CN115024355B - Preparation method of garlicin-based composite carrier coating for preserving chilled meat - Google Patents

Preparation method of garlicin-based composite carrier coating for preserving chilled meat Download PDF

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CN115024355B
CN115024355B CN202210643884.7A CN202210643884A CN115024355B CN 115024355 B CN115024355 B CN 115024355B CN 202210643884 A CN202210643884 A CN 202210643884A CN 115024355 B CN115024355 B CN 115024355B
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allicin
chilled meat
gelatin
based composite
composite carrier
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CN115024355A (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 an allicin-based composite carrier coating for preserving chilled meat, which comprises the following main components: allicin volatile oil, citric acid, pluronicF127, gelatin and glycerin, and the main steps are as follows: extracting allicin, identifying main components of the allicin, embedding the allicin by utilizing a special structure of Pluronic F127, adjusting the pH of gelatin, mixing the embedded allicin carrier with the gelatin according to a certain proportion to prepare the chilled meat fresh-keeping allicin-based composite carrier coating, extracting the allicin by adopting an organic solvent method, obtaining the optimal extraction process through the corresponding surface, and simultaneously utilizing the advantages of natural products and a carrier embedding method. The preparation method of the garlicin-based composite carrier coating for preserving chilled 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 spoilage of chilled meat products and the waste problem caused by too short chilled meat or holiday.

Description

Preparation method of garlicin-based composite carrier coating for preserving chilled meat
Technical Field
The invention relates to the technical field of natural product composite antistaling agent, in particular to a preparation method of an allicin-based composite carrier coating for preserving chilled meat.
Background
Meat food is an important food in daily life of people, and the statistics data of the national statistical bureau show that the average annual yield of meat in the last 5 years of China is close to 8500 ten thousand tons. However, the market of chilled meat is expanding, and problems are 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 chilled meat is generally short, and a large amount of waste is generated.
As a natural product with good antibacterial effect, the allicin has the advantages of low cost, high extraction rate and the like. Allicin plays a main bacteriostatic role in garlic, and the allicin is taken as a main effective component in garlic medicinal materials in Chinese pharmacopoeia. As early as 1946, rao et al research has demonstrated that allicin has broad-spectrum antimicrobial activity and antibacterial effect on both bacteria and fungi. Studies have also shown that allicin inhibits a number of pathogenic bacteria and viruses that are resistant to certain antibiotics. Meanwhile, the allicin has better antioxidation capability and has biological effects of resisting tumor, cardiovascular diseases and the like. Pluronic F127 is a slow release carrier, is nontoxic and low in price through FDA authentication, has excellent biocompatibility and stability, is an amphiphilic triblock copolymer, is composed of hydrophobic chain oxypropane (PPO) and hydrophilic chain polyethylene oxide (PEO), and can be self-assembled into micelles to form a three-dimensional network structure. Gelatin is collagen extracted from animal connective tissue or epidermis tissue, has no toxicity, no harm, low cost, good biocompatibility and degradability, is widely applied to carrier and protein film materials, can form a film outside food, and has isolation effect on water, oxygen and external microorganisms, thereby prolonging the shelf life of chilled fresh meat.
According to the invention, through a response surface analysis method, the optimal extraction process of allicin is explored by simulating a plurality of variables of material ratio, pH value before and after enzymolysis and enzymolysis time; determining the optimal bacteriostasis range of allicin through a minimum bacteriostasis concentration (MIC) experiment; the gelatin and Pluronic F127 are used for constructing the citric acid composite carrier coating of the allicin, thereby achieving the purpose of prolonging the shelf life of the chilled fresh pork. The invention is helpful to better solve the food safety problem of the spoilage of the chilled meat products and the waste problem caused by the too 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 an allicin-based composite carrier coating for preserving chilled meat, which solves the problems in the prior art.
In order to achieve the above purpose, the invention is realized by the following technical scheme: the preparation method of the allicin-based composite carrier coating for preserving chilled fresh meat is characterized in that the preparation method is used for obtaining an extraction scheme with higher extraction rate, namely 3.99, 0.17, 6.86 and 57.09min before enzymolysis, wherein the extraction rate of the allicin is higher, the enzymolysis time is 70min, the pH is 6.5 after enzymolysis, and the concentration of the allicin extract is 0.2 (the material ratio is 1:4) by adopting a single factor analysis method, and the extraction scheme with higher extraction rate is obtained by adopting a response surface analysis method. And comparing the product with a standard substance by using high performance liquid chromatography.
Further, the Pluronic F127 is weighed and dissolved by distilled water, then the mixture is mixed with garlic extract of Pluronic F127 solution=1:4, the pH value of the solution is regulated to 6.00-6.50 by 8% citric acid (w/v), and the mixture is subjected to low-temperature ultrasonic vibration for 15-20min to form stable emulsion.
Citric acid is first of all a common food additive. Ammonia substances are easy to generate in the spoilage process of meat products, so that the environment tends to be alkaline, the activity of allicin is weakened, and citric acid has a certain preservative effect while maintaining the pH stable.
Further, 55-60 parts of gelatin and 22.5-30 parts of glycerin are taken, water is added for dissolution, the mixture is refrigerated and kept stand for 12 hours at 0-4 ℃ and then sterilized by high-pressure steam for 10-15 minutes, the temperature is reduced and cooled to 30-25 ℃, the pH value of the solution is regulated to 6.0 by citric acid, preferably, the emulsion is slowly added into the gelatin solution, and 0.6 part of allicin gelatin composite carrier coating is prepared.
The invention provides a preparation method of an allicin-based composite carrier coating for preserving chilled meat, which has the following beneficial effects: the optimal extraction process by utilizing an organic solvent extraction method is obtained through calculation by utilizing a mathematical modeling method, so that the extraction efficiency of the allicin is greatly improved, and the multi-agronomic value of the allicin is promoted; the traditional allicin needs to be stable in an acidic environment, and the meat product is spoiled with the release of a large amount of ammonia substances, so that the stability of the allicin can be destroyed. Meanwhile, the gelatin has higher water content, and can also have a certain effect on the fresh-keeping characteristic in the process of isolating the rotten and oxidized chilled meat.
Drawings
FIG. 1 is a three-dimensional test response surface using Box-Behnken four factor interactions;
FIG. 2 is an HPLC analysis of allicin extract with standard allicin;
FIG. 3 is the effect of pH of chilled meat under different conditions;
FIG. 4 is the effect of TBA on chilled 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 chilled meat under different conditions;
FIG. 7 is a hot picture of the sensory index of chilled meat;
FIG. 8 is a view showing the state of chilled meat after being treated under different conditions;
FIG. 9 is a table of fresh pig lean meat assay recordings;
FIG. 10 is a graph showing peak heights of the extracts.
Detailed Description
Embodiments of the present invention are described in further detail below with reference to the accompanying drawings and examples. The following examples are illustrative of 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: the preparation method of the garlicin-based composite carrier coating for fresh-keeping of chilled meat comprises the following steps of extracting garlic, peeling and cleaning the garlic, crushing the garlic by using a refiner, and under the condition of considering only a single variable, (pH before enzymolysis, enzymolysis time, pH after enzymolysis and material ratio (95% ethanol)), centrifuging and filtering the garlic, concentrating the garlic under reduced pressure, and finally performing freeze-drying treatment to obtain a group of optimized extraction schemes, and establishing a mathematical model by using a corresponding surface method to obtain a more efficient extraction scheme.
According to 4 factors to be examined, 3 other factors are fixed when 1 factor is examined each time, and the enzymolysis temperature is 35 ℃.
a. The material ratio is 1:4 (g/mL), the pH after enzymolysis is 6.00, the enzymolysis time is 70min, the influence of the pH before enzymolysis on the allicin yield is examined, and the pH before enzymolysis is respectively regulated to be 3.60, 3.80, 4.00, 4.20 and 4.40.
b. The pH before enzymolysis is 4.00, the pH after enzymolysis is 6.00, the enzymolysis time is 70min, the influence of the material ratio on the allicin yield is examined, and the material ratio is respectively 1:1, 1:2, 1:3, 1:4 and 1:5.
c. The pH value before enzymolysis is 4.00, the material ratio is 1:4 (g/mL), the enzymolysis time is 70min, the influence of the pH value after enzymolysis on the allicin yield is examined, and the pH values after enzymolysis are respectively adjusted to be 5.00, 5.50, 6.00, 6.50 and 7.00.
d. The pH before enzymolysis is 4.00, the material ratio is 1:4 (g/mL), the pH after enzymolysis is 6.00, and the influence of the enzymolysis time on the allicin yield is examined, wherein the enzymolysis time is 30min, 50min, 70min, 90min and 110min respectively.
And (3) calculating the yield of allicin in each extracting solution through a formula (1).
Figure GDA0004189195940000041
Under the condition of considering only a single variable, the optimal process for extracting the allicin is determined, and each factor when the allicin extraction rate is highest is respectively that pH is 3.8 before enzymolysis, enzymolysis time is 70min,
pH after enzymolysis is 6.5, and the concentration of the garlic extract is 0.2 (material ratio is 1:4). The regression equation model of the Box-Behnken test is obvious, and the mismatch term (Lack of Fit) is not obvious, which shows that the test result has high fitting degree with the mathematical model, so that the optimal extraction factors are pH3.99 before enzymolysis, garlic extract concentration 0.17, pH6.86 after enzymolysis and enzymolysis time 57.09min.
Weighing Pluronic F127, dissolving in distilled water, mixing with Bulbus Allii extract/Pluronic F127 solution=1:4, and regulating pH to 6.00-6.50 with 8% citric acid (w/v), and performing low-temperature ultrasonic vibration for 15-20min to obtain stable emulsion.
Taking 55-60 parts of gelatin and 22.5-30 parts of glycerol, adding water for dissolution, refrigerating and standing for 12 hours at 0-4 ℃, sterilizing by high-pressure steam for 10-15 minutes, cooling to 30-25 ℃, regulating the pH value of the solution to 6.0 by using citric acid, and preferably, slowly adding the emulsion into the gelatin solution to prepare 0.6 part of allicin gelatin composite carrier coating.
Cutting fresh lean pork into small pieces with mass of 10g, respectively 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), uniformly smearing 4-5 drops on pork surface, and refrigerating in a refrigerator at 4deg.C. Sampling every other day of 0-13 days, and measuring and recording the pH value, volatile salt group, thiobarbituric acid reactant, total bacterial count and sensory index of each group of meat samples respectively as shown in figure 9;
to verify the primary active substance of the extracted product, HPLC detection and comparison of the extracted product with purchased standard was performed. From this, it can be analyzed that the retention times of the main characteristic peaks of the extract and the standard are substantially identical, as shown in fig. 10.
Although the extract had a peak with a slight difference, the extract was confirmed to be allicin.
During the experiment, the pH of each group of chilled fresh pork was increased from 6.29 to between 6.62-7.02. The Ste-water treatment group had a higher pH than the other groups. And at the end of refrigeration, the pH of Gel-F127 treated group was significantly lower (P < 0.05) than the other groups. The pH of the All treatment group and the F127-All treatment group decreased at the initial stage, and then the pH of the two groups gradually increased over the Gel-F127 treatment group (FIG. 3) five days later. It is seen that the treated chilled pork rose more slowly and more stably than the untreated pH.
Oxidation is an important cause of deterioration of pork, and the thiobarbituric acid reaction value (TBARS) reflects the degree of lipid oxidation of meat products, with greater TBARS reflecting greater degrees of oxidation of meat products [27] . All treatment, F127-All treatment and Gel-F127 treatment values were consistently lower than the control group for the same period. Wherein Gel-F127 is significant (P<0.05 Lower than the other groups (fig. 4).
The volatile basic nitrogen (TVB-N) is one of the common values for evaluating the quality of meat, the TVB-N value is increased due to the decomposition of protein, and the basic nitrogen content is regulated to be less than or equal to 15mg/100g in Chinese food safety national standard fresh (frozen) livestock and poultry products [23] . The initial content of TVB-N in the sample was 10.68mg/100g. During refrigeration, the TVB-N of each group has a gradually rising trend. Wherein All treatment groups and F127-All treatment groups were effective in inhibiting TVB-N production at the early stage, but to the thFive days begin with a rapid rise in their TVB-N beyond the specified level within 7 days, but the Gel-F127 treated group formed significant differences from the other groups (P<0.05 The standard was exceeded on day 11 (fig. 5).
Spoilage of fresh meat is mainly caused by microbial activity, and the total number of bacterial colonies in the quality safety requirement of the prepared meat products is less than or equal to 6log (CFU×g) -1 ) [28] . The total colony count of the control group is higher than that of other treatment groups in the same period, which shows that the allicin has better inhibition effect on bacteria on the surface of meat. And the colonies of the control group and the All treatment group exceeded the standard at 11 days, reaching 6.69log (CFU. Times.g) respectively -1 ) And 6.52log (CFU. Times.g) -1 ). The remaining two groups did not exceed the standard (fig. 6).
The heat map analysis of fresh meat sensory indexes is that the sensory index evaluation of the color (C) and the state (M) of the Gel-F127 group is obviously higher from the comparison of the color shades of the sensory index heat maps of each group of samples, and then the state evaluation of the F127-All group is similar to that of the Ste-water group, and the overall comparison of the Ste-water group is overall lower (figure 7). Of these, gel-F127 treatment group differed most significantly. The remaining groups scored below 5 points within 3 days except for the Gel-F127 treated group, which was below 5 points on day 7. The Ste-water group chilled fresh meat samples were dark in color and severely dehydrated; gel-F127 color was slightly darker than day 0, but overall, water was significantly better than the other three groups (FIG. 8).
In conclusion, the gelatin composite carrier coating containing Pluronic F127 coated natural allicin has positive effect in prolonging the shelf life of chilled fresh meat. The invention mainly combines allicin and other natural extraction products, and the natural extracts adopted at present mainly comprise chitosan, tea polyphenol and the like, compared with the research of the invention which adopts low-cost raw materials and low-cost experimental schemes; meanwhile, a new thought is provided for factors such as difficult utilization and difficult preservation of traditional natural products by constructing a microsphere structure for wrapping allicin.
The embodiments of the 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 embodiments were 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 (1)

1. The preparation method of the allicin-based composite carrier coating for fresh-keeping of chilled meat is characterized by preparing the extracted allicin into an embedding carrier, weighing Pluronic F127, dissolving with distilled water, mixing with Pluronic F127 solution=1:4, regulating the pH value of the solution to 6.00-6.50 with 8% citric acid, performing low-temperature ultrasonic vibration for 15-20min to form a stable emulsion, taking 55-60 parts of gelatin and 22.5-30 parts of glycerol, dissolving with water, refrigerating and standing for 12h at 0-4 ℃, sterilizing with high-pressure steam for 10-15min, cooling for 30-25 ℃, regulating the pH value of the solution to 6.0 with citric acid, and slowly adding the emulsion into the gelatin solution to prepare the allicin gelatin composite carrier coating.
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