CN118000250A - Quick-frozen film coating liquid for fruits and vegetables and preparation method thereof - Google Patents
Quick-frozen film coating liquid for fruits and vegetables and preparation method thereof Download PDFInfo
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- CN118000250A CN118000250A CN202410413896.XA CN202410413896A CN118000250A CN 118000250 A CN118000250 A CN 118000250A CN 202410413896 A CN202410413896 A CN 202410413896A CN 118000250 A CN118000250 A CN 118000250A
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- pineapple
- aloe
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- 239000007788 liquid Substances 0.000 title claims abstract description 56
- 235000012055 fruits and vegetables Nutrition 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000007888 film coating Substances 0.000 title claims description 31
- 238000009501 film coating Methods 0.000 title claims description 31
- 241000234671 Ananas Species 0.000 claims abstract description 43
- 235000007119 Ananas comosus Nutrition 0.000 claims abstract description 43
- 238000000576 coating method Methods 0.000 claims abstract description 42
- 239000011248 coating agent Substances 0.000 claims abstract description 41
- 235000011399 aloe vera Nutrition 0.000 claims abstract description 35
- 239000000284 extract Substances 0.000 claims abstract description 35
- 241001116389 Aloe Species 0.000 claims abstract description 34
- 238000010438 heat treatment Methods 0.000 claims abstract description 28
- 229940069521 aloe extract Drugs 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 11
- 239000000243 solution Substances 0.000 claims description 97
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 83
- 239000008367 deionised water Substances 0.000 claims description 49
- 229910021641 deionized water Inorganic materials 0.000 claims description 49
- 238000003756 stirring Methods 0.000 claims description 48
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 36
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 36
- 229920001661 Chitosan Polymers 0.000 claims description 32
- 125000002057 carboxymethyl group Chemical group [H]OC(=O)C([H])([H])[*] 0.000 claims description 32
- 229920001046 Nanocellulose Polymers 0.000 claims description 31
- 238000005406 washing Methods 0.000 claims description 30
- 230000001276 controlling effect Effects 0.000 claims description 28
- 239000000047 product Substances 0.000 claims description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 25
- 239000011259 mixed solution Substances 0.000 claims description 24
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 22
- 239000002244 precipitate Substances 0.000 claims description 20
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 18
- 238000001914 filtration Methods 0.000 claims description 18
- 229940013712 pineapple extract Drugs 0.000 claims description 18
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 16
- 238000000227 grinding Methods 0.000 claims description 13
- 238000006243 chemical reaction Methods 0.000 claims description 12
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 12
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- 238000009210 therapy by ultrasound Methods 0.000 claims description 12
- 238000009777 vacuum freeze-drying Methods 0.000 claims description 12
- 240000002234 Allium sativum Species 0.000 claims description 11
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 claims description 11
- 229920002678 cellulose Polymers 0.000 claims description 11
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- 239000000600 sorbitol Substances 0.000 claims description 11
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 229920000742 Cotton Polymers 0.000 claims description 8
- 238000005520 cutting process Methods 0.000 claims description 7
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 6
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- 235000019253 formic acid Nutrition 0.000 claims description 6
- 239000005457 ice water Substances 0.000 claims description 6
- 230000007935 neutral effect Effects 0.000 claims description 6
- 239000008055 phosphate buffer solution Substances 0.000 claims description 6
- 239000012264 purified product Substances 0.000 claims description 6
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- 238000010790 dilution Methods 0.000 claims description 5
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- 238000001816 cooling Methods 0.000 claims description 2
- 239000002159 nanocrystal Substances 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 229960002920 sorbitol Drugs 0.000 claims description 2
- 239000003963 antioxidant agent Substances 0.000 abstract description 14
- 230000003078 antioxidant effect Effects 0.000 abstract description 13
- 230000000694 effects Effects 0.000 abstract description 7
- 235000013305 food Nutrition 0.000 abstract description 7
- 230000003647 oxidation Effects 0.000 abstract description 6
- 238000007254 oxidation reaction Methods 0.000 abstract description 6
- 102000030523 Catechol oxidase Human genes 0.000 abstract description 5
- 108010031396 Catechol oxidase Proteins 0.000 abstract description 5
- 235000013824 polyphenols Nutrition 0.000 abstract description 5
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- 238000012360 testing method Methods 0.000 description 15
- 235000006708 antioxidants Nutrition 0.000 description 10
- 241000220225 Malus Species 0.000 description 8
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- 238000007865 diluting Methods 0.000 description 8
- 235000021016 apples Nutrition 0.000 description 7
- 238000007710 freezing Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- HHEAADYXPMHMCT-UHFFFAOYSA-N dpph Chemical compound [O-][N+](=O)C1=CC([N+](=O)[O-])=CC([N+]([O-])=O)=C1[N]N(C=1C=CC=CC=1)C1=CC=CC=C1 HHEAADYXPMHMCT-UHFFFAOYSA-N 0.000 description 6
- 235000019441 ethanol Nutrition 0.000 description 6
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- 238000003860 storage Methods 0.000 description 6
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- 230000029058 respiratory gaseous exchange Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- YDQWDHRMZQUTBA-UHFFFAOYSA-N Aloe emodin Chemical class C1=CC=C2C(=O)C3=CC(CO)=CC(O)=C3C(=O)C2=C1O YDQWDHRMZQUTBA-UHFFFAOYSA-N 0.000 description 2
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical class OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
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- 238000011056 performance test Methods 0.000 description 2
- -1 polyphenol compounds Chemical class 0.000 description 2
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 description 2
- 239000012488 sample solution Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 235000013311 vegetables Nutrition 0.000 description 2
- 244000144927 Aloe barbadensis Species 0.000 description 1
- 235000002961 Aloe barbadensis Nutrition 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- 108010004032 Bromelains Proteins 0.000 description 1
- 241000222122 Candida albicans Species 0.000 description 1
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Chemical class OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 description 1
- 241000588724 Escherichia coli Species 0.000 description 1
- 238000001157 Fourier transform infrared spectrum Methods 0.000 description 1
- 241000233866 Fungi Species 0.000 description 1
- 239000004365 Protease Substances 0.000 description 1
- 230000002292 Radical scavenging effect Effects 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 241000191967 Staphylococcus aureus Species 0.000 description 1
- 229930003268 Vitamin C Chemical class 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
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- 230000032683 aging Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000000845 anti-microbial effect Effects 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 235000019835 bromelain Nutrition 0.000 description 1
- 229940095731 candida albicans Drugs 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
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- 230000008859 change Effects 0.000 description 1
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- 238000001514 detection method Methods 0.000 description 1
- 238000000113 differential scanning calorimetry Methods 0.000 description 1
- MGJZITXUQXWAKY-UHFFFAOYSA-N diphenyl-(2,4,6-trinitrophenyl)iminoazanium Chemical compound [O-][N+](=O)C1=CC([N+](=O)[O-])=CC([N+]([O-])=O)=C1N=[N+](C=1C=CC=CC=1)C1=CC=CC=C1 MGJZITXUQXWAKY-UHFFFAOYSA-N 0.000 description 1
- 230000002255 enzymatic effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
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- 150000002632 lipids Chemical class 0.000 description 1
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- 230000004060 metabolic process Effects 0.000 description 1
- 239000003094 microcapsule Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
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- 230000035699 permeability Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 230000002335 preservative effect Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
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- 229910000077 silane Inorganic materials 0.000 description 1
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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
- A23B7/16—Coating with a protective layer; Compositions or apparatus therefor
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Wood Science & Technology (AREA)
- Zoology (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Preparation Of Fruits And Vegetables (AREA)
Abstract
The invention belongs to the technical field of food processing, and relates to a quick-frozen fruit and vegetable coating liquid and a preparation method thereof. The heat treatment process changes the structure of antioxidant components in aloe and pineapple extracts, releases more free antioxidants, and remarkably improves the bioavailability and antioxidant efficacy of the aloe and pineapple extracts; bromproteinase can reduce the oxidation of polyphenol by destroying the activity of polyphenol oxidase, and the antioxidant component in aloe extract can inhibit the browning of fruit and vegetable by neutralizing the radical activated by polyphenol oxidase.
Description
Technical Field
The invention belongs to the technical field of food processing, and particularly relates to a quick-frozen fruit and vegetable film coating liquid and a preparation method thereof.
Background
Currently, common methods for extending the shelf life of vegetables include low temperature and modified atmosphere storage. The low-temperature storage can reduce the metabolism activity of vegetables by controlling the ambient temperature of a storage room, thereby achieving the purpose of keeping the characteristics of food raw materials within a certain time range. The modified atmosphere preservation technology reduces the oxygen content and increases the carbon dioxide content by adjusting the gas components in the storage environment, thereby reducing the respiration rate, the decay rate and the physiochemical change speed of fruits and vegetables and effectively prolonging the shelf life of the fruits and vegetables. Although low temperature and modified atmosphere storage techniques have achieved significant results in the preservation of fruits and vegetables, they are relatively costly and sometimes difficult to meet the preservation requirements of all fruits and vegetables.
The edible film-coating fresh-keeping technology adopts natural edible substances such as sugar, protein, lipid and other edible substances to form an edible film, and the edible film is covered on the surface or the inner surface of food in a wrapping, coating or microcapsule mode to form a protective layer. The technology is safe, environment-friendly, low in cost and simple and convenient to operate. The fresh-keeping mechanism mainly comprises the steps of reducing the contact of food and air, reducing the speed of food oxidation and enzymatic browning of fruits and vegetables, reducing the pollution of external microorganisms to the food, reducing the moisture transmission speed and inhibiting the respiration intensity of the fruits and vegetables. However, the existing edible film coating fresh-keeping technology still has certain defects, and the addition of the preservative can improve the quality but possibly cause residual problems.
Disclosure of Invention
Based on the problems, the invention aims to provide a quick-frozen film coating liquid for fruits and vegetables and a preparation method thereof.
In order to solve the problems, the technical scheme provided by the invention is as follows: a quick-frozen film coating liquid for fruits and vegetables comprises carboxymethyl chitosan, bulbus Allii water extract, modified nanocrystalline cellulose, sodium tripolyphosphate, aloe extract, pineapple extract, and sorbitol.
A preparation method of a quick-frozen film coating liquid for fruits and vegetables comprises the following steps:
s1: preparing modified nano-crystalline cellulose;
S2: heat treatment of aloe and pineapple extracts;
S3: preparing film coating liquid by ultrasonic coating;
Preferably, the garlic water extract is prepared by using deionized water as a solvent to extract active ingredients by using ultrasonic wave assisted solvent extraction method through conventional technical means and utilizing ultrasonic wave assistance.
Preferably, the preparation of the modified nanocrystalline cellulose described in step S1 comprises the steps of:
A1: adding cotton fibers into a 64wt% sulfuric acid solution, controlling the temperature to be 45 ℃, stirring at 200-300 rpm for 15min, and standing for 12h to obtain a mixed solution; adding the mixed solution into deionized water for dilution by 15 times, centrifuging at 8000rpm for 3-5 min, filtering, taking the precipitate, adding the precipitate into deionized water for dilution by 15 times, centrifuging again, filtering, taking the precipitate, repeating for three times, and then placing the precipitate into a 1-10 kDa dialysis bag for washing to obtain a washing product;
A2: adding the washing product obtained in the step A1 into a rotary evaporator, controlling the pressure to 2.5-5 Kpa, the temperature to 40-60 ℃, the rotating speed to 100-160 rpm, the temperature of a condenser to 5-10 ℃, and evaporating for 1-2 h to obtain concentrated solution; adding 0.1mol/L sodium hydroxide solution into the concentrated solution to adjust the pH to be neutral, and carrying out ultrasonic treatment at the frequency of 100Hz for 10min to obtain a nanocellulose solution;
A3: adding 3-aminopropyl triethoxysilane into deionized water, regulating the pH to 6-6.9 by using 0.2mol/L acetic acid and 0.1mol/L sodium hydroxide solution, stirring at 200-300 rpm for 10min, and standing for 3h to obtain 3-aminopropyl triethoxysilane solution; slowly adding the 3-aminopropyl triethoxysilane solution into the nano cellulose solution prepared in the step A2 within 30min, stirring at 500rpm for 6-10 h at room temperature, centrifuging at 5000rpm for 10min after the reaction is completed, filtering, washing with deionized water, and performing vacuum freeze drying at 50 ℃ for 12h to obtain the modified nano crystal cellulose.
Preferably, the ratio of the cotton fiber to the sulfuric acid solution in the step A1 is 1 g:10-30 mL.
Preferably, the concentration of the concentrated solution in the step A2 is 5-8% by weight.
Preferably, the dosage ratio of the 3-aminopropyl triethoxysilane to the deionized water in the step A3 is 1 g:20-50 mL; the volume dosage of the 3-aminopropyl triethoxysilane solution is 5-15% of that of the nano cellulose solution.
Preferably, the heat treatment of aloe and pineapple extract described in step S2 comprises the steps of:
b1: cleaning fresh aloe leaf, removing outer skin, grinding into slurry by a grinder to obtain aloe slurry; dissolving aloe pulp in ethanol solution with the concentration of 30wt%, stirring at 300rpm for 15min, and standing at room temperature for 12-24 h to obtain an extracting solution;
B2: adding the extract prepared in the step B1 into a C18 reverse phase column, performing gradient washing with 0.1wt% formic acid aqueous solution and acetonitrile at a speed of 1mL/min, gradually increasing the initial acetonitrile ratio to 90% within 30min, performing single purification for 30min, performing purification twice, mixing the two purified products, and performing vacuum freeze drying at 40 ℃ for 24h to obtain aloe extract;
B3: cutting pineapple pulp into pieces of 1cm 3, and grinding into paste to obtain pineapple paste; putting pineapple puree into a constant-temperature water bath, controlling the temperature to be 45-55 ℃, controlling the pH value of a phosphate buffer solution to be 6.5-7, and controlling the time to be 30-120 min to obtain treated pineapple puree; adding the treated pineapple puree into deionized water with the mass volume being 3 times, stirring for 2-4 hours at 200rpm, centrifuging for 10-20 minutes at 12000rpm at-4 ℃, collecting supernatant, and drying for 24 hours at 30 ℃ in vacuum to obtain pineapple extract;
B4: dissolving the aloe extract prepared in the step B2 and the pineapple extract prepared in the step B3 in deionized water with the mass volume of 2 times, mixing, putting into a water bath kettle, heating at the constant temperature of 52 ℃ for 5-15 min, immediately putting into an ice water bath after the reaction is finished, rapidly cooling to room temperature, and vacuum drying at the temperature of 30 ℃ for 24h to obtain a heat treatment product.
Preferably, the ratio of aloe vera pulp to ethanol solution in step B1 is 1 g:6-10 mL.
Preferably, the purification detection wavelength in the step B2 is 220-260 nm.
Preferably, the ultrasonic coating preparation film coating liquid in the step S3 comprises the following steps:
C1: dissolving carboxymethyl chitosan in deionized water to obtain carboxymethyl chitosan solution; slowly adding the modified nanocrystalline cellulose prepared in the step A3 into carboxymethyl chitosan solution within 5min, controlling the temperature to be 50 ℃, continuously stirring at 300rpm for 15-30 min, and then using an ultrasonic cell grinder to treat in an ice bath at-4 ℃ for 5min under the power of 450W for 5s and stopping working for 5 s; obtaining a mixed solution A;
C2: adding sodium tripolyphosphate and sorbitol into the mixed solution A prepared in the step C1, performing 450W ultrasonic auxiliary treatment for 5-15 min, adding the heat treatment product prepared in the step B4 and the garlic water extract, stirring at 200rpm for 10min, and performing 450W ultrasonic treatment for 10min after stirring to obtain a coating liquid.
Preferably, the dosage ratio of the carboxymethyl chitosan to the deionized water in the step C1 is 1 g:50-100 mL; the mass dosage ratio of the modified nano-crystalline cellulose to the carboxymethyl chitosan is 0.1-1:1.
Preferably, the mass dosage ratio of the carboxymethyl chitosan, the sodium tripolyphosphate and the sorbitol in the step C2 is 1:0.1-0.5:1-2; the mass ratio of the heat treatment product, the garlic water extract and the carboxymethyl chitosan is 0.3-0.6:0.2-0.5:1.
The beneficial effects of the invention are as follows:
The invention changes the structure of antioxidant components in aloe and pineapple extracts through a heat treatment process, releases more free antioxidant, and remarkably improves the bioavailability and antioxidant efficacy. This advancement not only effectively suppresses the activity of polyphenol oxidase and oxidation of polyphenol substances, but also enhances the thermal stability of the antioxidant components in aloe and pineapple extracts. The protective film promoting the formation of the components on the surfaces of the fruits and vegetables can be kept more stable during storage, and the duration of the browning inhibition effect is prolonged. The aloe extract is rich in aloe-emodin, vitamin C and other antioxidant compounds, and can effectively remove free radicals and relieve oxidation of polyphenol compounds. Meanwhile, bromelain and other antioxidant components in the pineapple extract and compounds in the aloe extract cooperate to enhance the antioxidant capacity together, so that the oxidation process of polyphenols is effectively slowed down, and further the browning phenomenon is effectively inhibited. Bromproteinase can reduce the oxidation of polyphenol by destroying the activity of polyphenol oxidase, and the antioxidant component in aloe extract can inhibit the browning of fruit and vegetable by neutralizing the radical activated by polyphenol oxidase. The garlic water extract has broad-spectrum antibacterial activity and can effectively inhibit the growth of various bacteria and fungi; after heat treatment, the aloe and pineapple extracts may also exhibit better antimicrobial effects due to structural changes. The synergy can provide more comprehensive protection, reduce the pollution and growth of microorganisms on the surfaces of fruits and vegetables, and prolong the fresh-keeping period of the fruits and vegetables. Sorbitol is a natural polyol compound that reduces the freezing point of moisture and reduces ice crystal formation during freezing.
The carboxymethyl chitosan is used as a water-soluble high polymer, has good film forming property, and can form a uniform and transparent protective film on the surfaces of fruits and vegetables. The protective film can effectively isolate oxygen and microorganisms in the air, slow down the respiration rate of fruits and vegetables and delay the aging and decay processes. The modified nanocrystalline cellulose is used as a nanoscale reinforcing agent and uniformly dispersed in the carboxymethyl chitosan matrix, so that the mechanical property of the coating film is greatly improved by forming a nanoscale composite material, and the integrity of the coating film at low temperature is maintained; in addition, the hydrophobicity of the nano-crystalline cellulose modified by silane can effectively block moisture penetration, and the surface of fruits and vegetables is kept dry. The composite structure of carboxymethyl chitosan and modified nanocrystalline cellulose provides good film forming property and air permeability, is favorable for maintaining the proper microenvironment of the surfaces of fruits and vegetables, and reduces the water loss and oxidative damage after thawing. The carboxymethyl chitosan, the modified nanocrystalline cellulose and the sodium tripolyphosphate are all derived from natural or biological base materials, and the prepared coating liquid is environment-friendly, has good biodegradability, is environment-friendly and is harmless to human bodies.
The invention can effectively and evenly distribute the antioxidant components in the aloe and pineapple extracts by utilizing an ultrasonic coating method, and maximize the antioxidant and anti-browning effects. All the components are from nature, and the dosage of the additive can be reduced to the maximum extent through the precise control of the ultrasonic technology, so that the environment-friendly, safe and biodegradable food-grade coating liquid is prepared.
Drawings
FIG. 1 is a graph showing the low-temperature stability test of the coating liquids prepared in examples 1 to 4 of the present invention;
FIG. 2 is a graph showing antibacterial property test of the coating liquids prepared in examples 1 to 4 of the present invention;
FIG. 3 is an FTIR infrared spectrum of the coating liquid prepared in example 1 of the present invention;
FIG. 4 is an XRD diffraction pattern of the coating liquid prepared in example 1 of the present invention;
FIG. 5 is a graph showing the cell membrane damage rate of the coating liquids prepared in examples 1 to 4 and comparative example 1 according to the present invention after application to apples;
FIG. 6 shows DPPH removal rates of coating liquids prepared in examples 1 to 4 of the present invention and comparative example 1.
Detailed Description
The technical solutions of the present invention will be clearly and completely described in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments; all other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1: a preparation method of a quick-frozen film coating liquid for fruits and vegetables comprises the following steps:
s1: preparing modified nano-crystalline cellulose;
A1: 10g of cotton fiber is added into 100mL of 64wt% sulfuric acid solution, the temperature is controlled to be 45 ℃, stirring is carried out for 15min at 200rpm, and standing is carried out for 12h, thus obtaining mixed solution; adding 100mL of the mixed solution into 1400mL of deionized water, diluting for 15 times, centrifuging for 3min at 8000rpm, filtering, collecting precipitate, adding the precipitate into deionized water, diluting for 15 times, centrifuging again, filtering, collecting precipitate, repeating for three times, and washing in a 1kDa dialysis bag to obtain a washing product;
A2: adding the washing product obtained in the step A1 into a rotary evaporator, controlling the pressure to 2.5Kpa, the temperature to 40 ℃, the rotating speed to 100rpm, the temperature of a condenser to 5 ℃, and evaporating for 1h to obtain 100mL of concentrated solution with 5% concentration; adding 0.1mol/L sodium hydroxide solution into the concentrated solution to adjust the pH to be neutral, and carrying out ultrasonic treatment at the frequency of 100Hz for 10min to obtain a nanocellulose solution;
A3: adding 1g of 3-aminopropyl triethoxysilane into 20mL of deionized water, adjusting the pH to 6 by using 0.2mol/L acetic acid and 0.1mol/L sodium hydroxide solution, stirring at 200rpm for 10min, and standing for 3h to obtain a 3-aminopropyl triethoxysilane solution; slowly adding 5mL of 3-aminopropyl triethoxysilane solution into 100mL of the nano cellulose solution prepared in the step A2 within 30min, stirring at 500rpm at room temperature for 6h, centrifuging at 5000rpm for 10min after the reaction is completed, filtering, washing with deionized water, and performing vacuum freeze-drying at 50 ℃ for 12h to obtain modified nano crystalline cellulose;
S2: heat treatment of aloe and pineapple extracts;
b1: cleaning fresh aloe leaf, removing outer skin, grinding into slurry by a grinder to obtain aloe slurry; dissolving 10g of aloe pulp in 60mL of 30wt% ethanol solution, stirring at 300rpm for 15min, and standing at room temperature for 12h to obtain an extract;
B2: adding the extract prepared in the step B1 into a C18 reverse phase column, performing gradient washing with 0.1wt% formic acid aqueous solution and acetonitrile at a speed of 1mL/min, gradually increasing the initial acetonitrile ratio to 90% within 30min, performing single purification for 30min, detecting wavelength of 220nm, performing purification twice, mixing the two purified products, and performing vacuum freeze drying at 40 ℃ for 24h to obtain aloe extract;
b3: cutting pineapple pulp into pieces of 1cm 3, and grinding into paste to obtain pineapple paste; placing 10g of pineapple puree in a constant-temperature water bath, controlling the temperature to 45 ℃, controlling the pH of a phosphate buffer solution to be 6.5, and obtaining the processed pineapple puree after 30 minutes; adding 10g of treated pineapple puree into 30mL of deionized water, stirring at 200rpm for 2 hours, centrifuging at 12000rpm for 10 minutes at-4 ℃, collecting supernatant, and drying at 30 ℃ in vacuum for 24 hours to obtain pineapple extract;
B4: 2g of aloe extract prepared in the step B2 and 2g of pineapple extract prepared in the step B3 are dissolved in 8mL of deionized water, the mixture is placed in a water bath kettle, the mixture is heated at the constant temperature of 52 ℃ for 5min, the mixture is immediately placed in an ice water bath after the reaction is completed, the mixture is rapidly cooled to the room temperature, and the mixture is dried at the temperature of 30 ℃ in vacuum for 24h to obtain a heat treatment product;
S3: preparing film coating liquid by ultrasonic coating;
C1: 1g of carboxymethyl chitosan is dissolved in 50mL of deionized water to obtain carboxymethyl chitosan solution; slowly adding 0.1g of modified nanocrystalline cellulose prepared in the step A3 into carboxymethyl chitosan solution within 5min, controlling the temperature to be 50 ℃, continuously stirring at 300rpm for 15min, stopping using an ultrasonic cell grinder under the power of 450W for 5s, working for 5s, and treating in an ice bath at-4 ℃ for 5min; obtaining a mixed solution A;
C2: and (2) adding 0.1g of sodium tripolyphosphate, 1g of sorbitol and 450W of ultrasonic-assisted treatment for 5min into the mixed solution A prepared in the step (C1), adding 0.3g of the heat treatment product prepared in the step (B4) and 0.2g of the garlic water extract, stirring at 200rpm for 10min, and carrying out ultrasonic treatment at 450W for 10min after stirring is completed to obtain a coating liquid.
Example 2: a preparation method of a quick-frozen film coating liquid for fruits and vegetables comprises the following steps:
s1: preparing modified nano-crystalline cellulose;
A1: 10g of cotton fiber is added into 200mL of 64wt% sulfuric acid solution, the temperature is controlled to be 45 ℃, stirring is carried out for 15min at 240rpm, and standing is carried out for 12h, thus obtaining mixed solution; adding 200mL of the mixed solution into 2800mL of deionized water, diluting for 15 times, centrifuging for 4min at 8000rpm, filtering, collecting precipitate, adding the precipitate into deionized water, diluting for 15 times, centrifuging again, filtering, collecting precipitate, repeating for three times, and washing in a 4kDa dialysis bag to obtain a washing product;
a2: adding the washing product obtained in the step A1 into a rotary evaporator, controlling the pressure to 3.5Kpa, the temperature to 45 ℃, the rotating speed to 120rpm, the temperature of a condenser to 7 ℃, and evaporating for 1.5 hours to obtain a concentrated solution with the concentration of 6%; adding 0.1mol/L sodium hydroxide solution into the concentrated solution, adjusting the pH to be neutral, and carrying out ultrasonic treatment at the frequency of 100Hz for 10min to obtain a nanocellulose solution;
A3: adding 1g of 3-aminopropyl triethoxysilane into 35mL of deionized water, adjusting the pH to 6.2 by using 0.2mol/L acetic acid and 0.1mol/L sodium hydroxide solution, stirring at 240rpm for 10min, and standing for 3h to obtain a 3-aminopropyl triethoxysilane solution; slowly adding 10mL of 3-aminopropyl triethoxysilane solution into 100mL of the nano cellulose solution prepared in the step A2 within 30min, stirring for 7h at 500rpm at room temperature, centrifuging at 5000rpm for 10min after the reaction is completed, filtering, washing with deionized water, and performing vacuum freeze-drying at 50 ℃ for 12h to obtain modified nano crystalline cellulose;
S2: heat treatment of aloe and pineapple extracts;
b1: cleaning fresh aloe leaf, removing outer skin, grinding into slurry by a grinder to obtain aloe slurry; dissolving 10g of aloe pulp in 80mL of 30wt% ethanol solution, stirring at 300rpm for 15min, and standing at room temperature for 16h to obtain an extract;
B2: adding the extract prepared in the step B1 into a C18 reverse phase column, performing gradient washing with 0.1wt% formic acid aqueous solution and acetonitrile at a speed of 1mL/min, gradually increasing the initial acetonitrile ratio to 90% within 30min, performing single purification for 30min, detecting wavelength of 260nm, purifying twice, mixing the two purified products, and performing vacuum freeze drying at 40 ℃ for 24h to obtain aloe extract;
B3: cutting pineapple pulp into pieces of 1cm 3, and grinding into paste to obtain pineapple paste; placing 10g of pineapple puree in a constant-temperature water bath, controlling the temperature to be 50 ℃, controlling the pH value of a phosphate buffer solution to be 6.7, and obtaining the processed pineapple puree after 60 minutes; adding 10g of treated pineapple puree into 30mL of deionized water, stirring at 200rpm for 3 hours, centrifuging at 12000rpm for 15 minutes at-4 ℃, collecting supernatant, and drying at 30 ℃ in vacuum for 24 hours to obtain pineapple extract;
B4: 2g of aloe extract prepared in the step B2 and 2g of pineapple extract prepared in the step B3 are dissolved in 8mL of deionized water, the mixture is placed in a water bath kettle, the mixture is heated at the constant temperature of 52 ℃ for 9min, the mixture is immediately placed in an ice water bath after the reaction is completed, the mixture is rapidly cooled to the room temperature, and the mixture is dried at the temperature of 30 ℃ in vacuum for 24h to obtain a heat treatment product;
S3: preparing film coating liquid by ultrasonic coating;
C1: 1g of carboxymethyl chitosan is dissolved in 75mL of deionized water to obtain carboxymethyl chitosan solution; slowly adding 0.5g of modified nanocrystalline cellulose prepared in the step A3 into carboxymethyl chitosan solution within 5min, controlling the temperature to be 50 ℃, continuously stirring at 300rpm for 20min, stopping using an ultrasonic cell grinder under the power of 450W for 5s, working for 5s, and treating in an ice bath at-4 ℃ for 5min; obtaining a mixed solution A;
C2: and (2) adding 0.3g of sodium tripolyphosphate, 1.5g of sorbitol and 450W of ultrasonic auxiliary treatment for 9min into the mixed solution A prepared in the step (C1), adding 0.4g of heat treatment product and 0.3g of garlic water extract prepared in the step (B4), stirring at 200rpm for 10min, and carrying out ultrasonic treatment at 450W for 10min after stirring is completed to obtain a coating liquid.
Example 3: a preparation method of a quick-frozen film coating liquid for fruits and vegetables comprises the following steps:
s1: preparing modified nano-crystalline cellulose;
A1: 10g of cotton fiber is added into 250mL of 64wt% sulfuric acid solution, the temperature is controlled to be 45 ℃, and the stirring is carried out at 280rpm for 15min, and the mixture is kept stand for 12h to obtain a mixed solution; adding 250mL of the mixed solution into 3500mL of deionized water, diluting for 15 times, centrifuging for 5min at 8000rpm, filtering, collecting precipitate, adding the precipitate into deionized water, diluting for 15 times, centrifuging again, filtering, collecting precipitate, repeating for three times, and placing into an 8kDa dialysis bag for washing to obtain a washing product;
A2: adding the washing product obtained in the step A1 into a rotary evaporator, controlling the pressure to 4Kpa, the temperature to 55 ℃, the rotating speed to 150rpm, the condenser temperature to 8 ℃, and evaporating for 2 hours to obtain a concentrated solution with the concentration of 7%; adding 0.1mol/L sodium hydroxide solution into the concentrated solution, adjusting the pH to be neutral, and carrying out ultrasonic treatment at the frequency of 100Hz for 10min to obtain a nanocellulose solution;
a3: adding 1g of 3-aminopropyl triethoxysilane into 40mL of deionized water, adjusting the pH to 6.8 by using 0.2mol/L acetic acid and 0.1mol/L sodium hydroxide solution, stirring at 280rpm for 10min, and standing for 3h to obtain a 3-aminopropyl triethoxysilane solution; slowly adding 12mL of 3-aminopropyl triethoxysilane solution into 100mL of the nano cellulose solution prepared in the step A2 within 30min, stirring for 9h at 500rpm at room temperature, centrifuging at 5000rpm for 10min after the reaction is completed, filtering, washing with deionized water, and performing vacuum freeze-drying at 50 ℃ for 12h to obtain modified nano crystalline cellulose;
S2: heat treatment of aloe and pineapple extracts;
B1: cleaning fresh aloe leaf, removing outer skin, grinding into slurry by a grinder to obtain aloe slurry; dissolving 10g of aloe pulp in 90mL of 30wt% ethanol solution, stirring at 300rpm for 15min, and standing at room temperature for 20h to obtain an extract;
B2: adding the extract prepared in the step B1 into a C18 reverse phase column, performing gradient washing with 0.1wt% formic acid aqueous solution and acetonitrile at a speed of 1mL/min, gradually increasing the initial acetonitrile ratio to 90% within 30min, performing single purification for 30min, detecting wavelength of 240nm, performing purification twice, mixing the two purified products, and performing vacuum freeze drying at 40 ℃ for 24h to obtain aloe extract;
B3: cutting pineapple pulp into pieces of 1cm 3, and grinding into paste to obtain pineapple paste; 10g of pineapple puree is placed in a constant-temperature water bath, the temperature is controlled to be 52 ℃, the pH value of a phosphate buffer solution is controlled to be 6.9, and the time is 100min, so that the processed pineapple puree is obtained; adding 10g of treated pineapple puree into 30mL of deionized water, stirring at 200rpm for 3.5h, centrifuging at 12000rpm for 18min at-4 ℃, collecting supernatant, and vacuum drying at 30 ℃ for 24h to obtain pineapple extract;
b4: 2g of aloe extract prepared in the step B2 and 2g of pineapple extract prepared in the step B3 are dissolved in 8mL of deionized water, the mixture is placed into a water bath kettle, the mixture is heated at the constant temperature of 52 ℃ for 13min, the mixture is immediately placed into an ice water bath after the reaction is completed, the mixture is rapidly cooled to the room temperature, and the mixture is dried at the temperature of 30 ℃ in vacuum for 24h to obtain a heat treatment product;
S3: preparing film coating liquid by ultrasonic coating;
c1: 1g of carboxymethyl chitosan is dissolved in 80mL of deionized water to obtain carboxymethyl chitosan solution; slowly adding 0.8g of modified nanocrystalline cellulose prepared in the step A3 into carboxymethyl chitosan solution within 5min, controlling the temperature to be 50 ℃, continuously stirring at 300rpm for 25min, stopping using an ultrasonic cell grinder under the power of 450W for 5s, working for 5s, and treating in an ice bath at-4 ℃ for 5min; obtaining a mixed solution A;
C2: and (2) adding 0.4g of sodium tripolyphosphate, 1.8g of sorbitol and 450W of ultrasonic auxiliary treatment for 13min into the mixed solution A prepared in the step (C1), adding 0.5g of heat treatment product and 0.4g of garlic water extract prepared in the step (B4), stirring at 200rpm for 10min, and carrying out 450W ultrasonic treatment for 10min after stirring is completed to obtain a coating liquid.
Example 4: a preparation method of a quick-frozen film coating liquid for fruits and vegetables comprises the following steps:
s1: preparing modified nano-crystalline cellulose;
A1: adding 10g of cotton fiber into 300mL of 64wt% sulfuric acid solution, controlling the temperature to be 45 ℃, stirring at 300rpm for 15min, and standing for 12h to obtain a mixed solution; adding 300mL of the mixed solution into 4200mL of deionized water, diluting for 15 times, centrifuging for 5min at 8000rpm, filtering, collecting precipitate, adding the precipitate into deionized water, diluting for 15 times, centrifuging again, filtering, collecting precipitate, repeating for three times, and washing in a 10kDa dialysis bag to obtain a washing product;
A2: adding the washing product obtained in the step A1 into a rotary evaporator, controlling the pressure to 5Kpa, the temperature to 60 ℃, the rotating speed to 160rpm, the temperature of a condenser to 10 ℃, and evaporating for 2 hours to obtain concentrated solution with the concentration of 8%; adding 0.1mol/L sodium hydroxide solution into the concentrated solution, adjusting the pH to be neutral, and carrying out ultrasonic treatment at the frequency of 100Hz for 10min to obtain a nanocellulose solution;
A3: adding 2g of 3-aminopropyl triethoxysilane into 100mL of deionized water, adjusting the pH to 6.9 by using 0.2mol/L acetic acid and 0.1mol/L sodium hydroxide solution, stirring at 300rpm for 10min, and standing for 3h to obtain a 3-aminopropyl triethoxysilane solution; slowly adding 15mL of 3-aminopropyl triethoxysilane solution into 100mL of the nano cellulose solution prepared in the step A2 within 30min, stirring at 500rpm at room temperature for 10h, centrifuging at 5000rpm for 10min after the reaction is completed, filtering, washing with deionized water, and performing vacuum freeze-drying at 50 ℃ for 12h to obtain modified nano crystalline cellulose;
S2: heat treatment of aloe and pineapple extracts;
B1: cleaning fresh aloe leaf, removing outer skin, grinding into slurry by a grinder to obtain aloe slurry; dissolving 10g of aloe pulp in 100mL of 30wt% ethanol solution, stirring at 300rpm for 15min, and standing at room temperature for 24h to obtain an extract;
B2: adding the extract prepared in the step B1 into a C18 reverse phase column, performing gradient washing with 0.1wt% formic acid aqueous solution and acetonitrile at a speed of 1mL/min, gradually increasing the initial acetonitrile ratio to 90% within 30min, performing single purification for 30min, detecting wavelength of 260nm, purifying twice, mixing the two purified products, and performing vacuum freeze drying at 40 ℃ for 24h to obtain aloe extract;
B3: cutting pineapple pulp into pieces of 1cm 3, and grinding into paste to obtain pineapple paste; placing 10g of pineapple puree in a constant-temperature water bath, controlling the temperature to 55 ℃, controlling the pH value of a phosphate buffer solution to 7, and obtaining the processed pineapple puree for 120 min; adding 10g of treated pineapple puree into 30mL of deionized water, stirring at 200rpm for 4 hours, centrifuging at 12000rpm for 20 minutes at-4 ℃, collecting supernatant, and drying at 30 ℃ in vacuum for 24 hours to obtain pineapple extract;
b4: 2g of aloe extract prepared in the step B2 and 2g of pineapple extract prepared in the step B3 are dissolved in 8mL of deionized water, the mixture is placed in a water bath kettle, the mixture is heated at the constant temperature of 52 ℃ for 15min, the mixture is immediately placed in an ice water bath after the reaction is completed, the mixture is rapidly cooled to the room temperature, and the mixture is dried at the temperature of 30 ℃ in vacuum for 24h to obtain a heat treatment product;
S3: preparing film coating liquid by ultrasonic coating;
C1: 1g of carboxymethyl chitosan is dissolved in 100mL of deionized water to obtain carboxymethyl chitosan solution; slowly adding 1g of modified nanocrystalline cellulose prepared in the step A3 into carboxymethyl chitosan solution within 5min, controlling the temperature to be 50 ℃, continuously stirring at 300rpm for 30min, and then using an ultrasonic cell grinder to treat in an ice bath at-4 ℃ for 5min under the power of 450W for 5s after stopping working for 5 s; obtaining a mixed solution A;
C2: and (2) adding 0.5g of sodium tripolyphosphate, 2g of sorbitol and 450W of ultrasonic auxiliary treatment for 15min into the mixed solution A prepared in the step (C1), adding 0.6g of heat treatment product and 0.5g of garlic water extract prepared in the step (B4), stirring at 200rpm for 10min, and carrying out ultrasonic treatment at 450W for 10min after stirring is completed to obtain a coating liquid.
Comparative example 1: the same as in example 3, except that comparative example 1 was not added with pineapple extract.
Performance test: adding the coating liquid prepared in the examples 1-4 into deionized water for dilution by 10 times, cutting apples into pieces with the size of 1cm 3, adding the pieces into the diluted coating liquid, soaking for 2min, quick-freezing at the temperature of minus 35 ℃ for 2h, then transferring the pieces into the temperature of minus 20 ℃ for freezing for 7 days, and taking out the pieces after the freezing is finished for measuring the water loss rate: water loss = (initial weight before freezing-weight after freezing end)/initial weight before freezing; a control group was set, wherein the control group was different in that no coating liquid was used, and the test was repeated 3 times by immersing in the same volume of deionized water for 2 minutes, and the test results were as follows:
Table 1. Apple loss test results.
Low temperature performance test: the film coating liquid samples prepared in examples 1 to 4 of the present invention were respectively placed in DSC analysis sample trays for testing, the test temperature was set at-40 to 25 ℃, the heating rate was 5 ℃/min, the curve shift temperature in the low temperature region was recorded, three samples were taken for each example, and the average value was taken, and the results are shown in FIG. 1.
And (3) bacteriostasis rate test: fresh bacterial solutions of staphylococcus aureus, escherichia coli and candida albicans are prepared, the bacterial solution concentration is 1 multiplied by 10 8 CFU/mL, film coating liquid samples prepared in examples 1-4 of the invention are respectively added, the mixed bacterial solution is placed in a constant-temperature oscillator at 37 ℃ for culture for 24 hours, the total number of bacterial colonies of the bacterial solutions is recorded by adopting a plate colony counting method, the test is repeated for 3 times, the average value is taken, the bacterial solution without the samples is used as a control (all strains used in the test are purchased from the market), and the bacteriostasis rate (the bacteriostasis rate= (the bacterial number of 1-control sample/the bacterial number of experimental sample) ×100%) is calculated, and the test result is shown in fig. 2.
And (3) map measurement: coating a film coating liquid sample prepared in the embodiment 1 of the invention on a potassium bromide substrate, and measuring a spectrogram by using an FTIR spectrometer; coating liquid samples prepared in example 1 were coated on a monocrystalline silicon substrate, and diffraction patterns of the samples were measured by an X-ray diffractometer; the FTIR spectrum is shown in FIG. 3, and the XRD diffraction pattern is shown in FIG. 4.
Cell membrane damage rate test: 18 apples of similar size and maturity are selected and randomly divided into 6 groups, 1 to 4 groups of apples are treated by the coating liquid prepared in examples 1 to 4, and 5 groups of apples are treated by the coating liquid prepared in comparative example 1; group 6 was a control group, after the film coating liquid was naturally dried, all apples were refrigerated at 4 ℃ for 2 weeks, 1g of pulp was removed from each group of apples by the same weight, and after grinding, cell suspensions were prepared, and cell membrane damage rates (damage rate= (LDH release amount of treatment group/LDH release amount of control group) ×100%) were measured and calculated according to the instructions using LDH release kit, the test was repeated 3 times, and the average was taken, and the test results are shown in fig. 5.
DPPH clearance test: taking 2mLDPPH solution and 2mL of sample solution to be detected (respectively taking 0.1mL of coating solution prepared in examples 1-4 and coating solution prepared in comparative example 1 and dissolving in 5mL of absolute ethyl alcohol), uniformly mixing, placing for 30min in a dark place, taking absolute ethyl alcohol solution as a reference, and measuring absorbance value at 517nm, wherein DPPH solution is solution with concentration of 0.1mM prepared by taking absolute ethyl alcohol as solvent. The DPPH radical scavenging rate (scavenging rate= [1- (absorbance of sample and DPPH mixture-absorbance of sample solution without DPPH/absorbance of DPPH solution only ] ×100%) was calculated, and the test was repeated 3 times, and the result was averaged, as shown in fig. 6.
The results of fig. 1 show that the coating liquid prepared by the invention can have excellent stability at extremely low temperature, the results of fig. 2 show that the coating liquid prepared by the invention meets the safety standard and has extremely strong antibacterial property, and the results of fig. 3 and 4 show that the coating liquid prepared by the invention is safe and stable; as can be seen from the results of fig. 5 and table 1, the coating liquid prepared by the invention has extremely strong protective effect, remarkable antioxidation effect, effective fresh-keeping and stable at extremely low temperature; from the results shown in fig. 5 and 6, it is apparent that pineapple and aloe extracts significantly exert a synergistic effect in the coating liquid prepared by the present invention.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (6)
1. A preparation method of a quick-frozen film coating liquid for fruits and vegetables is characterized in that the quick-frozen film coating liquid for fruits and vegetables consists of carboxymethyl chitosan, garlic water extract, modified nanocrystalline cellulose, sodium tripolyphosphate, aloe extract, pineapple extract and sorbitol;
The preparation method of the quick-frozen film coating liquid for fruits and vegetables comprises the following steps:
s1: preparing modified nano-crystalline cellulose;
S2: heat treatment of aloe and pineapple extracts;
S3: preparing film coating liquid by ultrasonic coating;
the preparation of the modified nanocrystalline cellulose described in step S1 includes the steps of:
A1: adding cotton fibers into a 64wt% sulfuric acid solution, controlling the temperature to be 45 ℃, stirring at 200-300 rpm for 15min, and standing for 12h to obtain a mixed solution; adding the mixed solution into deionized water for dilution by 15 times, centrifuging at 8000rpm for 3-5 min, filtering, taking the precipitate, adding the precipitate into deionized water for dilution by 15 times, centrifuging again, filtering, taking the precipitate, repeating for three times, and then placing the precipitate into a 1-10 kDa dialysis bag for washing to obtain a washing product;
A2: adding the washing product obtained in the step A1 into a rotary evaporator, controlling the pressure to 2.5-5 Kpa, the temperature to 40-60 ℃, the rotating speed to 100-160 rpm, the temperature of a condenser to 5-10 ℃, and evaporating for 1-2 h to obtain concentrated solution; adding 0.1mol/L sodium hydroxide solution into the concentrated solution to adjust the pH to be neutral, and carrying out ultrasonic treatment at the frequency of 100Hz for 10min to obtain a nanocellulose solution;
A3: adding 3-aminopropyl triethoxysilane into deionized water, regulating the pH to 6-6.9 by acetic acid and sodium hydroxide solution, stirring at 200-300 rpm for 10min, and standing for 3h to obtain 3-aminopropyl triethoxysilane solution; slowly adding the 3-aminopropyl triethoxysilane solution into the nano cellulose solution prepared in the step A2 within 30min, stirring at 500rpm for 6-10 h at room temperature, centrifuging at 5000rpm for 10min after the reaction is completed, filtering, washing with deionized water, and performing vacuum freeze drying at 50 ℃ for 12h to obtain the modified nano crystal cellulose.
2. The preparation method of the quick-frozen film coating liquid for fruits and vegetables according to claim 1, wherein the dosage ratio of the cotton fiber to the sulfuric acid solution in the step A1 is 1 g:10-30 mL; the concentration of the concentrated solution in the step A2 is 5-8% by weight; the dosage ratio of the 3-aminopropyl triethoxysilane to the deionized water in the step A3 is 1 g:20-50 mL; the volume dosage of the 3-aminopropyl triethoxysilane solution is 5-15% of that of the nano cellulose solution.
3. The method for preparing the quick-frozen fruit and vegetable coating liquid according to claim 2, wherein the heat treatment of aloe and pineapple extract in the step S2 comprises the following steps:
b1: cleaning fresh aloe leaf, removing outer skin, grinding into slurry by a grinder to obtain aloe slurry; dissolving aloe pulp in ethanol solution with the concentration of 30wt%, stirring at 300rpm for 15min, and standing at room temperature for 12-24 h to obtain an extracting solution;
B2: adding the extract prepared in the step B1 into a C18 reverse phase column, performing gradient washing with 0.1wt% formic acid aqueous solution and acetonitrile at a speed of 1mL/min, gradually increasing the initial acetonitrile ratio to 90% within 30min, performing single purification for 30min, performing purification twice, mixing the two purified products, and performing vacuum freeze drying at 40 ℃ for 24h to obtain aloe extract;
B3: cutting pineapple pulp into pieces of 1cm 3, and grinding into paste to obtain pineapple paste; putting pineapple puree into a constant-temperature water bath, controlling the temperature to be 45-55 ℃, controlling the pH value of a phosphate buffer solution to be 6.5-7, and controlling the time to be 30-120 min to obtain treated pineapple puree; adding the treated pineapple puree into deionized water with the mass volume being 3 times, stirring for 2-4 hours at 200rpm, centrifuging for 10-20 minutes at 12000rpm at-4 ℃, collecting supernatant, and drying for 24 hours at 30 ℃ in vacuum to obtain pineapple extract;
B4: dissolving the aloe extract prepared in the step B2 and the pineapple extract prepared in the step B3 in deionized water with the mass volume of 2 times, mixing, putting into a water bath kettle, heating at the constant temperature of 52 ℃ for 5-15 min, immediately putting into an ice water bath after the reaction is finished, rapidly cooling to room temperature, and vacuum drying at the temperature of 30 ℃ for 24h to obtain a heat treatment product.
4. The method for preparing a quick-frozen film coating liquid for fruits and vegetables according to claim 3, wherein the dosage ratio of aloe pulp to ethanol solution in the step B1 is 1 g:6-10 mL.
5. The method for preparing the quick-frozen film coating liquid for fruits and vegetables according to claim 4, wherein the ultrasonic coating preparation film coating liquid in the step S3 comprises the following steps:
C1: dissolving carboxymethyl chitosan in deionized water to obtain carboxymethyl chitosan solution; slowly adding the modified nanocrystalline cellulose prepared in the step A3 into carboxymethyl chitosan solution within 5min, controlling the temperature to be 50 ℃, continuously stirring at 300rpm for 15-30 min, and then using an ultrasonic cell grinder to treat in an ice bath at-4 ℃ for 5min under the power of 450W for 5s and stopping working for 5 s; obtaining a mixed solution A;
C2: adding sodium tripolyphosphate and sorbitol into the mixed solution A prepared in the step C1, performing 450W ultrasonic auxiliary treatment for 5-15 min, adding the heat treatment product prepared in the step B4 and the garlic water extract, stirring at 200rpm for 10min, and performing 450W ultrasonic treatment for 10min after stirring to obtain a coating liquid.
6. The preparation method of the quick-frozen fruit and vegetable film coating liquid according to claim 5, which is characterized in that the dosage ratio of the carboxymethyl chitosan to the deionized water in the step C1 is 1 g:50-100 mL; the mass dosage ratio of the modified nano-crystalline cellulose to the carboxymethyl chitosan is 0.1-1:1; the mass dosage ratio of the carboxymethyl chitosan, the sodium tripolyphosphate and the sorbitol in the step C2 is 1:0.1-0.5:1-2; the mass ratio of the heat treatment product, the garlic water extract and the carboxymethyl chitosan is 0.3-0.6:0.2-0.5:1.
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Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102715233A (en) * | 2012-06-28 | 2012-10-10 | 华侨大学 | Carboxymethyl chitosan nano biological preservative and preparation method thereof |
| US20160002483A1 (en) * | 2013-03-14 | 2016-01-07 | Oregon State University | Nano-cellulose edible coatings and uses thereof |
| CN105949517A (en) * | 2016-07-04 | 2016-09-21 | 铜陵方正塑业科技有限公司 | Aloe vera gel-modified gamma-polyglutamic acid grafted pineapple leaf fiber packaging film and preparation method thereof |
| CN108056350A (en) * | 2018-01-11 | 2018-05-22 | 广东日可威富硒食品有限公司 | A kind of sports drink of the polysaccharide containing pineapple bran |
| CN112772714A (en) * | 2020-12-30 | 2021-05-11 | 上海交通大学 | Composite preservative film and preparation method and application thereof |
| KR102437635B1 (en) * | 2022-03-07 | 2022-08-29 | 윤여홍 | The method of manufacture of beef bulgogi sauce |
| WO2022223567A1 (en) * | 2021-04-21 | 2022-10-27 | Empa Eidgenössische Materialprüfungs- Und Forschungsanstalt | Sustainable food packaging |
| CN116602338A (en) * | 2023-05-17 | 2023-08-18 | 广西壮族自治区农业科学院 | Fresh-keeping method for effectively controlling browning of persimmon |
| CN116715884A (en) * | 2023-06-07 | 2023-09-08 | 广西科技师范学院 | Preparation method of modified cellulose nanocrystalline-chitosan-plant essential oil composite membrane |
| CN117378669A (en) * | 2023-11-10 | 2024-01-12 | 西安文理学院 | Fruit preservative and preparation method and application thereof |
-
2024
- 2024-04-08 CN CN202410413896.XA patent/CN118000250B/en active Active
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102715233A (en) * | 2012-06-28 | 2012-10-10 | 华侨大学 | Carboxymethyl chitosan nano biological preservative and preparation method thereof |
| US20160002483A1 (en) * | 2013-03-14 | 2016-01-07 | Oregon State University | Nano-cellulose edible coatings and uses thereof |
| CN105949517A (en) * | 2016-07-04 | 2016-09-21 | 铜陵方正塑业科技有限公司 | Aloe vera gel-modified gamma-polyglutamic acid grafted pineapple leaf fiber packaging film and preparation method thereof |
| CN108056350A (en) * | 2018-01-11 | 2018-05-22 | 广东日可威富硒食品有限公司 | A kind of sports drink of the polysaccharide containing pineapple bran |
| CN112772714A (en) * | 2020-12-30 | 2021-05-11 | 上海交通大学 | Composite preservative film and preparation method and application thereof |
| WO2022223567A1 (en) * | 2021-04-21 | 2022-10-27 | Empa Eidgenössische Materialprüfungs- Und Forschungsanstalt | Sustainable food packaging |
| KR102437635B1 (en) * | 2022-03-07 | 2022-08-29 | 윤여홍 | The method of manufacture of beef bulgogi sauce |
| CN116602338A (en) * | 2023-05-17 | 2023-08-18 | 广西壮族自治区农业科学院 | Fresh-keeping method for effectively controlling browning of persimmon |
| CN116715884A (en) * | 2023-06-07 | 2023-09-08 | 广西科技师范学院 | Preparation method of modified cellulose nanocrystalline-chitosan-plant essential oil composite membrane |
| CN117378669A (en) * | 2023-11-10 | 2024-01-12 | 西安文理学院 | Fruit preservative and preparation method and application thereof |
Non-Patent Citations (9)
| Title |
|---|
| MITHILESH YADAV ET AL: "Cellulose Nanocrystal Reinforced Chitosan Based UV Barrier Composite Films for Sustainable Packaging", 《POLYMERS》, vol. 12, no. 1, 13 January 2020 (2020-01-13), pages 1 - 22 * |
| YUZHEN DU ET AL: "Chitosan/cellulose nanocrystal biocomposite coating for fruit postharvest preservation", 《INDUSTRIAL CROPS & PRODUCTS》, vol. 205, no. 2023, 22 September 2023 (2023-09-22), pages 1 - 10, XP087427911, DOI: 10.1016/j.indcrop.2023.117543 * |
| 刘建勋等: "《中药药理学》", 31 January 2020, 中国协和医科大学出版社, pages: 131 - 134 * |
| 彭燕等: "两种环氧基硅烷偶联剂改性纤维素纳米晶体的制备及性能", 《塑料工业》, vol. 50, no. 4, 18 May 2022 (2022-05-18), pages 47 - 52 * |
| 朱顺顺等: "纤维素纳米晶制备方法及应用研究进展", 《核农学报》, vol. 36, no. 1, 31 December 2022 (2022-12-31), pages 174 - 182 * |
| 李世文等: "《一味中药祛顽疾 第7版》", 30 April 2023, 河南科学技术出版社, pages: 22 * |
| 李冈荣等: "《汉方中草药对症图典 第4册》", 30 September 2015, 新疆科技卫生出版社, pages: 134 - 135 * |
| 梁小彩等: "速冻苹果块可食性涂膜技术研究", 《安徽农业科学》, vol. 40, no. 22, 29 October 2012 (2012-10-29), pages 11411 - 11413 * |
| 董泽义等: "壳聚糖保鲜膜研究进展", 《食品与发酵工业》, vol. 40, no. 6, 31 December 2014 (2014-12-31), pages 147 - 151 * |
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