CN115024355A - Preparation method of allicin-based fresh-keeping coating for chilled fresh meat by composite carrier coating - Google Patents

Preparation method of allicin-based fresh-keeping coating for chilled fresh meat by composite carrier coating Download PDF

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CN115024355A
CN115024355A CN202210643884.7A CN202210643884A CN115024355A CN 115024355 A CN115024355 A CN 115024355A CN 202210643884 A CN202210643884 A CN 202210643884A CN 115024355 A CN115024355 A CN 115024355A
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allicin
enzymolysis
fresh
coating
meat
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CN115024355B (en
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仇晓阳
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College of Science and Technology of Ningbo University
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    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23BPRESERVING, e.g. BY CANNING, MEAT, FISH, EGGS, FRUIT, VEGETABLES, EDIBLE SEEDS; CHEMICAL RIPENING OF FRUIT OR VEGETABLES; THE PRESERVED, RIPENED, OR CANNED PRODUCTS
    • A23B4/00General methods for preserving meat, sausages, fish or fish products
    • A23B4/10Coating with a protective layer; Compositions or apparatus therefor
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23BPRESERVING, e.g. BY CANNING, MEAT, FISH, EGGS, FRUIT, VEGETABLES, EDIBLE SEEDS; CHEMICAL RIPENING OF FRUIT OR VEGETABLES; THE PRESERVED, RIPENED, OR CANNED PRODUCTS
    • A23B4/00General methods for preserving meat, sausages, fish or fish products
    • A23B4/14Preserving with chemicals not covered by groups A23B4/02 or A23B4/12
    • A23B4/18Preserving with chemicals not covered by groups A23B4/02 or A23B4/12 in the form of liquids or solids
    • A23B4/20Organic compounds; Microorganisms; Enzymes
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00Food compositions, function of food ingredients or processes for food or foodstuffs
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A40/00Adaptation technologies in agriculture, forestry, livestock or agroalimentary production
    • Y02A40/90Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in food processing or handling, e.g. food conservation

Abstract

The invention discloses a preparation method of a fresh-keeping coating for chilled meat by using a compound carrier coating based on garlicin, which mainly comprises the following components: allicin volatile oil, citric acid, Pluronic F127, gelatin and glycerol, and mainly comprises the following steps: the method comprises the steps of extracting allicin, identifying main components of the allicin, embedding the allicin by using a special structure of Pluronic F127, adjusting the pH value of gelatin, mixing an embedded allicin carrier with the gelatin according to a certain proportion, preparing the allicin-based composite carrier coating for keeping the chilled fresh meat fresh, adopting an organic solvent method in the process of extracting the allicin, obtaining an optimal extraction process through corresponding surfaces, and simultaneously utilizing the advantages of natural products and a carrier embedding method. The preparation method of the allicin-based composite carrier coating for the fresh-keeping coating of the cold fresh meat has better performance in the aspects of extraction cost, utilization rate and the like, and is beneficial to better solving the food safety problem of putrefaction of the cold fresh meat product and the waste problem caused by too short cold fresh meat or holidays.

Description

Preparation method of allicin-based fresh-keeping coating for chilled fresh meat by composite carrier coating
Technical Field
The invention relates to the technical field of natural product composite preservatives, in particular to a method for preparing a fresh-keeping coating for chilled meat by using a composite carrier coating based on garlicin.
Background
The meat food is an important food in daily life of people, and the statistical data of the national statistical bureau shows that the annual average yield of meat in nearly 5 years in China is nearly 8500 ten thousand tons. However, the market of chilled fresh meat is continuously expanded, and problems are also caused, such as microbial contamination in the preservation and processing process of meat products and various uncertain factors in the transportation process, so that the spoilage and deterioration of meat foods are accelerated, the shelf life of the chilled fresh meat is generally short, and a large amount of waste is generated.
Allicin is a natural product with good bacteriostatic effect, and has the advantages of low cost, high extraction rate and the like. Garlicin plays a main role in inhibiting bacteria in garlic, and is taken as a main effective component in garlic medicinal materials in Chinese pharmacopoeia. Rao et al, as early as 1946, have demonstrated that allicin has broad-spectrum antimicrobial activity and bacteriostatic effects on both bacteria and fungi. Studies have also shown that allicin inhibits some pathogenic bacteria and viruses that are resistant to specific antibiotics. Meanwhile, the allicin has better oxidation resistance and has biological effects of resisting tumors, cardiovascular diseases and the like. Pluronic F127 is a slow release carrier, is nontoxic and low in price through FDA certification, has excellent biocompatibility and stability, is an amphiphilic triblock copolymer, consists of hydrophobic chain propylene oxide (PPO) and hydrophilic chain polyethylene oxide (PEO), can be self-assembled into micelles, and forms a three-dimensional network structure. Gelatin is collagen extracted from connective tissues or epidermal tissues of animals, is nontoxic and harmless, has low cost, good biocompatibility and degradability, is frequently applied to carriers and protein film materials, can form a film outside food, has an isolation effect on water, oxygen and external microorganisms, and thus prolongs the shelf life of the chilled fresh meat.
The optimal extraction process of the allicin is explored by simulating a plurality of variables of material ratio, pH values before and after enzymolysis and enzymolysis time through a response surface analysis method; determining the optimal inhibitory range of the allicin through a Minimum Inhibitory Concentration (MIC) experiment; gelatin and Pluronic F127 are used for constructing a citric acid composite carrier coating of the allicin, thereby achieving the purpose of prolonging the shelf life of the cold fresh pork. The invention is helpful to better solve the food safety problem of the putrefaction of the chilled meat products and the waste problem caused by the over-short shelf life of the chilled meat.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method of a fresh-keeping coating for cold fresh meat based on a composite carrier coating of allicin, which solves the problems provided in the background technology.
In order to achieve the purpose, the invention is realized by the following technical scheme: a preparation method of a fresh-keeping coating for cold fresh meat based on a compound carrier coating of garlicin comprises the steps of obtaining a pH value before enzymolysis of 3.8, a pH value after enzymolysis of 70min and a pH value after enzymolysis of 6.5 which have high garlicin extraction rate and a garlic extract concentration of 0.2 (material ratio of 1:4) by a single-factor analysis method, and obtaining an extraction scheme of higher extraction rate of pH value before enzymolysis of 3.99, a garlic extract concentration of 0.17, a pH value after enzymolysis of 6.86 and an enzymolysis time of 57.09min by using a response surface analysis method on the basis. And comparing the product with a standard by high performance liquid chromatography.
Further, Pluronic F127 is weighed and dissolved by distilled water, then an oil phase and a water phase are mixed according to the ratio of 1:4 (garlic extract: Pluronic F127 solution), the pH value of the solution is adjusted to 6.00-6.50 by 8 percent citric acid (w/v), and ultrasonic oscillation is carried out for 15-20min at low temperature, thus forming stable emulsion.
First, citric acid is a common food additive. Ammonia substances are easily generated in the putrefaction process of meat products, so that the environment tends to be alkaline, the allicin activity is weakened, and citric acid has a certain preservative effect while the pH value can be kept stable.
Further, 55-60 parts of gelatin and 22.5-30 parts of glycerol are taken, water is added for dissolution, the mixture is refrigerated at the temperature of 0-4 ℃ and kept stand for 12 hours, then high-pressure steam sterilization is carried out for 10-15 minutes, the temperature is reduced to 30-25 ℃, the pH value of the solution is adjusted to 6.0 by citric acid, and preferably, the emulsion is slowly added into the gelatin solution, so as to prepare 0.6 part of the gelatin composite carrier coating of the allicin.
The invention provides a preparation method of a fresh-keeping coating for chilled meat by using a compound carrier coating based on garlicin, which has the following beneficial effects: by utilizing a mathematical modeling method, the optimal extraction process of the allicin by utilizing an organic solvent extraction method is obtained through calculation, so that the extraction efficiency of the allicin is greatly improved, and the multiple agricultural values of the allicin are promoted; the traditional allicin needs to be relatively stable in an acid environment, and the deterioration of meat products is accompanied by the release of a large amount of ammonia substances, so that the stability of the allicin can be damaged. Meanwhile, the gelatin has higher water content, and can also have certain effect on the fresh-keeping characteristic in the process of isolating the oxidation of the cold fresh meat rot.
Drawings
FIG. 1 is a three-dimensional test response surface applying the interaction of four factors of Box-Behnken;
FIG. 2 is an HPLC analysis of allicin extract with allicin as a standard;
FIG. 3 is the effect of pH on chilled fresh meat under different conditions;
figure 4 is the effect of TBA on chilled fresh meat under different conditions;
FIG. 5 is the effect of TVB-N on chilled meat under different conditions;
FIG. 6 is the effect of the total number of colonies of cold fresh meat under different conditions;
FIG. 7 is a sensory index heat map slice result for chilled meat;
FIG. 8 shows the state of chilled meat after different treatments;
FIG. 9 is a table of fresh pig lean meat measurement records;
FIG. 10 is the peak height of the extract.
Detailed Description
The embodiments of the present invention will be described in further detail with reference to the drawings and examples. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
As shown in fig. 1-10, the present invention provides a technical solution: a method for preparing a fresh-keeping coating for cold fresh meat by using a composite carrier coating based on garlicin comprises the steps of extracting garlic, peeling and cleaning, crushing by using a homogenizer, carrying out centrifugal filtration and reduced pressure concentration under the condition of only considering single variable (pH before enzymolysis, enzymolysis time, pH after enzymolysis and material ratio (95% ethanol)), and carrying out freeze drying treatment to obtain a group of optimized extraction schemes.
According to the 4 factors to be examined, another 3 factors are fixed for each 1 factor, and the enzymolysis temperature is 35 ℃.
a. The material ratio is 1:4(g/mL), the pH value after enzymolysis is 6.00, the enzymolysis time is 70min, the influence of the pH value before enzymolysis on the garlicin yield is considered, and the pH values before enzymolysis are respectively adjusted to be 3.60, 3.80, 4.00, 4.20 and 4.40.
b. The pH value before enzymolysis is 4.00, the pH value after enzymolysis is 6.00, the enzymolysis time is 70min, and the influence of the material ratio on the garlicin yield is examined, wherein the material ratio is 1:1, 1:2, 1:3, 1:4 and 1:5 respectively.
c. pH before enzymolysis is 4.00, material ratio is 1:4(g/mL), enzymolysis time is 70min, influence of pH after enzymolysis on garlicin yield is considered, and pH after enzymolysis is respectively adjusted to be 5.00, 5.50, 6.00, 6.50 and 7.00.
d. The pH value before enzymolysis is 4.00, the material ratio is 1:4(g/mL), the pH value after enzymolysis is 6.00, and the influence of the enzymolysis time on the garlicin yield is examined, wherein the enzymolysis is carried out for 30min, 50min, 70min, 90min and 110min respectively.
Calculating the allicin yield in each extracting solution by the formula (1).
Figure BDA0003685161610000041
Determining optimal process of extracting allicin under the condition of only considering single variable, wherein the factors of highest allicin extraction rate are respectively pH3.8 before enzymolysis, enzymolysis time 70min,
After enzymolysis, the pH value is 6.5, and the concentration of the garlic extract is 0.2 (material ratio is 1: 4). The regression equation model in the Box-Behnken test is obvious, and the mismatch term (Lock of Fit) is not obvious, which shows that the test result has high fitting degree with the mathematical model, so the optimal extraction factors are pH3.99 before enzymolysis, the garlic extract concentration is 0.17, pH6.86 after enzymolysis and the enzymolysis time is 57.09 min.
Pluronic F127 is weighed, dissolved by distilled water, mixed with an oil phase, a water phase and a water phase which are 1:4 (garlic extract: Pluronic F127 solution), and then the pH value of the solution is adjusted to 6.00-6.50 by 8 percent citric acid (w/v) and ultrasonic oscillation is carried out for 15-20min at low temperature, thus forming stable emulsion.
Dissolving 55-60 parts of gelatin and 22.5-30 parts of glycerol in water, refrigerating at 0-4 ℃, standing for 12h, sterilizing with high-pressure steam for 10-15min, cooling to 30-25 ℃, adjusting the pH value of the solution to 6.0 with citric acid, and preferably, slowly adding the emulsion into the gelatin solution to prepare 0.6 part of the gelatin composite carrier coating of allicin.
Fresh pork is cut into small pieces with the mass of 10g, 4-5 drops of the small pieces are uniformly smeared on the surface of pork by using Ste-water (sterile water), All (allicin), F127-All (Pluronic F127 garlic extract solution) and Gel-F127 (Pluronic F127 gelatin coating loaded with garlic extract), and the pork is put into a refrigerator with the temperature of 4 ℃. Every other day, sampling for 0-13 days, and respectively measuring and recording the pH value, the volatile base, the thiobarbituric acid reactant, the total number of colonies and the sensory index of each group of meat samples as shown in figure 9;
in order to verify the main active substance of the extracted product, HPLC detection and comparison of the extracted product with the purchased standard were performed. It can be analyzed that the retention times of the major characteristic peaks of the extract and the standard are substantially identical, as shown in fig. 10.
Although the extracts have a hetero peak and the peak heights are slightly different, the extracts are confirmed to be allicin.
During the experiment, the pH of each group of cold fresh pork increased from 6.29 to between 6.62 and 7.02. The Ste-water treatment group had a higher pH than the other groups. And at the end of cold storage, the pH of Gel-F127 treated group was significantly lower (P <0.05) than the other groups. The initial pH drop occurred in the All-treated group and the F127-All treated group, and five days later, the pH of both groups gradually increased over the Gel-F127 treated group (FIG. 3). It is clear that the treated chilled fresh pork rises more slowly and more stably than the untreated pH.
Oxidation is an important cause of pork deterioration, and the thiobarbituric acid reaction value (TBARS) reflects the lipid oxidation degree of meat products, and the higher the TBARS value is, the higher the oxidation degree of meat products is [27] . Values of All treated group, F127-All treated group and Gel-F127 treated group were always lower than those of the control group at the same period. Wherein Gel-F127 is significant (P)<0.05) lower than the other groups (fig. 4).
Volatile basic nitrogen (TVB-N) is one of the common values for meat quality evaluation, decomposition of proteinWill cause the TVB-N value to rise, and the salt-based nitrogen content is regulated to be less than or equal to 15mg/100g to be qualified in the fresh (frozen) livestock and poultry products of the national standard of Chinese food safety [23] . The initial TVB-N content of the sample is 10.68mg/100 g. During cold storage, TVB-N of each group shows a gradually rising trend. Wherein the All-treated group and the F127-All treated group were effective in inhibiting the formation of TVB-N in the early stage, but their TVB-N rapidly increased to exceed the predetermined content within 7 days by the fifth day, but the Gel-F127 treated group was significantly different from the other groups (P)<0.05), exceeded the standard on day 11 (fig. 5).
The putrefaction of fresh meat is mainly caused by activity of microorganism, and the total number of colony in the quality safety requirement of the prepared meat product should be less than or equal to 6log (CFU × g) -1 ) [28] . The colony count of the control group is higher than that of other treated groups at the same time, which shows that the allicin has better inhibition effect on bacteria on the surface of meat. And colonies in the control group and All treated groups were out of standard at day 11 and reached 6.69log (CFU. multidot.g) respectively -1 ) And 6.52log (CFU g) -1 ). The remaining two groups did not exceed the standard (fig. 6).
The sensory index of fresh meat was analyzed by heat mapping in which the sensory index evaluations of color (C) and state (M) were significantly higher in the Gel-F127 group, followed by the F127-All group, with the state evaluation similar to that of the Ste-water group and overall lower in comparison to that of the Ste-water group, as seen from the comparison of the shade of color of the sensory index heat map of each group of samples (FIG. 7). Of these, the Gel-F127 treatment group differed most significantly. All groups scored less than 5 points within 3 days except the Gel-F127 treated group, which scored less than 5 points on day 7. The Ste-water group chilled fresh meat samples were dark in color and heavily dehydrated; the color of Gel-F127 is slightly deepened compared with 0 day, but the overall state and the water wettability are obviously superior to those of other three groups (figure 8).
In conclusion, the gelatin composite carrier coating containing Pluronic F127 wrapped natural allicin has a positive effect on prolonging the shelf life of cold fresh meat. The allicin is mainly combined with other natural extracts, the currently adopted natural extracts mainly comprise chitosan, tea polyphenol and the like, and compared with the research, the research adopts an experimental scheme of low-price raw materials and low cost; meanwhile, a new idea is provided for the factors that the traditional natural product is difficult to utilize and store and the like by constructing a microsphere structure wrapping the allicin.
The embodiments of the present invention have been presented for purposes of illustration and description, and are not intended to be exhaustive or limited to the invention in the form disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art. The embodiment was chosen and described in order to best explain the principles of the invention and the practical application, and to enable others of ordinary skill in the art to understand the invention for various embodiments with various modifications as are suited to the particular use contemplated.

Claims (6)

1. The preparation method of the fresh-keeping coating for the cold fresh meat based on the allicin composite carrier coating is characterized by extracting the allicin, preparing the extracted allicin into an embedded carrier, and mixing the embedded carrier with gelatin to prepare the fresh-keeping coating for the cold fresh meat based on the allicin composite carrier coating.
2. The method of preparing a fresh-keeping coating for chilled meat with an allicin-based composite washcoat of claim 1, wherein: the allicin is extracted by the following method: garlic is peeled and cleaned, crushed by a homogenizer, subjected to centrifugal filtration and reduced pressure concentration under the condition of only considering single variable, and finally subjected to freeze drying to obtain a group of optimized extraction schemes, and a new experimental sample group is obtained by using a mathematical model on the basis, and then the optimal extraction optimization conditions are obtained by verification experiments and corresponding surface method analysis.
3. The method of preparing a fresh-keeping coating of chilled meat with an allicin-based composite washcoat of claim 1, wherein: the single variable is based on 4 factors to be inspected, another 3 factors are fixed when 1 factor is inspected each time, and the enzymolysis temperature is 35 ℃;
a. the material ratio is 1:4, the pH value after enzymolysis is 6.00, the enzymolysis time is 70min, the influence of the pH value before enzymolysis on the garlicin yield is considered, and the pH values before enzymolysis are respectively adjusted to be 3.60, 3.80, 4.00, 4.20 and 4.40;
b. the pH value before enzymolysis is 4.00, the pH value after enzymolysis is 6.00, the enzymolysis time is 70min, and the influence of the material ratio on the garlicin yield is examined, wherein the material ratio is 1:1, 1:2, 1:3, 1:4 and 1:5 respectively;
c. the pH value before enzymolysis is 4.00, the material ratio is 1:4, the enzymolysis time is 70min, the influence of the pH value after enzymolysis on the garlicin yield is inspected, and the pH values after enzymolysis are respectively regulated to be 5.00, 5.50, 6.00, 6.50 and 7.00;
d. pH before enzymolysis is 4.00, material ratio is 1:4, pH after enzymolysis is 6.00, and influence of enzymolysis time on garlicin yield is examined, wherein enzymolysis is carried out for 30min, 50min, 70min, 90min and 110min respectively;
calculating the allicin yield in each extracting solution by a formula (1);
Figure FDA0003685161600000011
Figure FDA0003685161600000021
4. the method of preparing a fresh-keeping coating of chilled meat with an allicin-based composite washcoat of claim 1, wherein: under the condition that only single variable is considered, the optimal process for extracting the allicin by the corresponding surface method determines that the optimal process for extracting the allicin has the highest allicin extraction rate and comprises the factors of pH3.8 before enzymolysis, 70min after enzymolysis, pH6.5 after enzymolysis and 0.2 of garlic extract concentration, the regression equation model of the Box-Behnken test is obvious and the mismatching item is not obvious, and the test result is high in fitting degree with the mathematical model, so that the optimal extraction factors comprise pH3.99 before enzymolysis, 0.17 of garlic extract concentration, pH6.86 after enzymolysis and 57.09min after enzymolysis.
5. The method of preparing a fresh-keeping coating of chilled meat with an allicin-based composite washcoat of claim 1, wherein: preparing the extracted allicin into an embedding carrier, weighing Pluronic F127, dissolving with distilled water, mixing with an oil phase and a water phase at a ratio of 1:4, adjusting the pH value of the solution to 6.00-6.50 with 8% citric acid, and ultrasonically oscillating at low temperature for 15-20min to form a stable emulsion.
6. The method for preparing the fresh-keeping coating on the chilled fresh meat by using the allicin-based composite carrier coating according to claim 1, wherein 55-60 parts of gelatin and 22.5-30 parts of glycerol are taken and dissolved by adding water, the mixture is refrigerated and kept stand at 0-4 ℃ for 12h, then is sterilized by high-pressure steam for 10-15min, is cooled to 30-25 ℃, is used for adjusting the pH value of the solution to 6.0 by using citric acid, and the emulsion is slowly added into the gelatin solution to prepare 0.6 part of the allicin-based gelatin composite carrier coating.
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