CN114698682A - Slow-release limonene embedded substance, preparation method thereof and application of slow-release limonene embedded substance in fruit and vegetable bacteriostasis and fresh keeping - Google Patents
Slow-release limonene embedded substance, preparation method thereof and application of slow-release limonene embedded substance in fruit and vegetable bacteriostasis and fresh keeping Download PDFInfo
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- CN114698682A CN114698682A CN202210459169.8A CN202210459169A CN114698682A CN 114698682 A CN114698682 A CN 114698682A CN 202210459169 A CN202210459169 A CN 202210459169A CN 114698682 A CN114698682 A CN 114698682A
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- XMGQYMWWDOXHJM-UHFFFAOYSA-N limonene Chemical compound CC(=C)C1CCC(C)=CC1 XMGQYMWWDOXHJM-UHFFFAOYSA-N 0.000 title claims abstract description 194
- 229940087305 limonene Drugs 0.000 title claims abstract description 106
- 235000001510 limonene Nutrition 0.000 title claims abstract description 97
- 239000000126 substance Substances 0.000 title claims abstract description 47
- 235000012055 fruits and vegetables Nutrition 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000007789 sealing Methods 0.000 claims abstract description 64
- 229920000881 Modified starch Polymers 0.000 claims abstract description 51
- 239000004368 Modified starch Substances 0.000 claims abstract description 51
- 235000019426 modified starch Nutrition 0.000 claims abstract description 51
- 229920002472 Starch Polymers 0.000 claims abstract description 47
- 235000019698 starch Nutrition 0.000 claims abstract description 45
- 239000008107 starch Substances 0.000 claims abstract description 45
- 238000009931 pascalization Methods 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000003756 stirring Methods 0.000 claims abstract description 18
- 239000000203 mixture Substances 0.000 claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000011049 filling Methods 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 10
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- 238000003825 pressing Methods 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 28
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- 235000013336 milk Nutrition 0.000 claims description 16
- 239000008267 milk Substances 0.000 claims description 16
- 210000004080 milk Anatomy 0.000 claims description 16
- 229920002261 Corn starch Polymers 0.000 claims description 14
- 239000008120 corn starch Substances 0.000 claims description 14
- 238000004321 preservation Methods 0.000 claims description 14
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- 238000010438 heat treatment Methods 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 238000009835 boiling Methods 0.000 claims description 9
- XMGQYMWWDOXHJM-JTQLQIEISA-N (+)-α-limonene Chemical group CC(=C)[C@@H]1CCC(C)=CC1 XMGQYMWWDOXHJM-JTQLQIEISA-N 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 3
- 229920001685 Amylomaize Polymers 0.000 claims description 2
- 229940099112 cornstarch Drugs 0.000 claims description 2
- 229940100486 rice starch Drugs 0.000 claims description 2
- 238000009461 vacuum packaging Methods 0.000 claims description 2
- 229940100445 wheat starch Drugs 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 9
- 238000003860 storage Methods 0.000 abstract description 6
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- 235000013399 edible fruits Nutrition 0.000 abstract 2
- 235000013311 vegetables Nutrition 0.000 abstract 2
- 241000220223 Fragaria Species 0.000 description 39
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- 230000000052 comparative effect Effects 0.000 description 19
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- 235000011363 Fragaria x ananassa Nutrition 0.000 description 13
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- 238000007873 sieving Methods 0.000 description 7
- 238000001179 sorption measurement Methods 0.000 description 7
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- 230000003385 bacteriostatic effect Effects 0.000 description 5
- 235000013305 food Nutrition 0.000 description 5
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 230000003578 releasing effect Effects 0.000 description 3
- 235000005979 Citrus limon Nutrition 0.000 description 2
- 244000131522 Citrus pyriformis Species 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000013270 controlled release Methods 0.000 description 2
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- NOOLISFMXDJSKH-UTLUCORTSA-N (+)-Neomenthol Chemical compound CC(C)[C@@H]1CC[C@@H](C)C[C@@H]1O NOOLISFMXDJSKH-UTLUCORTSA-N 0.000 description 1
- 125000000545 (4R)-limonene group Chemical group 0.000 description 1
- KJPRLNWUNMBNBZ-QPJJXVBHSA-N (E)-cinnamaldehyde Chemical compound O=C\C=C\C1=CC=CC=C1 KJPRLNWUNMBNBZ-QPJJXVBHSA-N 0.000 description 1
- 241000228245 Aspergillus niger Species 0.000 description 1
- 244000063299 Bacillus subtilis Species 0.000 description 1
- 235000014469 Bacillus subtilis Nutrition 0.000 description 1
- NOOLISFMXDJSKH-UHFFFAOYSA-N DL-menthol Natural products CC(C)C1CCC(C)CC1O NOOLISFMXDJSKH-UHFFFAOYSA-N 0.000 description 1
- 241000588724 Escherichia coli Species 0.000 description 1
- 241000191967 Staphylococcus aureus Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
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- 238000010170 biological method Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229940117916 cinnamic aldehyde Drugs 0.000 description 1
- KJPRLNWUNMBNBZ-UHFFFAOYSA-N cinnamic aldehyde Natural products O=CC=CC1=CC=CC=C1 KJPRLNWUNMBNBZ-UHFFFAOYSA-N 0.000 description 1
- 239000001926 citrus aurantium l. subsp. bergamia wright et arn. oil Substances 0.000 description 1
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- 235000019441 ethanol Nutrition 0.000 description 1
- DZGCGKFAPXFTNM-UHFFFAOYSA-N ethanol;hydron;chloride Chemical compound Cl.CCO DZGCGKFAPXFTNM-UHFFFAOYSA-N 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
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- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000010335 hydrothermal treatment Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 1
- 239000010501 lemon oil Substances 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229940041616 menthol Drugs 0.000 description 1
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 235000008935 nutritious Nutrition 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
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- 230000003068 static effect Effects 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
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- 239000002699 waste material Substances 0.000 description 1
Images
Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23B—PRESERVING, e.g. BY CANNING, MEAT, FISH, EGGS, FRUIT, VEGETABLES, EDIBLE SEEDS; CHEMICAL RIPENING OF FRUIT OR VEGETABLES; THE PRESERVED, RIPENED, OR CANNED PRODUCTS
- A23B7/00—Preservation or chemical ripening of fruit or vegetables
- A23B7/14—Preserving or ripening with chemicals not covered by groups A23B7/08 or A23B7/10
- A23B7/144—Preserving or ripening with chemicals not covered by groups A23B7/08 or A23B7/10 in the form of gases, e.g. fumigation; Compositions or apparatus therefor
- A23B7/152—Preserving or ripening with chemicals not covered by groups A23B7/08 or A23B7/10 in the form of gases, e.g. fumigation; Compositions or apparatus therefor in a controlled atmosphere comprising other gases in addition to CO2, N2, O2 or H2O ; Elimination of such other gases
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23P—SHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
- A23P10/00—Shaping or working of foodstuffs characterised by the products
- A23P10/30—Encapsulation of particles, e.g. foodstuff additives
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
-
- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W90/00—Enabling technologies or technologies with a potential or indirect contribution to greenhouse gas [GHG] emissions mitigation
- Y02W90/10—Bio-packaging, e.g. packing containers made from renewable resources or bio-plastics
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Wood Science & Technology (AREA)
- Zoology (AREA)
- Preparation Of Fruits And Vegetables (AREA)
- Storage Of Fruits Or Vegetables (AREA)
Abstract
The invention discloses a slow-release limonene embedded substance, a preparation method thereof and application thereof in fruit and vegetable bacteriostasis and fresh-keeping, comprising the following steps: (1) gelatinizing starch, dropwise adding 2-4 times of anhydrous ethanol into the starch paste at the temperature of 80-90 ℃, and keeping stirring; centrifuging, taking out precipitate, drying and crushing to obtain modified starch; (2) mixing limonene with modified starch according to the mass ratio of more than or equal to 0.1, placing the mixture in a vacuum sealing bag, and placing the vacuum sealing bag under a vacuum condition for 12-24 hours; (3) and (3) placing the vacuum sealing bag in a treatment kettle of high hydrostatic pressure equipment, filling water in the treatment kettle, sealing the treatment kettle, applying pressure of 50-300 MPa, and maintaining the pressure for 10-30 min to obtain the slow-release limonene embedded substance. The invention can effectively improve the slow release performance of the limonene, the embedding material is used for bacteriostasis and fresh keeping of the fruits and the vegetables, and the storage time of the fruits and the vegetables at normal temperature can be obviously prolonged.
Description
Technical Field
The invention belongs to the field of fruit and vegetable preservation, and particularly relates to a preparation method of a slow-release limonene embedded substance and application of the slow-release limonene embedded substance in strawberry bacteriostasis and preservation.
Background
The fruits and vegetables are natural nutritious food, contain various nutrient substances required by people, and are easy to rot in the storage, transportation and sale processes due to strong seasonality and regionality and high water content in the production of the fruits and vegetables. At present, the technical means for fruit and vegetable fresh-keeping can be mainly divided into three categories: physical, chemical and biological methods. In the physical method, the high hydrostatic pressure fresh-keeping technology is to process under static high pressure (100 + 1000MPa) and certain temperature to cause the non-covalent bond destruction or formation of food components, denature and inactivate biological high molecular substances in food, and kill microorganisms in food to achieve the purpose of fresh-keeping, and has the advantages of uniform action, short treatment time, low energy consumption and less pollution.
In the chemical method, because of the problem of safe residue of chemical preservatives, the high requirements of consumers on food safety cannot be met, and the natural extract serving as the preservative is gradually a research hotspot in the field of fruit and vegetable preservation. Limonene is called limonene and has the fragrance of lemon, and can be used as a raw material for preparing artificial orange flower, sweet flower, lemon and bergamot oil, and the source of limonene is mainly waste orange peel. Limonene has been proved to have a good bacteriostatic action, can effectively inhibit escherichia coli, staphylococcus aureus, bacillus subtilis, aspergillus niger and the like, the dosage of limonene is not limited by the international daily-use flavor and fragrance association, and limonene cannot accumulate in a human body to generate toxic and side effects, so that limonene has been widely used for fresh keeping of fruits and vegetables in recent years. However, in the practical application process of limonene, the use of limonene is often limited due to the high volatility of limonene at normal temperature, so that an embedding means is necessary to improve the slow release effect of limonene, and therefore limonene is better applied to the field of fruit and vegetable preservation.
The linear component of starch mainly comprises linear fragments of amylose and branched chain, and can form non-covalent inclusion compounds with various small molecules in food, such as iodine, alcohol, fatty acid and ester thereof, emulsifier, aromatic compounds and the like. In forming the molecular complex, amylose exists as a left-handed single helix, with hydroxyl groups on the outer surface and methylene and glycosidic linkages on the inner surface, thus forming a hydrophilic outer surface and a hydrophobic helical cavity capable of accommodating guest molecules, the helices tending to pack together to form a V-shaped crystal structure. Researches have proved that the aroma substances such as menthol and cinnamaldehyde are embedded by the modified starch with V-type crystals to realize the slow release effect, but the encapsulation method mostly adopts a mode of firstly pasting and then carrying out hydrothermal treatment, has the defects of time consumption and low recovery ratio, and causes slow formation speed of the embedded substances and loss of soluble polymers in the filtering process. In addition, the final product requires a drying process, which results in loss of retained ligand. Besides encapsulation in a liquid phase system, the method also has a solid encapsulation method, has simple and convenient operation process, can avoid the defects, and has the limitations of low encapsulation efficiency and insufficient slow-release effect. Therefore, the modified starch solid encapsulation technology needs to be improved, so that the preparation method of the embedding substance with the slow release performance, which is simpler and more convenient to operate, lower in cost and better in effect, is realized.
Disclosure of Invention
The invention aims to provide a limonene solid encapsulation method with slow release performance, which is characterized in that limonene is embedded by modified starch, high hydrostatic pressure treatment is applied, limonene can be pushed to contact with the surface of the modified starch or binding sites of pores on the premise of not damaging the limonene, the adsorption of the modified starch on the limonene is improved, the effect of slowly releasing the limonene at normal temperature is achieved, and then the bacteriostasis and fresh keeping of fruits and vegetables are realized.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
a preparation method of a slow-release limonene inclusion comprises the following steps:
(1) preparing modified starch; gelatinizing starch, dropwise adding 2-4 times of anhydrous ethanol into the starch paste at the temperature of 80-90 ℃, and keeping stirring; centrifuging, taking the precipitate, drying and crushing to obtain modified starch;
(2) modified starch mixed limonene: mixing limonene with modified starch according to the mass ratio of more than or equal to 0.1, placing the mixture in a vacuum sealing bag, and placing the vacuum sealing bag for 12-24 hours under a vacuum condition;
(3) high hydrostatic pressure treatment: and (3) placing the vacuum sealing bag in a treatment kettle of high hydrostatic pressure equipment, filling water in the treatment kettle, sealing the treatment kettle, applying pressure of 50-300 MPa, maintaining the pressure for 10-30 min, and taking out the modified starch-limonene mixture of the vacuum sealing bag to obtain the slow-release limonene embedded substance.
Preferably, the method for gelatinizing the starch in the step (1) comprises any one of the following steps:
1) preparing starch into starch milk, heating in a boiling water bath or an oil bath, and stirring for more than 1h for gelatinization;
2) a DMSO method, preparing starch into starch milk by using DMSO solution with the concentration of more than 70%, heating in a boiling water bath, and stirring for more than 1h for gelatinization;
3) and (3) an alkaline method, namely dropwise adding an alkaline solution into the starch milk, and stirring for more than 1 hour to gelatinize.
Preferably, the mass fraction of the starch milk is 10-15%.
Preferably, the alkali solution is a KCl, KOH, NaOH solution.
Preferably, the starch of step (1) is high amylose starch, with an amylose content of greater than 50%; the starch is corn starch, rice starch and wheat starch.
Preferably, the water content of the modified starch in the step (1) is 14-16%.
Preferably, the vacuum sealing bag in the step (2) is a PAPE vacuum packaging bag, and the vacuum condition is-0.06-0.1 MPa.
Preferably, the mass ratio of the modified starch to the limonene is 1: 1-4; the limonene is d-limonene (d-limonene).
Preferably, the applied pressure during the high hydrostatic pressure treatment in the step (3) is 100-200 MPa; the adding amount of the sample is 10-30% of the volume of the treatment kettle.
The slow-release limonene embedded substance prepared by the method is applied to bacteriostasis and fresh keeping of fruits and vegetables, the embedded substance and the fruits and vegetables are placed in a sealed box, and the mass ratio of the embedded substance to the fruits and vegetables is more than or equal to 2: 300; preferably, the mass ratio of the embedding material to the fruits and vegetables is 2-10: 300.
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention can obviously improve the adsorption rate of limonene, the prepared modified starch is adopted to adsorb limonene and high hydrostatic pressure treatment is applied, the adsorption rate can reach 61.1-68.8% at most, and the encapsulation rate can reach 60.8-85.9%.
(2) The embedding substance prepared by the invention has slow release performance on limonene, a sample prepared by high hydrostatic pressure treatment has better slow release effect on limonene, and compared with non-embedded limonene (volatilization is finished after 1 day), the slow release effect can be prolonged to more than 4 days.
(3) Compared with the traditional methods such as spray drying and the like, the method disclosed by the invention is carried out at normal temperature, so that the loss of limonene under a high-temperature condition is avoided, and the process energy consumption is low; the invention is a solid encapsulation method, compared with the traditional embedding method carried out in a liquid phase system, the invention has the advantages of simple and convenient operation steps, lower cost and good embedding effect.
(4) The starch in the invention has wide source and low cost, and the preparation method of the modified starch is various and simple, thus being suitable for industrial production.
(5) The characteristic of the slow-release limonene of the embedding object prepared by the invention can be used for fresh-keeping of fruits and vegetables, and the embedding object can achieve the effect of prolonging the shelf life of the fruits and vegetables without directly contacting with the fruit and vegetable products.
Drawings
FIG. 1 is a graph showing the release of the entrapments prepared in example 2 and comparative example 2 at 25 ℃ and 37% relative humidity.
Detailed Description
The examples and comparative examples were based on high amylose corn starch and waxy corn starch, but should not be construed as limiting the scope of the invention.
Example 1
(1) Preparing modified starch: preparing high-amylose corn starch into 10% starch milk by using 95% DMSO solution, and heating and gelatinizing in a boiling water bath; after cooling to 90 ℃, dropwise adding 3 times of volume of absolute ethyl alcohol into the starch paste, and keeping stirring; centrifuging, taking out precipitate, drying, crushing and sieving to obtain modified starch;
(2) modified starch mixed limonene: mixing modified starch and limonene according to the mass ratio of 1:4, placing in a vacuum sealing bag, and placing for 24 hours under a vacuum condition;
(3) high hydrostatic pressure treatment: and (3) placing the vacuum sealing bag in a treatment kettle of high hydrostatic pressure equipment, filling water in the treatment kettle, sealing the treatment kettle, applying 100MPa pressure, maintaining the pressure for 30min, and taking out the modified starch-limonene mixture of the vacuum sealing bag to obtain the slow-release limonene inclusion compound.
(4) The application of the embedding object in strawberry bacteriostasis and preservation: uniformly placing the strawberries in a 1.5L sealing box according to the mass ratio of the embedding substances to the strawberries of 2:300, placing the embedding substances at the corners of the sealing box without directly contacting the strawberries, covering the sealing box, and storing at normal temperature.
Example 2
(1) Preparing modified starch: preparing high-amylose corn starch into 10% starch milk by using 95% DMSO solution, and heating and gelatinizing in a boiling water bath; after cooling to 90 ℃, dropwise adding 3 times of volume of absolute ethyl alcohol into the starch paste, and keeping stirring; centrifuging, taking out precipitate, drying, crushing and sieving to obtain modified starch;
(2) modified starch mixed limonene: mixing modified starch and limonene according to the mass ratio of 1:2, placing in a vacuum sealing bag, and placing for 24 hours under a vacuum condition;
(3) high hydrostatic pressure treatment: and (3) placing the vacuum sealing bag in a treatment kettle of high hydrostatic pressure equipment, filling water in the treatment kettle, sealing the treatment kettle, applying 100MPa pressure, maintaining the pressure for 30min, and taking out the modified starch-limonene mixture of the vacuum sealing bag to obtain the slow-release limonene embedded substance.
(4) The application of the embedding object in strawberry bacteriostasis and preservation: uniformly placing the strawberries in a 1.5L sealing box according to the mass ratio of the embedding substances to the strawberries of 2:300, placing the embedding substances at the corners of the sealing box without directly contacting the strawberries, covering the sealing box, and storing at normal temperature.
Example 3
1) Preparing modified starch: preparing high-amylose corn starch into 10% starch milk by using 95% DMSO solution, and heating and gelatinizing in a boiling water bath; after cooling to 90 ℃, dropwise adding 3 times of volume of absolute ethyl alcohol into the starch paste, and keeping stirring; centrifuging, taking out precipitate, drying, crushing and sieving to obtain modified starch;
(2) modified starch mixed limonene: mixing modified starch and limonene according to the mass ratio of 1:1, placing in a vacuum sealing bag, and placing for 24 hours under a vacuum condition;
(3) high hydrostatic pressure treatment: and (3) placing the vacuum sealing bag in a treatment kettle of high hydrostatic pressure equipment, filling water in the treatment kettle, sealing the treatment kettle, applying 100MPa pressure, maintaining the pressure for 30min, and taking out the modified starch-limonene mixture of the vacuum sealing bag to obtain the slow-release limonene embedded substance.
(4) The application of the embedding object in strawberry bacteriostasis and preservation: uniformly placing the strawberries in a 1.5L sealing box according to the mass ratio of the embedding substances to the strawberries being 4:300, placing the embedding substances at the corners of the sealing box without directly contacting the strawberries, covering the sealing box, and storing at normal temperature.
Example 4
1) Preparing modified starch: preparing high-amylose corn starch into 10% starch milk by using 95% DMSO solution, and heating and gelatinizing in a boiling water bath; after cooling to 90 ℃, dropwise adding 3 times of volume of absolute ethyl alcohol into the starch paste, and keeping stirring; centrifuging, taking out precipitate, drying, crushing and sieving to obtain modified starch;
(2) modified starch mixed limonene: mixing modified starch and limonene according to the mass ratio of 1:1, placing in a vacuum sealing bag, and placing for 24 hours under a vacuum condition;
(3) high hydrostatic pressure treatment: and (3) placing the vacuum sealing bag in a treatment kettle of high hydrostatic pressure equipment, filling water in the treatment kettle, sealing the treatment kettle, applying 100MPa pressure, maintaining the pressure for 30min, and taking out the modified starch-limonene mixture of the vacuum sealing bag to obtain the slow-release limonene embedded substance.
(4) The application of the embedding material in strawberry bacteriostasis and preservation: uniformly placing the strawberries in a 1.5L sealing box according to the mass ratio of the embedding substances to the strawberries of 2:300, placing the embedding substances at the corners of the sealing box without directly contacting the strawberries, covering the sealing box, and storing at normal temperature.
Example 5
(1) Preparing modified starch: dropwise adding 3mol/L NaOH into 10% starch milk, continuously stirring for 1h for gelatinization, neutralizing the pH value to about 7 by using 3mol/L ethanol hydrochloric acid solution, dropwise adding 3 times of volume of anhydrous ethanol into the starch milk, and keeping stirring; centrifuging, taking out precipitate, drying, crushing and sieving to obtain modified starch;
(2) modified starch mixed limonene: mixing modified starch and limonene according to the mass ratio of 1:4, placing in a vacuum sealing bag, and placing for 24 hours under a vacuum condition;
(3) high hydrostatic pressure treatment: and (3) placing the vacuum sealing bag in a treatment kettle of high hydrostatic pressure equipment, filling water in the treatment kettle, sealing the treatment kettle, applying 100MPa pressure, maintaining the pressure for 30min, and taking out the modified starch-limonene mixture of the vacuum sealing bag to obtain the slow-release limonene embedded substance.
(4) The application of the embedding object in strawberry bacteriostasis and preservation: uniformly placing the strawberries in a 1.5L sealing box according to the mass ratio of the embedding substances to the strawberries of 2:300, placing the embedding substances at the corners of the sealing box without directly contacting the strawberries, covering the sealing box, and storing at normal temperature.
Example 6
(1) Preparing modified starch: preparing high-amylose corn starch into 10% starch milk by using 95% DMSO solution, and heating and gelatinizing in a boiling water bath; after cooling to 90 ℃, dropwise adding 3 times of volume of absolute ethyl alcohol into the starch paste, and keeping stirring; centrifuging, taking out precipitate, drying, crushing and sieving to obtain modified starch;
(2) modified starch mixed limonene: mixing modified starch and limonene according to the mass ratio of 1:4, placing in a vacuum sealing bag, and placing for 24 hours under a vacuum condition;
(3) high hydrostatic pressure treatment: and (3) placing the vacuum sealing bag in a treatment kettle of high hydrostatic pressure equipment, filling water in the treatment kettle, sealing the treatment kettle, applying a pressure of 200MPa, maintaining the pressure for 15min, and taking out the modified starch-limonene mixture of the vacuum sealing bag to obtain the slow-release limonene embedded substance.
(4) The application of the embedding object in strawberry bacteriostasis and preservation: uniformly placing the strawberries in a 1.5L sealing box according to the mass ratio of the embedding substances to the strawberries of 2:300, placing the embedding substances at the corners of the sealing box without directly contacting the strawberries, covering the sealing box, and storing at normal temperature.
Example 7
(1) Preparing modified starch: preparing high amylose corn starch into 10% starch milk, heating in an oil bath, and continuously stirring for 1h for gelatinization; after cooling to 90 ℃, dropwise adding 3 times of volume of absolute ethyl alcohol into the starch paste, and keeping stirring; centrifuging, taking out precipitate, drying, crushing and sieving to obtain modified starch;
(2) modified starch mixed limonene: mixing modified starch and limonene according to the mass ratio of 1:4, placing in a vacuum sealing bag, and placing for 24 hours under a vacuum condition;
(3) high hydrostatic pressure treatment: and (3) placing the vacuum sealing bag in a treatment kettle of high hydrostatic pressure equipment, filling water in the treatment kettle, sealing the treatment kettle, applying 100MPa pressure, maintaining the pressure for 30min, and taking out the modified starch-limonene mixture of the vacuum sealing bag to obtain the slow-release limonene embedded substance.
(4) The application of the embedding object in strawberry bacteriostasis and preservation: uniformly placing the strawberries in a 1.5L sealing box according to the mass ratio of the embedding substances to the strawberries of 2:300, placing the embedding substances at the corners of the sealing box without directly contacting the strawberries, covering the sealing box, and storing at normal temperature.
Comparative example 1
Comparative example 1 differs from example 4 in that the native starch from which the destructurized starch is prepared is waxy corn starch, and is otherwise the same as that prepared in example 4.
Comparative example 2
Comparative example 2 is different from example 2 in that modified starch mixed with limonene is not subjected to high hydrostatic pressure treatment, and the other preparation is the same as example 2.
Comparative example 3
Comparative example 3 differs from example 3 in that the ratio of the embedding mass to the strawberry mass is 1:300, and the other preparation is the same as example 3.
Evaluation of Effect
1. Limonene content determination and controlled release performance evaluation
The method for measuring the content of limonene in the embedded substance comprises the following steps: accurately weigh 5mg of the investment into a 2mL microcentrifuge tube, add 0.5mL of 0.1M KOH solution, and vigorously mix the dispersion (for at least 30min) with a vortex mixer to give a clear solution. Then 0.5mL of ethyl acetate was added and mixed vigorously with a vortex mixer for 30 s. The mixture was centrifuged (9,391g,1min), and the supernatant collected after complete separation and analyzed by gas chromatography. And (4) converting the peak area of the limonene into the concentration according to the limonene standard.
The limonene content of the embedding materials prepared in examples 1-7 and comparative examples 1-3 was tested as shown in Table 1.
TABLE 1 limonene adsorption and encapsulation efficiency of the inclusion
As can be seen from Table 1 above, the embedding material prepared in example 2 has a somewhat higher limonene adsorption rate and encapsulation rate than the embedding material prepared in comparative example 2, and the high hydrostatic pressure treatment in the present invention is proved to improve the adsorption of limonene by the modified starch. The higher limonene adsorption of example 4 relative to comparative example 1 demonstrates that the modified starch prepared from waxy corn starch does not adsorb limonene as well as high amylose corn starch, probably due to the low amylose content of waxy corn starch, indicating that the source of starch is important in preparing the investment and that appropriate gelatinization methods are selected for the different starch feedstocks. As can be seen from examples 1, 6 and 7, the three gelatinization methods provided by the present invention all have good effect in preparing modified starch. From examples 1-7, it can be seen that the method provided by the invention can increase the encapsulation efficiency of limonene to above about 70%, which proves that the method effectively improves the encapsulation effect of limonene.
In addition, the limonene-releasing properties of the inclusion prepared in example 2 and comparative example 2 were investigated under certain conditions of temperature and relative humidity. 1.0g of the inclusion was placed in a plate and placed in a desiccator (37%, 25 ℃) having a certain humidity for a certain period of time, and the change in the content of limonene in the inclusion was analyzed by gas chromatography (see FIG. 1).
Tests show that the release rate of limonene from the inclusion prepared in example 2 is lower than that of the inclusion prepared in comparative example 2, and that both inclusions can achieve the effect of controlled release of limonene. Only 30% of the limonene was released from the inclusion prepared in example 2 after standing for 96 h; the embedding material prepared in comparative example 2 is completely released after being placed for 72 hours; and the same-mass limonene is completely released within 30 hours, which proves that the preparation method of the slow-release limonene embedded substance provided by the invention has an obvious effect.
2. Application of embedding object in strawberry bacteriostasis and preservation
The experiment is divided into an experimental group, a control group and a blank group, and the samples used in the experimental group are the embedded substances prepared in the examples and the comparative examples. The control group was non-embedded limonene and the blank group was added with neither limonene nor embedding.
The experimental conditions are room temperature environment, the experimental period is 7 days, and the Chinese strawberry in the box is subjected to mass loss (%), rotting grade (%), chroma (C), soluble solid content (%) and hardness (kgf/cm)2) The measurement of (1).
As can be seen from table 2, after 7 days of storage, the strawberries in the inclusion treated groups prepared in examples 1 to 7 and comparative examples 1 to 3 exhibited better quality loss, rot level, chroma, soluble solid content and hardness than those of the control group and the blank group, which indicates that the preparation method provided by the present invention indeed effectively delays the rot of strawberries during storage by slowly releasing limonene. In addition, it was also noted in terms of odor that the strawberries of the blank group developed an acid odor after 7 days of storage, whereas the strawberries of examples 1 to 7 and comparative examples 1 to 3 had no noticeable rancid odor. Compared with the examples 1 to 7, the comparative examples 1 to 3 are poorer in performance of each index, which shows that the final fresh-keeping and bacteriostatic effect of the embedding object is related to the content of limonene contained in the embedding object, the more limonene can be loaded in the embedding object, the better the final bacteriostatic and fresh-keeping effect is, compared with the examples 2 and 4, the embedding object prepared in the example 1 has a better bacteriostatic and fresh-keeping effect on strawberries, which shows that the addition proportion of the limonene is very important when the embedding object is prepared, and the more limonene is added in the threshold value range, the better the preservative effect of the final embedding object is exerted. Compared with comparative example 3, the fresh-keeping effect of examples 3 and 4 is better, which shows that when the embedding material is used for strawberry fresh keeping, the more the amount of the embedding material is put into, the better the bacteriostatic fresh-keeping effect is.
TABLE 2 application of the embedding substance in strawberry bacteriostasis and preservation (after 7 days of storage)
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. A preparation method of a slow-release limonene embedded substance is characterized by comprising the following steps:
(1) gelatinizing starch, dropwise adding 2-4 times of anhydrous ethanol into the starch paste at 80-90 ℃, and keeping stirring; centrifuging, taking out precipitate, drying and crushing to obtain modified starch;
(2) mixing limonene with modified starch according to the mass ratio of more than or equal to 0.1, placing the mixture in a vacuum sealing bag, and placing the vacuum sealing bag for 12-24 hours under a vacuum condition;
(3) and (3) placing the vacuum sealing bag in a treatment kettle of high hydrostatic pressure equipment, filling water in the treatment kettle, sealing the treatment kettle, applying pressure of 50-300 MPa, maintaining the pressure for 10-30 min, and taking out the modified starch-limonene mixture of the vacuum sealing bag to obtain the slow-release limonene embedded substance.
2. The method for preparing the starch paste as claimed in claim 1, wherein the method for gelatinizing the starch in the step (1) comprises any one of the following:
1) preparing starch into starch milk, heating in boiling water bath or oil bath, stirring for more than 1h, and gelatinizing;
2) preparing starch into starch milk by using DMSO (dimethyl sulfoxide) solution with the concentration of more than 70%, heating in a boiling water bath, and stirring for more than 1h for gelatinization;
3) adding the starch milk dropwise with an alkali solution, and stirring for more than 1h for gelatinization.
3. The preparation method according to claim 2, wherein the mass fraction of the starch milk is 10-15%.
4. The method of claim 3, wherein the alkali solution is KCl, KOH, or NaOH solution.
5. The preparation method according to any one of claims 1 to 4, wherein the starch in step (1) is high amylose starch, the amylose content being greater than 50%; the starch is corn starch, rice starch and wheat starch; the water content of the modified starch is 14-16%.
6. The preparation method according to any one of claims 1 to 4, wherein the vacuum sealed bag in the step (2) is a PAPE vacuum packaging bag, and the vacuum degree is-0.06 to-0.1 MPa.
7. The preparation method according to any one of claims 1 to 4, wherein the mass ratio of the modified starch to the limonene is 1: 1-4; the limonene is dextro-limonene.
8. The method according to any one of claims 1 to 4, wherein the high hydrostatic pressure treatment in step (3) is performed under a pressure of 100 to 200 MPa; the adding amount of the sample is 10-30% of the volume of the treatment kettle.
9. A slow release limonene inclusion prepared according to any one of claims 1-8.
10. The application of the slow-release limonene inclusion in fruit and vegetable bacteriostasis and freshness preservation according to claim 9, wherein the inclusion and the fruit and vegetable are placed in a sealed box, and the mass ratio of the inclusion to the fruit and vegetable is more than or equal to 2: 300.
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| US4911952A (en) * | 1987-07-10 | 1990-03-27 | The United States Of America As Represented By The Secretary Of Agriculture | Encapsulation by entrapment within matrix of unmodified starch |
| CN110064375A (en) * | 2019-04-11 | 2019-07-30 | 华南理工大学 | A kind of modified starch preparation method with efficient absorption and controlled release ethylene |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4911952A (en) * | 1987-07-10 | 1990-03-27 | The United States Of America As Represented By The Secretary Of Agriculture | Encapsulation by entrapment within matrix of unmodified starch |
| CN110064375A (en) * | 2019-04-11 | 2019-07-30 | 华南理工大学 | A kind of modified starch preparation method with efficient absorption and controlled release ethylene |
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| 关天旺等: "柠檬烯的防腐作用及抑菌机理研究进展", 《保鲜与加工》 * |
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