Preparation method of preservative for preventing shrimp heads from blackening
By combining ingredients such as bamboo leaf flavonoid powder, an effective shrimp head preservative was prepared, which solved the problems of substance residue, excessive addition and high cost in the existing fresh preservative, and achieved the effect of preventing shrimp head from becoming black and prolonging the shelf life.
Patent Information
- Application Number
- CN202510245863.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-03-04
- Publication Date
- 2025-05-27
AI Technical Summary
The existing preservatives that turn black on shrimp heads have problems such as redecomposing and causing substance residues, excessive addition, resulting in excessive sulfur dioxide residues, high cost and poor insurance effects.
An effective shrimp head preservative was prepared by using a combination of bamboo leaf flavonoid powder, ε-polylysine powder, prulandosaccharide powder, chitosan powder, protease inhibitor and rosemaryol powder.
This fresh preservative effectively prevents the shrimp's head from becoming black, oxidizing and collapse, maintains moisture in the shrimp body, has excellent cooking effect, and has antioxidant function, extends the shelf life of the shrimp and maintains quality.
Smart Images
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Abstract
Description
Technical Field
[0001] The present invention relates to the field of preparation of preservatives, and particularly to a method for preparing a preservative for preventing the head of shrimp from turning black. Background Art
[0002] During the storage of shrimp, polyphenol oxidase in the head will catalyze the conversion of tyrosine into melanin, resulting in blackening. It is necessary to appropriately use preservatives to inhibit the enzyme activity or block the oxidation reaction. Common preservatives include ascorbic acid (vitamin C), which can prevent oxidation; citric acid can adjust the pH value and inhibit enzyme activity; sodium chloride has antibacterial effects, trehalose is used as a natural humectant to keep the moisture of shrimp bodies; disodium EDTA is a metal ion chelating agent, which may inhibit metal-dependent enzymes. Currently, the commercially available preservatives for preventing the head of shrimp from turning black mainly have the following problems. First, there will be problems of substance residues during the re-decomposition of the preservative, including residues of substances that affect physical health. Second, the problem of excessive addition. In order to extend the shelf life and improve the appearance, some merchants may excessively add preservatives such as sodium metabisulfite, which may lead to excessive sulfur dioxide residues, thus posing a potential threat to human health. Third, the current trend is to research and develop natural and harmless preservatives. Plant extracts or biological agents may become safer preservatives. However, they have the problems of high cost and poor preservation effect. Summary of the Invention
[0003] Based on the existing technology, the technical problem to be solved by the present invention is to provide a method for preparing a preservative for preventing the head of shrimp from turning black to solve the above problems.
[0004] The technical solution of the present invention:
[0005] A preservative for preventing the head of shrimp from turning black, comprising the following raw materials in parts by weight: 10-15 parts of bamboo leaf flavone powder, 4-6 parts of ε-polylysine powder, 3-4 parts of pullulan polysaccharide powder, 1-2 parts of chitosan powder, 0.4-0.6 part of protease inhibitor, and 0.05-0.08 part of rosmarinic acid powder. It includes the following steps:
[0006] S1. Dissolve the chitosan powder in an acetic acid solution and stir magnetically to obtain a chitosan acetic acid solution;
[0007] S2. Mix the bamboo leaf flavone powder, rosmarinic acid powder and protease inhibitor, dissolve them in an ethanol solution, and stir magnetically to obtain an alcohol mixture;
[0008] S3. Mix the ε-polylysine powder and pullulan polysaccharide powder, dissolve them in water, and stir to obtain an aqueous solution;
[0009] S4. Mix the chitosan acetic acid solution, the alcohol mixture and the aqueous solution to obtain the finished product.
[0010] Further, in step S1, the volume fraction of the acetic acid solution is 0.3 - 0.5%, the magnetic stirring time is 1 - 1.2 h, and the temperature is 35 - 40 °C.
[0011] Further, in step S2, the volume concentration of the ethanol solution is 60 - 65%, the magnetic stirring time is 1.5 - 2 h, and the temperature is 20 - 30 °C.
[0012] Further, the protease inhibitor is Kunitz-type trypsin inhibitor or Bowman-Birk type trypsin inhibitor.
[0013] The preparation of bamboo leaf flavonoids includes the following steps: collecting bamboo leaves, drying, and pulverizing to obtain bamboo leaf powder; degreasing the bamboo leaf powder to remove the waxy layer, impregnating with n-hexane, and performing ultrasonic stirring to obtain a bamboo leaf solution; adding the bamboo leaf solution to a mixed enzyme for enzymatic hydrolysis to obtain an enzymatic hydrolysate; purifying, concentrating, and drying the enzymatic hydrolysate to obtain bamboo leaf flavonoid powder.
[0014] Further, the drying is light-avoiding lyophilization with moisture ≤ 5%; the pulverizing is passing through a 60-mesh sieve.
[0015] Further, the mass-volume ratio of the bamboo leaf powder to n-hexane is 1:12 - 15, the ultrasonic stirring frequency is 30 - 40 kHz, and the time is 20 - 30 min.
[0016] Further, the mixed enzyme is cellulase and N-acetylmuramyl glycan hydrolase, the mass ratio of cellulase to N-acetylmuramyl glycan hydrolase is 4 - 6:1, the addition amount of the mixed enzyme is 1.2 - 1.4% of the mass of the bamboo leaf solution, the enzymatic hydrolysis conditions are 40 - 50 °C, the pH value is 5.5 - 7.5, and the enzymatic hydrolysis time is 4 - 5 h.
[0017] Compared with the prior art, the beneficial effects of the present invention are as follows:
[0018] (1) The shrimp head preservative prepared by the present invention can effectively prevent the phenomena of blackening, oxidation, collapse, and internal material loss of the shrimp head, and has a better cooking effect.
[0019] (2) The shrimp head preservative prepared by the present invention can have an antioxidant function, effectively prevent the shrimp head from blackening and oxidizing, and the product quality can be maintained at a good level. Specific Embodiments
[0020] To better understand the technical content of the present invention and describe the technical solution clearly and completely, specific embodiments are provided below to further illustrate the present invention. The following are only some embodiments of the present invention.
[0021] The materials, reagents, etc. used in the embodiments of the present invention can be obtained from commercial channels without special instructions.
[0022] In this example, the raw material components used are as follows: The cellulase is purchased from Sichuan Huatang Juri Biotechnology Co., Ltd., food grade, with an enzyme activity of 100,000 and an active substance content of 99%; and the N-acetylmuramyl glycan hydrolase is purchased from Wuhan Huaxiang Kejie Biotechnology Co., Ltd., food grade, with an active ingredient content of 99%.
[0023] Preparation Example 1
[0024] Steps for preparing bamboo leaf flavonoids: (1) Collect Phyllostachys heterocycla var. pubescens leaves with a growth age of 3 - 4 years, whose flavonoid content > 8%, wash them clean, air-dry, freeze-dry them in the dark to make the moisture ≤ 5%, and pulverize them through a 60-mesh sieve to obtain Phyllostachys heterocycla var. pubescens leaf powder; (2) Degrease the Phyllostachys heterocycla var. pubescens leaf powder to remove the wax layer, impregnate it with n-hexane, the mass-volume ratio of Phyllostachys heterocycla var. pubescens leaf powder to n-hexane is 1:12, stir it with ultrasonic at 30 kHz for 20 min to obtain a Phyllostachys heterocycla var. pubescens leaf solution; (3) Add the Phyllostachys heterocycla var. pubescens leaf solution to a mixed enzyme for enzymatic hydrolysis. The mixed enzyme is a cellulase and an N-acetylmuramyl glycan hydrolase with a mass ratio of 4:1, the addition amount of the mixed enzyme is 1.2% of the mass of the Phyllostachys heterocycla var. pubescens leaf solution, the enzymatic hydrolysis conditions are 40°C, pH value of 5.5, and the enzymatic hydrolysis time is 4 h. After enzymatic hydrolysis, an enzymatic hydrolysate is obtained; Purify, concentrate, and dry the enzymatic hydrolysate to obtain bamboo leaf flavonoid powder.
[0025] Preparation Example 2
[0026] Steps for preparing bamboo leaf flavonoids: (1) Collect Phyllostachys heterocycla var. pubescens leaves with a growth age of 3 - 4 years, whose flavonoid content > 8%, wash them clean, air-dry, freeze-dry them in the dark to make the moisture ≤ 5%, and pulverize them through a 60-mesh sieve to obtain Phyllostachys heterocycla var. pubescens leaf powder; (2) Degrease the Phyllostachys heterocycla var. pubescens leaf powder to remove the wax layer, impregnate it with n-hexane, the mass-volume ratio of Phyllostachys heterocycla var. pubescens leaf powder to n-hexane is 1:15, stir it with ultrasonic at 40 kHz for 30 min to obtain a Phyllostachys heterocycla var. pubescens leaf solution; (3) Add the Phyllostachys heterocycla var. pubescens leaf solution to a mixed enzyme for enzymatic hydrolysis. The mixed enzyme is a cellulase and an N-acetylmuramyl glycan hydrolase with a mass ratio of 6:1, the addition amount of the mixed enzyme is 1.4% of the mass of the Phyllostachys heterocycla var. pubescens leaf solution, the enzymatic hydrolysis conditions are 50°C, pH value of 7.5, and the enzymatic hydrolysis time is 5 h. After enzymatic hydrolysis, an enzymatic hydrolysate is obtained; Purify, concentrate, and dry the enzymatic hydrolysate to obtain bamboo leaf flavonoid powder.
[0027] Preparation Example 3
[0028] Preparation steps of bamboo leaf flavonoids: (1) Collect bamboo leaves of Phyllostachys pubescens with a growth age of 3 - 4 years, whose flavonoid content > 8%, wash them clean, air-dry, quickly freeze-dry in the dark to make the water content ≤ 5%, and pulverize through a 60-mesh sieve to obtain bamboo leaf powder; (2) Degrease and remove the wax layer from the bamboo leaf powder, impregnate with n-hexane, the mass-volume ratio of the bamboo leaf powder to n-hexane is 1:15, stir with ultrasonic at 40 kHz for 25 min to obtain a bamboo leaf solution; (3) Add the bamboo leaf solution to a mixed enzyme for enzymatic hydrolysis. The mixed enzyme is a cellulase and an N-acetylmuramidase with a mass ratio of 5:1, the addition amount of the mixed enzyme is 1.3% of the mass of the bamboo leaf solution, the enzymatic hydrolysis conditions are 45 °C, pH value is 7, and the enzymatic hydrolysis time is 4.5 h. After enzymatic hydrolysis, obtain an enzymatic hydrolysate; Purify, concentrate, and dry the enzymatic hydrolysate to obtain bamboo leaf flavonoid powder.
[0029] Example 1
[0030] A preservative for preventing the head of shrimp from turning black, comprising the following raw materials in parts by weight: 10 parts of bamboo leaf flavonoid powder prepared by the method of Preparation Example 1, 4 parts of ε-polylysine powder, 3 parts of pullulan polysaccharide powder, 1 part of chitosan powder, 0.4 part of Kunitz-type trypsin inhibitor, and 0.05 part of rosmarinic acid powder. It includes the following preparation steps:
[0031] Step (1): Dissolve chitosan powder in an acetic acid solution with a volume fraction of 0.3%, stir magnetically for 1 h at a temperature of 35 °C to obtain a chitosan acetic acid solution;
[0032] Step (2): Mix bamboo leaf flavonoid powder, rosmarinic acid powder and protease inhibitor, dissolve in an ethanol solution with a volume concentration of 60%, stir magnetically for 1.5 h at a temperature of 20 °C to obtain an alcohol mixture;
[0033] Step (3): Mix ε-polylysine powder and pullulan polysaccharide powder, dissolve in water, and stir to obtain an aqueous solution;
[0034] Step (4): Mix the chitosan acetic acid solution, the alcohol mixture and the aqueous solution to obtain the finished product.
[0035] Example 2
[0036] A preservative for preventing the head of shrimp from turning black, comprising the following raw materials in parts by weight: 15 parts of bamboo leaf flavonoid powder prepared by the method of Preparation Example 2, 6 parts of ε-polylysine powder, 4 parts of pullulan polysaccharide powder, 2 parts of chitosan powder, 0.6 part of Bowman-Birk type trypsin inhibitor, and 0.08 part of rosmarinic acid powder. It includes the following preparation steps:
[0037] Step (1): Dissolve chitosan powder in an acetic acid solution with a volume fraction of 0.5%, stir magnetically for 1.2 h at a temperature of 40 °C to obtain a chitosan acetic acid solution;
[0038] Step (ii): Mix the bamboo leaf flavonoid powder, rosmarinol powder and protease inhibitor, dissolve them in an ethanol solution with a volume concentration of 65%, stir magnetically for 2 h at a temperature of 30 °C to obtain an alcohol mixture.
[0039] Step (iii): Mix the ε-polylysine powder and pullulan polysaccharide powder, dissolve them in water and stir to obtain an aqueous solution.
[0040] Step (iv): Mix the chitosan acetate solution, the alcohol mixture and the aqueous solution to obtain the finished product.
[0041] Example 3
[0042] A preservative for preventing the head of shrimp from turning black, comprising the following raw materials in parts by weight: 12 parts of bamboo leaf flavonoid powder prepared by the method of Preparation Example 3, 5 parts of ε-polylysine powder, 3 parts of pullulan polysaccharide powder, 2 parts of chitosan powder, 0.5 part of Bowman-Birk type trypsin inhibitor, and 0.06 part of rosmarinol powder. The preparation steps are as follows:
[0043] Step (i): Dissolve the chitosan powder in an acetic acid solution with a volume fraction of 0.4%, stir magnetically for 1 h at a temperature of 35 °C to obtain a chitosan acetate solution.
[0044] Step (ii): Mix the bamboo leaf flavonoid powder, rosmarinol powder and protease inhibitor, dissolve them in an ethanol solution with a volume concentration of 65%, stir magnetically for 1.5 h at a temperature of 25 °C to obtain an alcohol mixture.
[0045] Step (iii): Mix the ε-polylysine powder and pullulan polysaccharide powder, dissolve them in water and stir to obtain an aqueous solution.
[0046] Step (iv): Mix the chitosan acetate solution, the alcohol mixture and the aqueous solution to obtain the finished product.
[0047] Comparative Example 1
[0048] The difference between Comparative Example 1 and Example 3 is that the ε-polylysine powder is removed from the raw materials, and the other raw materials and preparation methods are the same as those in Example 3.
[0049] Comparative Example 2
[0050] The difference between Comparative Example 2 and Example 3 is that the pullulan polysaccharide powder is removed from the raw materials, and the other raw materials and preparation methods are the same as those in Example 3.
[0051] Comparative Example 3
[0052] The difference between Comparative Example 3 and Example 3 is that the chitosan powder and rosmarinol powder are removed from the raw materials, and the other raw materials and preparation methods are the same as those in Example 3.
[0053] Comparative Example 4
[0054] The difference between Comparative Example 4 and Example 3 is that Bowman-Birk type trypsin inhibitor and rosmarinic acid powder are removed from the raw materials, and the other raw materials and preparation methods are the same as those of Example 3.
[0055] Comparative Example 5
[0056] The difference between Comparative Example 4 and Example 3 is that in the step of preparing bamboo leaf flavonoid powder by the method of Preparation Example 3 in the raw materials, the steps of removing the waxy layer and enzymatic hydrolysis are removed, and the other methods are the same as those of Preparation Example 3, and the raw materials and methods are the same as those of Example 3.
[0057] Commercially available control
[0058] The commercially available preservative is produced by Xiamen Mindeyou Food Technology Co., Ltd., and its main components are trehalose, sodium citrate, sodium carbonate and starch.
[0059] Blank control
[0060] An equal amount of pure water is used as the blank control.
[0061] Sensory evaluation test:
[0062] Soak the fresh shrimp heads with the preservatives of Examples 1-3, Comparative Examples 1-5, commercially available control and blank control. Dilute the preservatives of Examples 1-3 and Comparative Examples 1-5, and soak them after diluting 15 times. The commercially available control is soaked according to its instruction method. The soaking time is 15 min, the room temperature is 18-20 °C, and 10 sample shrimps (of the same size) are randomly selected for each treatment. At 24 h after soaking and 6 months after freezing respectively, a sensory evaluation group (10 people) comprehensively scores the sensory quality of the shrimp meat according to Table 1, and finally takes the average value.
[0063] Table 1 Sensory evaluation form
[0064]
[0065] Table 2 Scoring form
[0066]
[0067]
[0068] The results show that the preservatives prepared by the methods of Examples 1-3 have good preservation effects on fresh shrimps. In the comparative examples and the control, there are phenomena such as blackening of the shrimp heads, collapse of the shrimp heads and loss of internal substances in appearance, and both the smell and the soup-making effect are worse than those of Examples 1-3. It shows that the preservative prepared by the present invention can have an antioxidant function, effectively prevent the shrimp heads from turning black and oxidizing, and the product quality can be maintained at a good level.
[0069] Determination of disulfide bond content
[0070] Refer to the determination of the disulfide bond content in foods in the National Food Safety Standard - Standard for the Use of Food Additives (GB 2760-2014), and the pretreatment refers to the sensory evaluation test.
[0071] The calculation formula for the disulfide bond content is: Disulfide bond content = A×D / (C×B)
[0072] Wherein, A represents the absorbance value of the sample - the absorbance value of the blank, B represents the protein concentration of the test solution (mg / mL), C represents the molar absorptivity (the value is 13600 mol -1 ·cm -1 ·L), and D is the dilution factor.
[0073] Determination of carbonyl group content
[0074] Refer to the National Food Safety Standard (GB 5009.5-2016).
[0075] The calculation formula for the carbonyl group content is: Carbonyl group content (nmoL / mg protein) = (OD370nm - blank) / (22000×concentration (mg / mL))×125×105.
[0076] Table 3 Index test table
[0077] Group <![CDATA[Disulfide bond content (mol / 10 5 g)]]> Carbonyl content (nmoL / mg protein) Example 1 3.4 1.4 Example 2 3.1 1.3 Example 3 3.3 1.2 Comparative Example 1 4.8 2.3 Comparative Example 2 5.0 2.7 Comparative Example 3 5.1 2.6 Comparative Example 4 4.7 3.1 Comparative Example 5 4.6 2.5 Commercially available control 5.2 3.9 Blank control 9.3 7.1
[0078] The test results show that the mean value of the sensory evaluation of the preservatives prepared in Examples 1-3 of the present invention is 8 points, which is higher than that of Comparative Examples 1-5 and the control. The disulfide bond content is less than 3.5 moL / 10 5 g, and the carbonyl group content is less than 1.5 nmoL / mg protein, which is superior to Comparative Examples 1-5 and the control. It can be seen that the shrimp head preservative developed by the present invention can significantly extend the storage period of shrimp and has a significant effect in terms of antioxidant. Changing the raw materials or the preparation method in the comparative examples cannot achieve the application effect of this method.
[0079] The above are only the exemplary embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principle of the present invention shall be included within the protection scope of the present invention.
Claims
1. A preservative for preventing shrimp heads from turning black, characterized in that: The invention comprises the following raw materials in parts by weight: 10-15 parts of bamboo leaf flavonoid powder, 4-6 parts of epsilon-polylysine powder, 3-4 parts of pullulan powder, 1-2 parts of chitosan powder, 0.4-0.6 parts of protease inhibitor and 0.05-0.08 parts of rosemary phenol powder.
2. A preservative for preventing shrimp heads from turning black as claimed in claim 1, characterized in that: The method comprises the following preparation steps: S1, dissolving chitosan powder in acetic acid solution, stirring magnetically to obtain chitosan acetic acid solution; S2, mixing bamboo leaf flavonoid powder, rosemary phenol powder and protease inhibitor, dissolving in ethanol solution, and magnetically stirring to obtain an alcohol mixture; S3, mixing ε-polylysine powder and pullulan powder, dissolving in water, stirring to obtain an aqueous solution; S4, mixing the chitosan acetic acid solution, the alcohol mixed solution and the aqueous solution to obtain a finished product.
3. The method for preparing a preservative for preventing shrimp heads from turning black as claimed in claim 2, characterized in that: Step S1, the volume fraction of the acetic acid solution is 0.3-0.5%, the magnetic stirring time is 1-1.2h, and the temperature is 35-40°C.
4. The method for preparing a preservative for preventing shrimp heads from turning black as claimed in claim 2, characterized in that: Step S2, the volume concentration of the ethanol solution is 60-65%, the magnetic stirring time is 1.5-2h, and the temperature is 20-30°C.
5. A preservative for preventing shrimp heads from turning black as claimed in claim 1, characterized in that: The protease inhibitor is a Kunitz-type trypsin inhibitor or a Bowman-Birk-type trypsin inhibitor.
6. A preservative for preventing shrimp heads from turning black as claimed in claim 1, characterized in that: The preparation of bamboo leaf flavonoids comprises the following steps: collecting bamboo leaves, drying, and crushing to obtain bamboo leaf powder; defatting the bamboo leaf powder to remove the wax layer, soaking with n-hexane, and ultrasonically stirring to obtain a bamboo leaf solution; adding a mixed enzyme to the bamboo leaf solution for enzymolysis to obtain an enzymolysis solution; purifying, concentrating, and drying the enzymolysis solution to obtain bamboo leaf flavonoids powder.
7. A preservative for preventing shrimp heads from turning black as claimed in claim 6, characterized in that: The drying is light-proof quick freeze drying, with a moisture content of ≤5%; and the pulverizing is passing through a 60-mesh sieve.
8. A preservative for preventing shrimp heads from turning black as claimed in claim 6, characterized in that: The mass volume ratio of the moso bamboo leaf powder to n-hexane is 1:12-15, and the ultrasonic stirring is 30-40kHz for 20-30min.
9. A preservative for preventing shrimp heads from turning black as claimed in claim 6, characterized in that: The mixed enzyme is cellulase and N-acetyl murein polysaccharide hydrolase in a mass ratio of 4-6:1, the added amount of the mixed enzyme is 1.2-1.4% of the mass of the bamboo leaf solution, the enzymatic hydrolysis conditions are 40-50°C, the pH value is 5.5-7.5, and the enzymatic hydrolysis time is 4-5h.