuum dry to obtain wolfberry essence powder;

[0065] (5) Hydrolysis: add 0.5 g of wolfberry essence powder to 15 g of deionized water, then add 3 mg of alkaline protease, adjust the pH to 8.1 with 0.1 mol / L sodium hydroxide, raise the temperature to 65°C, hydrolyze for 5 h, then raise the temperature to 100°C, inactivate the enzyme for 5 min, centrifuge, and freeze-dry the supernatant to obtain wolfberry amino acid powder;

[0066] (6) Tablet pressing: The wolfberry amino acid powder is pressed into tablets by a tablet press to obtain wolfberry amino acid essence tablets.

[0067] Comparative Example 3:

[0068] The difference between Comparative Example 3 and Example 1 is that: Step (2) is extracted by hot water extraction;

[0069] The specific steps are as follows:

[0070] (1) Defatting: Add 10 g of wolfberry powder to 25 g of n-hexane, heat to 60° C., stir for 5 h, centrifuge, air-dry and sieve through an 80-mesh sieve to obtain defatted wolfberry powder;

[0071] (2) Hot water extraction: add 5 g wolfberry to 100 g deionized water, heat to 85°C, adjust the pH to 1.5 with 0.1 mol / L hydrochloric acid, extract twice, each time for 1.5 h, filter, combine the two filtrates, adjust the pH to neutral with 0.1 mol / L sodium hydroxide, and concentrate 10 times the volume to obtain an extract;

[0072] (3) Alcohol precipitation: add 50 g of the extract to 250 g of 95% ethanol solution, cool to 4°C, let stand for 32 h, centrifuge, and vacuum dry to obtain enzymatic hydrolyzate powder;

[0073] (4) Pretreatment: add 1 g of enzymatic hydrolysis powder to 15 g of deionized water, adjust the pH to 7.8 with 0.1 mol / L sodium hydroxide, raise the temperature to 80-85°C, stir and react for 60 h, then adjust the pH to 4.4 with 0.1 mol / L hydrochloric acid, centrifuge and vacuum dry to obtain wolfberry essence powder;

[0074] (5) Hydrolysis: 0.5 g of wolfberry essence powder was added to 15 g of deionized water, and then 3 mg of alkaline protease and 1 mg of alkaline amylase were added. The pH was adjusted to 8.2 with 0.1 mol / L sodium hydroxide, and the temperature was raised to 65° C., and the hydrolysis was carried out for 5 h. The temperature was then raised to 100° C., and the enzyme was inactivated for 5 min. The mixture was centrifuged, and the supernatant was freeze-dried to obtain wolfberry amino acid powder.

[0075] (6) Tablet pressing: The wolfberry amino acid powder is pressed into tablets by a tablet press to obtain wolfberry amino acid essence tablets.

[0076] Performance Testing:

[0077] Hydrolysis degree: The hydrolysis degree of the wolfberry amino acid powder prepared in the example and the comparative example was tested by ninhydrin colorimetry. The results are shown in Table 1.

[0078] Antioxidant activity: The wolfberry amino acid powder prepared in the example and the comparative example was added to the ABTS solution to obtain an ABTS solution containing wolfberry amino acids at a concentration of 1 mg / mL. The solution was fully shaken for 15 minutes in the dark, and the absorbance was tested at a wavelength of 734 nm after centrifugation. The ABTS free radical scavenging rate was calculated. The results are shown in Table 1.

[0079] Emulsification: The wolfberry amino acid powder prepared in the examples and comparative examples was dispersed in soybean oil, and the pH value was adjusted to 7.0, 8.0, 9.0 and 10.0 with 0.1 mol / L sodium hydroxide to obtain a wolfberry amino acid solution with a concentration of 1 mg / mL, and then mixed at 10000 r / min for 2 min. The emulsions at 0 min and 10 min were taken out from the bottom (diluted 100 times with 0.1% SDS). Then, the A0 and A1 of the emulsions were measured at a wavelength of 500 nm. 10 , the emulsification activity index (EAI) and emulsion stability index (ESI) were calculated, and the results are shown in Table 1.

[0080] Table 1 Performance test results

[0081]

[0082]

[0083] Data Analysis:

[0084] From the data analysis of Examples 1 to 3, it can be seen that the wolfberry amino acid powder prepared by the present invention exhibits excellent properties in many aspects, including hydrolysis degree, antioxidant activity, emulsification activity and emulsification stability.

[0085] The results of Example 1 show that the pretreated wolfberry amino acid powder has a high degree of hydrolysis and antioxidant properties. The data of Comparative Example 1 further verified the importance of pretreatment. The pretreatment process effectively improved the degree of hydrolysis of the amino acid powder, which may be related to the Maillard reaction of polysaccharides and proteins during the enzymatic hydrolysis process. The Maillard reaction refers to the process in which sugars and amino acids react to form new flavors and nutrients under heating or other conditions. This reaction not only changes the morphology of the protein and increases the exposed surface area, but also may produce compounds that help to improve antioxidant activity. In addition, the improvement in emulsification activity and emulsification stability observed in Example 1 is significant, which is closely related to the change in protein morphology after pretreatment. The larger surface area and improved molecular structure help to enhance the emulsification properties, allowing the wolfberry amino acid powder to be more effectively stable in the aqueous and oil phases.

[0086] By comparing the data of Example 1 with Comparative Example 2, it can be seen that alkaline amylase significantly improves the antioxidant activity of wolfberry amino acid powder. Alkaline amylase treatment can increase the number of reducing ends of the molecular chain, thereby improving its antioxidant capacity. At the same time, alkaline amylase adjusts the molecular chain structure and exposes more hydrophobic surfaces, promoting the formation of a three-dimensional network structure through hydrophobic interactions, thereby further improving the emulsification activity and stability.

[0087] Comparison of the data of Example 1 and Comparative Example 3 shows that the use of cellulase and pectinase to treat defatted wolfberry powder can significantly improve the subsequent preparation of wolfberry amino acids compared to traditional hot water extraction. Cellulase and pectinase promote the release of polysaccharides and proteins by effectively decomposing cell walls and other biomacromolecules. This process greatly improves the extraction efficiency of amino acids and lays the foundation for subsequent applications.

[0088] In summary, the data of the examples show that the functional properties of wolfberry amino acid powder can be significantly improved through appropriate pretreatment and enzymatic hydrolysis technology. These findings provide new technical support for the development and application of wolfberry amino acids, and also provide valuable references for research in related fields.

[0089] Those skilled in the art should understand that the discussion of any of the above embodiments is merely illustrative and is not intended to imply that the scope of the present invention is limited to these examples. Under the concept of the present invention, the technical features in the above embodiments or different embodiments may be combined, the steps may be implemented in any order, and there are many other variations of the different aspects of the present invention as described above, which are not provided in detail for the sake of simplicity.

Claims

1. A method for producing wolfberry amino acid essence tablets, characterized in that: The following steps are involved: (1) defatting: defatting the wolfberry powder with n-hexane to obtain defatted wolfberry powder; (2) Enzymatic hydrolysis: using composite enzyme 1 to enzymatically hydrolyze the defatted wolfberry powder to obtain an enzymatic hydrolyzate; (3) Alcohol precipitation: using ethanol to precipitate the enzymatic hydrolysate to obtain enzymatic hydrolysate powder; (4) Pretreatment: Add the enzymatic hydrolyzed powder to deionized water, adjust the pH to 7.5-8 with sodium hydroxide, raise the temperature to 80-85° C., stir and react for 48-72 hours, then adjust the pH to 4-5 with hydrochloric acid, centrifuge and vacuum dry to obtain wolfberry essence powder; (5) hydrolysis: using compound enzyme 2 to hydrolyze the wolfberry essence powder to obtain wolfberry amino acid powder; (6) tableting: pressing the wolfberry amino acid powder into tablets using a tablet press to obtain wolfberry amino acid essence tablets; In the step (2), the complex enzyme 1 is a mixture of cellulase and pectinase in a weight ratio of 10-20:3-6; In the step (5), the complex enzyme 2 is a mixture of alkaline protease and alkaline amylase in a weight ratio of 2-4:0.5-1.

5.

2. The method for producing the wolfberry amino acid essence tablet according to claim 1, characterized in that: In the step (1), the weight ratio of wolfberry powder to n-hexane is 2:3-6.

3. The method for producing the wolfberry amino acid essence tablet according to claim 1, characterized in that: The degreasing temperature in step (1) is 55-60° C. and the degreasing time is 4-6 hours.

4. The method for producing the wolfberry amino acid essence tablet according to claim 1, characterized in that: The temperature of the enzymatic hydrolysis in step (2) is 50-60° C. and the time is 2-3 hours.

5. The method for producing the wolfberry amino acid essence tablet according to claim 1, characterized in that: The temperature of the alcohol precipitation in step (3) is 2-5°C and the time is 24-36h.

6. The method for producing the wolfberry amino acid essence tablet according to claim 1, characterized in that: In the step (4), the weight ratio of the enzymatic hydrolysis powder to deionized water is 1:10-20.

7. The method for producing the wolfberry amino acid essence tablet according to claim 1, characterized in that: The hydrolysis temperature in step (5) is 60-65° C. and the time is 4-6 hours.

8. A wolfberry amino acid essence tablet, characterized in that: The wolfberry amino acid essence tablets are obtained by the production method of any one of claims 1 to 7.

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