CN114698682B - Sustained-release limonene embedded material, preparation method thereof and application thereof in fruit and vegetable antibacterial fresh-keeping - Google Patents
Sustained-release limonene embedded material, preparation method thereof and application thereof in fruit and vegetable antibacterial fresh-keeping Download PDFInfo
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- CN114698682B CN114698682B CN202210459169.8A CN202210459169A CN114698682B CN 114698682 B CN114698682 B CN 114698682B CN 202210459169 A CN202210459169 A CN 202210459169A CN 114698682 B CN114698682 B CN 114698682B
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- XMGQYMWWDOXHJM-UHFFFAOYSA-N limonene Chemical compound CC(=C)C1CCC(C)=CC1 XMGQYMWWDOXHJM-UHFFFAOYSA-N 0.000 title claims abstract description 184
- 229940087305 limonene Drugs 0.000 title claims abstract description 101
- 235000001510 limonene Nutrition 0.000 title claims abstract description 92
- 235000012055 fruits and vegetables Nutrition 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 9
- 238000013268 sustained release Methods 0.000 title claims description 4
- 239000012730 sustained-release form Substances 0.000 title claims description 4
- 239000000463 material Substances 0.000 title description 10
- 238000007789 sealing Methods 0.000 claims abstract description 69
- 229920000881 Modified starch Polymers 0.000 claims abstract description 53
- 235000019426 modified starch Nutrition 0.000 claims abstract description 53
- 239000004368 Modified starch Substances 0.000 claims abstract description 51
- 239000000126 substance Substances 0.000 claims abstract description 46
- 229920002472 Starch Polymers 0.000 claims abstract description 44
- 235000019698 starch Nutrition 0.000 claims abstract description 42
- 239000008107 starch Substances 0.000 claims abstract description 42
- 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 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 238000011049 filling Methods 0.000 claims abstract description 10
- 239000002244 precipitate Substances 0.000 claims abstract description 10
- 238000010298 pulverizing process Methods 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 4
- 238000003825 pressing Methods 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 28
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 21
- 229920002261 Corn starch Polymers 0.000 claims description 14
- 239000008120 corn starch Substances 0.000 claims description 14
- 235000013336 milk Nutrition 0.000 claims description 14
- 239000008267 milk Substances 0.000 claims description 14
- 210000004080 milk Anatomy 0.000 claims description 14
- 229920000856 Amylose Polymers 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 10
- 238000009835 boiling Methods 0.000 claims description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 7
- XMGQYMWWDOXHJM-JTQLQIEISA-N (+)-α-limonene Chemical group CC(=C)[C@@H]1CCC(C)=CC1 XMGQYMWWDOXHJM-JTQLQIEISA-N 0.000 claims description 2
- 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
- 239000003513 alkali Substances 0.000 claims 2
- 238000003860 storage Methods 0.000 abstract description 6
- 241000220223 Fragaria Species 0.000 description 52
- 235000021012 strawberries Nutrition 0.000 description 38
- 230000000052 comparative effect Effects 0.000 description 19
- 230000000694 effects Effects 0.000 description 16
- 235000016623 Fragaria vesca Nutrition 0.000 description 14
- 235000011363 Fragaria x ananassa Nutrition 0.000 description 14
- 238000005538 encapsulation Methods 0.000 description 12
- 239000000243 solution Substances 0.000 description 10
- 238000001179 sorption measurement Methods 0.000 description 8
- 238000000643 oven drying Methods 0.000 description 7
- 238000007873 sieving Methods 0.000 description 7
- 238000001816 cooling Methods 0.000 description 6
- 235000013305 food Nutrition 0.000 description 5
- 239000007943 implant Substances 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- 238000004321 preservation Methods 0.000 description 4
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 235000005979 Citrus limon Nutrition 0.000 description 2
- 244000131522 Citrus pyriformis Species 0.000 description 2
- 239000012670 alkaline solution Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000013270 controlled release Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 238000004817 gas chromatography Methods 0.000 description 2
- 210000003000 inclusion body Anatomy 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 235000016709 nutrition Nutrition 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000003755 preservative agent Substances 0.000 description 2
- 230000002335 preservative effect Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 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
- 230000002378 acidificating effect Effects 0.000 description 1
- 150000001491 aromatic compounds Chemical class 0.000 description 1
- 230000003385 bacteriostatic effect Effects 0.000 description 1
- 238000010170 biological method Methods 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
- 239000000306 component Substances 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 235000012041 food component Nutrition 0.000 description 1
- 239000005428 food component Substances 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000001027 hydrothermal synthesis 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
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 235000013599 spices Nutrition 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 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
- 230000002588 toxic effect Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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
Landscapes
- 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 embedding substance, a preparation method thereof and application thereof in fruit and vegetable antibacterial fresh-keeping, comprising the following steps: (1) Gelatinizing starch, dropwise adding 2-4 times of absolute ethyl alcohol into the starch paste at 80-90 ℃ and stirring; centrifuging, collecting precipitate, drying, and pulverizing to obtain modified starch; (2) Mixing limonene and modified starch according to the mass ratio of not less than 0.1, placing the mixture in a vacuum sealing bag, and placing the vacuum sealing bag under the vacuum condition for 12-24 hours; (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 embedding substance. The invention can effectively improve the slow release performance of the limonene, and the embedded matter is used for bacteriostasis and fresh-keeping of fruits and vegetables, and can obviously prolong the storage time of the fruits and vegetables at normal temperature.
Description
Technical Field
The invention belongs to the field of fruit and vegetable fresh-keeping, and particularly relates to a preparation method of a slow-release limonene embedded matter and application of the slow-release limonene embedded matter in strawberry antibacterial fresh-keeping.
Background
The fruits and vegetables are natural nutritional food, contain various nutritional substances required by life of people, and are easy to rot in the processes of storage, transportation and sales due to strong seasonality and high regional property of fruit and vegetable production and high water content. At present, the technical means for fruit and vegetable fresh-keeping can be mainly divided into three types: physical, chemical and biological methods. In the physical method, the high hydrostatic pressure fresh-keeping technology is to process under static high pressure (100-1000 MPa) and a certain temperature to cause non-covalent bond destruction or formation of food components, denature and inactivate biological polymer substances in food and kill microorganisms in food to achieve the purpose of fresh keeping.
In the chemical method, the safety residue problem of the chemical preservative can not meet the high requirements of consumers on food safety, and the natural extract is used as the preservative, so that the natural extract becomes a research hot spot in the field of fruit and vegetable preservation. Limonene alias limonene has lemon fragrance, and can be used as raw material for preparing artificial orange flower, sweet flower, lemon and bergamot oil, and the source is mainly waste orange peel. The limonene has proved to have good antibacterial effect, can effectively inhibit escherichia coli, staphylococcus aureus, bacillus subtilis, aspergillus niger and the like, is expressed as an unlimited amount by the international daily essence and spice society, and has been widely used for fruit and vegetable fresh-keeping in recent years because the limonene cannot accumulate in a human body to generate toxic and side effects. However, in the practical application process of limonene, the high volatility of the limonene at normal temperature often limits the use of the limonene, so that an embedding method is necessary to improve the slow release effect of the limonene, and the limonene is better applied to the field of fruit and vegetable fresh-keeping.
The linear component of starch mainly comprises amylose and some linear fragments of branched side chains, and can form non-covalent inclusion compounds with various small molecules in food such as iodine, alcohol, fatty acid and esters thereof, emulsifying agents, aromatic compounds and the like. In forming the molecular complex, amylose exists in the form of a left-handed single helix, with hydroxyl groups on the outer surface and methylene and glycosidic linkages on the inner surface, thus forming a hydrophobic helical cavity with a hydrophilic outer surface and capable of accommodating the guest molecule, and the helices tend to pack together to form a V-shaped crystal structure. It has been proved by researches that the slow release effect can be achieved by embedding the fragrant substances such as menthol, cinnamaldehyde and the like into the modified starch with V-shaped crystals, however, the encapsulation method mostly adopts a pasting mode and then a hydrothermal mode, has the defects of time consumption and low recovery ratio, and causes slow formation speed of embedding 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, there are also solid encapsulation methods, which have simple operation process, can avoid the above disadvantages, but have the limitations of low encapsulation efficiency and poor slow release effect. Based on this, there is a need for improved solid encapsulation technology for modified starches to achieve a method for preparing an implant with sustained release properties that is simpler to operate, less costly and more effective.
Disclosure of Invention
The invention aims to provide a limonene solid encapsulation method with slow release performance, which is characterized in that modified starch is used for embedding limonene, and high hydrostatic pressure treatment is applied at the same time, so that the limonene can be pushed to contact on the surface or the binding sites of pores of the modified starch on the premise of not damaging the limonene, the adsorption of the modified starch to the limonene is improved, the slow release effect of the limonene is achieved at normal temperature, and further 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 embedding substance, which comprises the following steps:
(1) Preparing modified starch; gelatinizing starch, dropwise adding 2-4 times of absolute ethyl alcohol into the starch paste at 80-90 ℃ and stirring; centrifuging, collecting precipitate, drying, and pulverizing to obtain modified starch;
(2) Modified starch mixed limonene: mixing limonene and modified starch according to the mass ratio of not less than 0.1, placing the mixture in a vacuum sealing bag, and placing the vacuum sealing bag under the vacuum condition for 12-24 hours;
(3) High hydrostatic pressure treatment: 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 embedding substance.
Preferably, the method for gelatinizing starch in step (1) comprises any of the following:
1) Preparing starch into starch milk by a high-temperature hydrothermal method, heating in a boiling water bath or an oil bath, and stirring for more than 1h to gelatinize;
2) Preparing starch into starch milk by DMSO solution with concentration of above 70%, heating in boiling water bath, stirring for above 1 hr, and gelatinizing;
3) The alkaline method is to add alkaline solution into starch milk drop by drop, keep stirring for more than 1h to gelatinize.
Preferably, the mass fraction of the starch milk is 10-15%.
Preferably, the alkaline solution is KCl, KOH, naOH solution.
Preferably, the starch in 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 modified starch of step (1) has a water content of 14-16%.
Preferably, the vacuum sealing bag in the step (2) adopts a PAPE vacuum packaging bag, and the vacuum condition is that the vacuum degree is-0.06 to-0.1 MPa.
Preferably, the mass ratio of the modified starch to the limonene is 1:1-4; the limonene is d-limonene.
Preferably, in the high hydrostatic pressure treatment in the step (3), the applied pressure is 100-200 MPa; the addition amount of the sample is 10-30% of the volume of the treatment kettle.
The application of the slow-release limonene embedded substance prepared by the method in bacteriostasis and fresh-keeping of fruits and vegetables is characterized in that the embedded substance and the fruits and vegetables are placed in a sealing 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 embedded matter 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 the limonene, the prepared modified starch is adopted to adsorb the limonene and high hydrostatic pressure treatment is applied, the adsorption rate can reach 61.1-68.8%, and the encapsulation rate can reach 60.8-85.9%.
(2) The embedded material prepared by the invention has slow release property on limonene, and the sample prepared by high hydrostatic pressure treatment has better slow release effect on limonene, and can be released for more than 4 days longer than the sample without embedded limonene (volatilized after 1 day).
(3) Compared with the traditional spray drying method, the method avoids the loss of the limonene under the high temperature condition, and has low process energy consumption; compared with the traditional embedding method carried out under a liquid phase system, the solid-state encapsulation method has the advantages of simple operation steps, lower cost and good embedding effect.
(4) The modified starch has wide sources and low cost, and the preparation method of the modified starch is various and simple and is suitable for industrial production.
(5) The prepared embedded substance has the characteristic of slowly releasing the limonene, can be used for preserving fruits and vegetables, and can achieve the effect of prolonging the shelf life of the fruits and vegetables without directly contacting with the fruits and vegetables.
Drawings
FIG. 1 is a graph showing the release of the entrapping immobilization pellets prepared in example 2 and comparative example 2 at 25℃and 37% relative humidity.
Detailed Description
Examples and comparative examples high amylose corn starch and waxy corn starch are used as raw materials, but should not limit the scope of the invention.
Example 1
(1) Preparing modified starch: preparing high-amylose corn starch into starch milk with the mass fraction of 10% by using 95% DMSO solution, and heating and gelatinizing in a boiling water bath; after cooling to 90 ℃,3 times of absolute ethyl alcohol is added into the starch paste dropwise, and stirring is kept; centrifuging, collecting precipitate, oven drying, pulverizing, and sieving to obtain modified starch;
(2) Modified starch mixed limonene: mixing modified starch and limonene according to a mass ratio of 1:4, placing in a vacuum sealing bag, and placing under vacuum condition for 24h;
(3) High hydrostatic pressure treatment: 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 embedding substance.
(4) The application of the embedded substance in strawberry bacteriostasis and fresh-keeping: taking strawberries according to the mass ratio of the embedding substance to the strawberries of 2:300, uniformly placing the strawberries in a 1.5L sealing box, placing the embedding substance at corners of the sealing box, not directly contacting the strawberries, covering the sealing box, and storing the strawberries at normal temperature.
Example 2
(1) Preparing modified starch: preparing high-amylose corn starch into starch milk with the mass fraction of 10% by using 95% DMSO solution, and heating and gelatinizing in a boiling water bath; after cooling to 90 ℃,3 times of absolute ethyl alcohol is added into the starch paste dropwise, and stirring is kept; centrifuging, collecting precipitate, oven drying, pulverizing, and sieving to obtain modified starch;
(2) Modified starch mixed limonene: mixing modified starch and limonene according to a mass ratio of 1:2, placing in a vacuum sealing bag, and placing under vacuum condition for 24h;
(3) High hydrostatic pressure treatment: 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 embedding substance.
(4) The application of the embedded substance in strawberry bacteriostasis and fresh-keeping: taking strawberries according to the mass ratio of the embedding substance to the strawberries of 2:300, uniformly placing the strawberries in a 1.5L sealing box, placing the embedding substance at corners of the sealing box, not directly contacting the strawberries, covering the sealing box, and storing the strawberries at normal temperature.
Example 3
1) Preparing modified starch: preparing high-amylose corn starch into starch milk with the mass fraction of 10% by using 95% DMSO solution, and heating and gelatinizing in a boiling water bath; after cooling to 90 ℃,3 times of absolute ethyl alcohol is added into the starch paste dropwise, and stirring is kept; centrifuging, collecting precipitate, oven drying, pulverizing, and sieving to obtain modified starch;
(2) Modified starch mixed limonene: mixing modified starch and limonene according to a mass ratio of 1:1, placing the mixture in a vacuum sealing bag, and placing the vacuum sealing bag under a vacuum condition for 24 hours;
(3) High hydrostatic pressure treatment: 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 embedding substance.
(4) The application of the embedded substance in strawberry bacteriostasis and fresh-keeping: according to the mass ratio of the embedded matters to the strawberries of 4:300, strawberries are taken and uniformly placed in a 1.5L sealing box, the embedded matters are placed at corners of the sealing box and are not in direct contact with the strawberries, the sealing box is covered, and the strawberries are stored at normal temperature.
Example 4
1) Preparing modified starch: preparing high-amylose corn starch into starch milk with the mass fraction of 10% by using 95% DMSO solution, and heating and gelatinizing in a boiling water bath; after cooling to 90 ℃,3 times of absolute ethyl alcohol is added into the starch paste dropwise, and stirring is kept; centrifuging, collecting precipitate, oven drying, pulverizing, and sieving to obtain modified starch;
(2) Modified starch mixed limonene: mixing modified starch and limonene according to a mass ratio of 1:1, placing the mixture in a vacuum sealing bag, and placing the vacuum sealing bag under a vacuum condition for 24 hours;
(3) High hydrostatic pressure treatment: 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 embedding substance.
(4) The application of the embedded substance in strawberry bacteriostasis and fresh-keeping: taking strawberries according to the mass ratio of the embedding substance to the strawberries of 2:300, uniformly placing the strawberries in a 1.5L sealing box, placing the embedding substance at corners of the sealing box, not directly contacting the strawberries, covering the sealing box, and storing the strawberries at normal temperature.
Example 5
(1) Preparing modified starch: dropwise adding 3mol/L NaOH into 10% starch milk, continuously stirring for 1h to gelatinize, neutralizing the pH value of 3mol/L ethanol acid solution to about 7, dropwise adding 3 times volume of absolute ethanol into the starch paste, and keeping stirring; centrifuging, collecting precipitate, oven drying, pulverizing, and sieving to obtain modified starch;
(2) Modified starch mixed limonene: mixing modified starch and limonene according to a mass ratio of 1:4, placing in a vacuum sealing bag, and placing under vacuum condition for 24h;
(3) High hydrostatic pressure treatment: 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 embedding substance.
(4) The application of the embedded substance in strawberry bacteriostasis and fresh-keeping: taking strawberries according to the mass ratio of the embedding substance to the strawberries of 2:300, uniformly placing the strawberries in a 1.5L sealing box, placing the embedding substance at corners of the sealing box, not directly contacting the strawberries, covering the sealing box, and storing the strawberries at normal temperature.
Example 6
(1) Preparing modified starch: preparing high-amylose corn starch into starch milk with the mass fraction of 10% by using 95% DMSO solution, and heating and gelatinizing in a boiling water bath; after cooling to 90 ℃,3 times of absolute ethyl alcohol is added into the starch paste dropwise, and stirring is kept; centrifuging, collecting precipitate, oven drying, pulverizing, and sieving to obtain modified starch;
(2) Modified starch mixed limonene: mixing modified starch and limonene according to a mass ratio of 1:4, placing in a vacuum sealing bag, and placing under vacuum condition for 24h;
(3) High hydrostatic pressure treatment: 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 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 embedding substance.
(4) The application of the embedded substance in strawberry bacteriostasis and fresh-keeping: taking strawberries according to the mass ratio of the embedding substance to the strawberries of 2:300, uniformly placing the strawberries in a 1.5L sealing box, placing the embedding substance at corners of the sealing box, not directly contacting the strawberries, covering the sealing box, and storing the strawberries at normal temperature.
Example 7
(1) Preparing modified starch: preparing high-amylose corn starch into starch milk with the mass fraction of 10%, heating in an oil bath, and continuously stirring for 1h to gelatinize; after cooling to 90 ℃,3 times of absolute ethyl alcohol is added into the starch paste dropwise, and stirring is kept; centrifuging, collecting precipitate, oven drying, pulverizing, and sieving to obtain modified starch;
(2) Modified starch mixed limonene: mixing modified starch and limonene according to a mass ratio of 1:4, placing in a vacuum sealing bag, and placing under vacuum condition for 24h;
(3) High hydrostatic pressure treatment: 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 embedding substance.
(4) The application of the embedded substance in strawberry bacteriostasis and fresh-keeping: taking strawberries according to the mass ratio of the embedding substance to the strawberries of 2:300, uniformly placing the strawberries in a 1.5L sealing box, placing the embedding substance at corners of the sealing box, not directly contacting the strawberries, covering the sealing box, and storing the strawberries at normal temperature.
Comparative example 1
Comparative example 1 differs from example 4 in that the raw starch of the modified starch prepared is waxy corn starch, otherwise the same as that of example 4.
Comparative example 2
Comparative example 2 was different from example 2 in that modified starch was not subjected to high hydrostatic pressure treatment after mixing limonene, and the preparation was otherwise the same as that of example 2.
Comparative example 3
Comparative example 3 differs from example 3 in that the ratio of the embedded material to the strawberry mass was 1:300, otherwise the same preparation as example 3.
Evaluation of Effect
1. Limonene content measurement and controlled release performance evaluation
The method for measuring the content of limonene in the embedded material comprises the following steps: accurately weigh 5mg of the entrapping material in a 2mL microcentrifuge tube, add 0.5mL of 0.1M KOH solution, and vigorously mix the dispersion (at least 30 min) using a vortex mixer to give a clear solution. Then 0.5mL ethyl acetate was added and mixed vigorously with a vortex mixer for 30s. The mixture was centrifuged (9,399 g,1 min), and the supernatant was collected after complete separation and analyzed by gas chromatography. Peak area of limonene was converted to concentration according to the limonene standard.
The limonene content of the prepared implants of examples 1-7 and comparative examples 1-3 was tested as shown in Table 1.
Table 1 limonene adsorption and encapsulation efficiency of the implants
As can be seen from Table 1 above, the inclusion compound prepared in example 2 has a higher limonene adsorption and encapsulation efficiency than that of comparative example 2, and the high hydrostatic pressure treatment in the present invention is proved to improve the limonene adsorption of the modified starch. The higher adsorption of limonene compared to comparative example 1, example 4, demonstrates that modified starches prepared with waxy corn starch do not have as much adsorption effect on limonene 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 inclusion compound and that a suitable gelatinization process is selected for the different starch materials. As can be seen from examples 1, 6 and 7, the three gelatinization methods provided by the present invention all achieve good results in the preparation of modified starch. From examples 1-7, it can be seen that the method provided by the invention can improve the encapsulation efficiency of limonene to more than about 70%, and the encapsulation effect of limonene is effectively improved.
In addition, the limonene slow release properties of the implants prepared in example 2 and comparative example 2 were investigated under certain temperature and relative humidity conditions. 1.0g of the inclusion bodies were placed in a desiccator (37%, 25 ℃) with a certain humidity in a dish for a while, and the inclusion bodies were analyzed for the change in the content of limonene by gas chromatography (see FIG. 1).
The test shows that the embedded material prepared in example 2 has lower release rate of limonene than the embedded material prepared in comparative example 2, and both embedded materials can achieve the controlled release effect of limonene. The inclusion prepared in example 2 released only 30% of the limonene after 96 hours of standing; the embedding substance prepared in comparative example 2 was completely released after being left for 72 hours; and the mass limonene is completely released after 30 hours, so that the preparation method of the slow-release limonene embedding substance provided by the invention has obvious effect.
2. Application of embedding substance in strawberry bacteriostasis and fresh-keeping
The experiments were divided into an experimental group, a control group and a blank group, and samples used in the experimental group were the implants prepared in examples and comparative examples. The control group was non-embedded limonene, and the blank group was neither added with limonene nor embedded.
The experimental conditions were room temperature environment with an experimental period of 7 days, and the strawberries in the box were taken for mass loss (%), number of rotting (%), chroma (C), soluble solids content (%) and hardness (kgf/cm) 2 ) Is measured.
As can be seen from the above Table 2, after 7 days of storage, the quality loss, the number of rotting stages, the chroma, the content of soluble solids and the hardness of the strawberry of the embedded treatment group prepared in examples 1 to 7 and comparative examples 1 to 3 are superior to those of the control group and the blank group, and the preparation method provided by the invention is proved to effectively delay the rotting of the strawberry in the storage process by slowly releasing limonene. In addition, the strawberries of the blank group were odorous and developed an acidic odor after 7 days of storage, whereas strawberries of the treatment groups of examples 1 to 7 and comparative examples 1 to 3 had no noticeable rancid odor. Compared with examples 1-7, comparative examples 1-3 show poorer performance of various indexes, which shows that the final fresh-keeping and antibacterial effects of the embedded objects are related to the content of limonene contained in the embedded objects, the more limonene can be loaded in the embedded objects, the better the final fresh-keeping and antibacterial effects are, and compared with examples 2 and 4, the better the fresh-keeping and antibacterial effects of the embedded objects prepared in example 1 on strawberries are, which shows that the addition proportion of limonene is important when the embedded objects are prepared, and the more the addition amount of limonene is in a threshold range, the more the fresh-keeping effect of the final embedded objects is beneficial. The preservation effect of examples 3 and 4 is better than that of comparative example 3, indicating that the greater the amount of the embedding substance that is put into the preservation of the strawberry, the better the bacteriostatic preservation effect.
Table 2 application of the embedded matters in strawberry bacteriostasis and fresh-keeping (after 7 days of storage)
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.
Claims (7)
1. The preparation method of the slow-release limonene embedded matter is characterized by comprising the following steps of:
(1) Gelatinizing starch, dropwise adding 2-4 times of absolute ethyl alcohol into the starch paste at the temperature of 80-90 ℃ and stirring; centrifuging, collecting precipitate, drying, and pulverizing to obtain modified starch;
(2) Mixing limonene and modified starch according to the mass ratio of not less than 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) 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 a modified starch-limonene mixture of the vacuum sealing bag to obtain a slow-release limonene embedding substance;
the method for gelatinizing starch in the step (1) comprises any one of the following steps:
1) Preparing starch into starch milk with the mass fraction of 10-15%, heating in boiling water bath or oil bath, and stirring for more than 1h to gelatinize;
2) Preparing starch into starch milk by using DMSO solution with concentration of more than 70%, heating in boiling water bath, and stirring for more than 1h to gelatinize;
3) Dropwise adding an alkali solution into the starch milk, and stirring for more than 1h to gelatinize;
the starch in the step (1) is high-amylose starch, and the content of the amylose starch is more than 50%; the starch is corn starch, rice starch and wheat starch; the water content of the modified starch is 14-16%.
2. The method according to claim 1, wherein the alkali solution is a KOH solution or a NaOH solution.
3. The method according to claim 1 or 2, wherein the vacuum sealing bag in the step (2) is a PAPE vacuum packaging bag, and the vacuum condition is vacuum degree of-0.06 to-0.1 MPa.
4. The preparation method according to claim 1 or 2, wherein the mass ratio of the modified starch to the limonene is 1:1-4; the limonene is dextro-limonene.
5. The preparation method according to claim 1 or 2, wherein the pressure applied in the high hydrostatic pressure treatment in the step (3) is 100 to 200mpa; the addition amount of the sample is 10-30% of the volume of the treatment kettle.
6. A sustained-release limonene embedded prepared by the method of any one of claims 1-5.
7. The application of the slow-release limonene embedded in fruit and vegetable antibacterial fresh-keeping as claimed in claim 6, wherein the embedded and the fruit and vegetable are placed in a sealing box, and the mass ratio of the embedded to the fruit and vegetable is more than or equal to 2:300.
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Citations (2)
| 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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Patent Citations (2)
| 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 |
Non-Patent Citations (1)
| Title |
|---|
| 淀粉基食品微胶囊递送体系的构建及其控释特性研究进展;王百龙等;《食品科学》(第15期);第329-337页 * |
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