CN105285077A - Composite coating film fresh keeping agent containing persimmon leaf flavones as well as preparation method and application of composite coating film fresh keeping agent - Google Patents

Composite coating film fresh keeping agent containing persimmon leaf flavones as well as preparation method and application of composite coating film fresh keeping agent Download PDF

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Publication number
CN105285077A
CN105285077A CN201510580604.2A CN201510580604A CN105285077A CN 105285077 A CN105285077 A CN 105285077A CN 201510580604 A CN201510580604 A CN 201510580604A CN 105285077 A CN105285077 A CN 105285077A
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persimmon leaf
parts
fresh keeping
keeping agent
composite
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李文香
樊铭聪
吴昊
王世清
张鑫
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Qingdao Agricultural University
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Qingdao Agricultural University
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A40/00Adaptation technologies in agriculture, forestry, livestock or agroalimentary production
    • Y02A40/90Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in food processing or handling, e.g. food conservation

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  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

The invention relates to a composite coating film fresh keeping agent containing persimmon leaf flavones and having characteristics of oxidation resistance and bacteriostasis, as well as a preparation method and application of the composite coating film fresh keeping agent, and belongs to the technical field of fresh keeping of fresh agricultural products. The composite fresh keeping agent consists of the following raw materials in parts by weight: 0.5-1.5 parts of persimmon leaf flavones, 10-30 parts of carboxymethyl chitosan, 30-40 parts of glycerine, 5-10 parts of calcium chloride, 10-20 parts of polyethylene glycol, 0.3-0.5 part of tween 20 and 1000 parts of water. According to the composite fresh keeping agent provided by the invention, all the components have a synergistic reaction, so that the hygroscopicity and the homogeneity of composite coating film fresh keeping agent are improved, the filming integrity is strengthened, and after being air-dried, coating films are not cracked, so that the coating films not only have favorable properties of resisting air and resisting dampness but also have excellent antioxidative and antibacterial effects and obvious fresh keeping effects; all the components of the composite fresh keeping agent disclosed by the invention are environmental-friendly, good in water solubility, easy to clean and free from toxic and side residues, so that the composite fresh keeping agent has broad market prospects.

Description

A kind of composite coating preservative containing persimmon leaf flavone and preparation method thereof and application
Technical field
The present invention relates to a kind of composite preservative, be specifically related to a kind ofly containing persimmon leaf flavone, there is composite coating preservative of anti-oxidant, antagonistic property and preparation method thereof and application, belong to fresh agricultural products technical field of preservation of fresh.
Background technology
Persimmon leaf is the leaf of calamander persimmon (DiospyroskakiThunb.), and China produces the maximum country of persimmon in the world, and often produce fresh persimmon more than 70 ten thousand tons per year, persimmon leaf is the accessory substance of persimmon industry.Therefore, there is abundant persimmon leaf resource in China.Persimmon leaf has the multiple effects such as clearing heat and detoxicating, moistening lung cardiac stimulant, antibechic hemostasis, anti-cancer and cancer-preventing, is just day by day subject to people's attention in recent years.Main composition-the flavone compound of persimmon leaf, has the multiple physiologically actives such as anticancer, anti-oxidant, antibacterial.Along with the continuous excavation to persimmon leaf value, market has constantly occurred the processed goods of persimmon leaf, as persimmon leaf tea, persimmon leaf milk tea, persimmon leaf beverage etc., but there is not been reported about the application of persimmon leaf flavone in the agricultural product post-harvest fresh-keepings such as fresh fruit, dish, bacterium.Therefore persimmon leaf is developed and utilized, therefrom extract natural anti-oxidation, bacteriostasis efficacy composition is applied to the fresh-keeping of the fresh agricultural products such as fruit, dish, bacterium, not only open the new way of persimmon leaf efficiency utilization, simultaneously also for fresh agricultural products wide spectrum, exploitation that is efficient, multifunctional natural antistaling agent provide new approaches, safe, the green preservation realizing the fresh agricultural products such as fruit, dish, bacterium is had important practical significance.
Current existing fresh agricultural products preservation technique many employings fresh chemically, coating-film fresh-keeping are more common in wax liquid film, though these fresh-keeping measures can at the fresh-keeping effect to a certain degree improving fresh agricultural products, but the residual quantity of chemical preservative is larger, long-term absorption easily causes " three cause ", i.e. carcinogenic, teratogenesis, mutagenesis, its security is subject to the generally query of people; And most wax liquid film also can only play certain choke, the wet effect of resistance.Along with consumer's craving for green, organic food, really, dish, the fresh agricultural products such as bacterium fresh-keeping, be badly in need of finding a kind of green, that crude antistaling agent that is efficient, broad-spectrum antibacterial carrys out substituted chemistry be fresh-keeping.Therefore, the present invention is by will the flavones that extract from persimmon leaf and water-soluble good CMC compound, develop and a kind ofly novel there is the antibacterial and multifunctional natural composite coating preservative had no side effect of antioxidation activity, high-efficiency broad spectrum, will have broad application prospects.
Summary of the invention
, its security comparatively large for fresh agricultural products employing fresh chemically residual quantities such as existing fruit, dish, bacterium is subject to consumer and queries; And coating antistaling agent generally only has certain choke, the wet effect of resistance, lack the realistic problem of the multifunctional comprehensive fresh-keeping effects such as anti-oxidant and suppression microbial activities, the invention provides a kind of composite preservative containing persimmon leaf flavone and preparation method thereof and application
Present invention also offers a kind of preparation method and application of the composite preservative containing persimmon leaf flavone, by improving flavones dissolution process, improving flavones meltage, strengthening its antioxidation activity and bactericidal effect.
The technical scheme that the present invention is adopted to achieve these goals is:
The invention provides a kind of composite preservative containing persimmon leaf flavone, be made up of following raw material:
Persimmon leaf flavone 0.5-1.5 part, CMC 10-30 part, glycerine 30-40 part, calcium chloride 5-10 part, polyethylene glycol 10-20 part, polysorbas20 0.3-0.5 part, 1000 parts, water.
Further, the molecular weight of described polyethylene glycol optimization is 200-600.
Further, the extraction of described persimmon leaf flavone adopts following methods to obtain:
(1) by the powder of persimmon leaf with 45vol% ethanolic solution according to solid-liquid ratio 1:35(g/mL) mix, then add acetic acid adjust ph, add in supersonic extractors after stirring, be warming up to 50 DEG C with the heating rate of 3-5 DEG C/min, under power is 500W condition, re-extract three times;
(2) merge extract and filter, filtrate to during close to Transparent color, removes ethyl acetate layer with separatory funnel through extraction into ethyl acetate, then after concentrating in a rotary evaporator, freeze drying, obtains persimmon leaf flavone.
Further, in step (1), described in add acetic acid adjust ph be 4-5.
Further, the time of described extraction is 20min.
Present invention also offers a kind of preparation method of composite preservative, comprise the following steps:
(1) weight portion CMC, calcium chloride, polyethylene glycol, polysorbas20 are mixed with water, ultrasonic wave added dissolves, and stirs, obtains CMC base fluid;
(2) parts by weight of glycerin is mixed with persimmon leaf flavone, after stirring, obtain flavones-glycerine mixed liquor;
(3) flavones-glycerine mixed liquor is mixed with CMC base fluid, stir, obtain compositional liquor;
(4) compositional liquor is carried out bubble-free in vacuum outgas to compositional liquor under vacuum conditions.
In addition, present invention also offers the application of composite preservative in fresh agricultural products is fresh-keeping.
The using method of composite preservative provided by the invention is: select fresh, without the fresh agricultural products such as fruit, dish, bacterium that rots, have no mechanical damage, after cleaning up by the clean tap water of flowing, naturally dry, then infusion method or spray-on process is adopted to make to be coated with the prefabricated persimmon leaf flavone-CMC composite preservative of last layer at raw material surface uniform, carry out after natural air drying packing, storing and transporting, good fresh-keeping effect can be played.
In the process that the present invention extracts at persimmon leaf flavone, by changing Alcohol system pH, farthest can keep the stability extracting flavones in solution, reducing the destruction of other extraction conditions to active ingredient; Meanwhile, change solution system pH value, also can reduce the solubility of impurity component in ethanolic solution, thus improve object---the recovery rate of persimmon leaf flavone and purity.The composite coating preservative of the present invention's exploitation, in compound process, first carries out premixed by raw material, can improve the meltage of persimmon leaf flavone in CMC base fluid; The collaborative anti-oxidant and bacteriostatic activity of this composite preservative is significantly improved by the compound of the two.
Beneficial effect of the present invention is:
(1) recovery rate of persimmon leaf flavone and purity high; Persimmon leaf flavone and CMC compound, it is anti-oxidant, bacteriostatic activity significantly improves, and natural, the nontoxic pair of this multiple antistaling agent remains;
(2) by optimizing flavones dissolution process, improving flavones content in antistaling agent, enhancing anti-oxidant, the antibacterial activity of composite preservative;
(3) each component synergy of composite preservative provided by the invention, by adding the coalescents such as calcium chloride, polyethylene glycol, Tween-20 in right amount, improve hygroscopicity, the homogeneity of composite preservative film, strengthen the integrality of film forming, make air-dry after do not ftracture, not only have good choke, moisture barrier property, have excellent anti-oxidant, antibacterial, fungistatic effect, fresh-keeping effect is obvious simultaneously; The each component environmental protection of the present invention, good water solubility, easy cleaning, nontoxic pair remains, and has wide market prospects.
Detailed description of the invention
Below by embodiment, the present invention will be further elaborated, it is to be understood that following explanation is only to explain the present invention, do not limit its content.
Ethanolic solution used in the present invention is the aqueous solution of ethanol.
embodiment 1
An extraction for persimmon leaf flavone, is characterized in that, adopts following methods to extract:
(1) powder of persimmon leaf is mixed according to solid-liquid ratio 1g:35mL with 45vol% ethanolic solution, then add acetic acid and regulate pH value to 4, add after stirring in supersonic extractors, 50 DEG C are warming up to the heating rate of 3 DEG C/min, under power is 500W condition, re-extract three times, each 20min; (2) merge extract and filter, filtrate to during close to Transparent color, removes ethyl acetate layer with separatory funnel through extraction into ethyl acetate, then after concentrating in a rotary evaporator, freeze drying, obtains persimmon leaf flavone.
A composite preservative containing persimmon leaf flavone, raw material is:
Persimmon leaf flavone extract 0.5 part, CMC 30 parts, glycerine 30 parts, 5 parts, calcium chloride, polyethylene glycol (molecular weight is 200) 20 parts, Tween-20 0.3 part, 1000 parts, water.
The preparation method of composite preservative is as follows:
(1) weight portion CMC, calcium chloride, polyethylene glycol, polysorbas20 are mixed with water, ultrasonic wave added dissolves, and stirs, obtains CMC base fluid;
(2) parts by weight of glycerin is mixed with persimmon leaf flavone, after stirring, obtain flavones-glycerine mixed liquor;
(3) flavones-glycerine mixed liquor is mixed with CMC base fluid, stir, obtain compositional liquor;
(4) compositional liquor is carried out bubble-free in vacuum outgas to compositional liquor under vacuum conditions.
embodiment 2
An extraction for persimmon leaf flavone, is characterized in that, adopts following methods to extract:
(1) powder of persimmon leaf mixes according to solid-liquid ratio 1g:35mL with 45vol% ethanolic solution, then adds acetic acid and regulates pH value to 5, add in supersonic extractors after stirring, 50 DEG C are warming up to the heating rate of 4 DEG C/min, under power is 500W condition, re-extract three times, each 20min;
(2) merge extract and filter, filtrate to during close to Transparent color, removes ethyl acetate layer with separatory funnel through extraction into ethyl acetate, then after concentrating in a rotary evaporator, freeze drying, obtains persimmon leaf flavone.
A composite preservative containing persimmon leaf flavone extract, raw material is:
Persimmon leaf flavone extract 0.95 part, CMC 19 parts, glycerine 36 parts, 7.8 parts, calcium chloride, polyethylene glycol (molecular weight is 400) 15 parts, polysorbas20 0.4 part, 1000 parts, water.
Preparation method is with embodiment 1.
embodiment 3
An extraction for persimmon leaf flavone, is characterized in that, adopts following methods to extract:
(1) powder of persimmon leaf mixes according to solid-liquid ratio 1g:35mL with 45vol% ethanolic solution, then add acetic acid and regulate pH value to 4.5, then the citric acid monoglyceride accounting for persimmon leaf quality 20% is added, add after stirring in supersonic extractors, 50 DEG C are warming up to the heating rate of 4 DEG C/min, under power is 500W condition, re-extract three times, each 20min;
(2) merge extract and filter, filtrate to during close to Transparent color, removes ethyl acetate layer with separatory funnel through extraction into ethyl acetate, then after concentrating in a rotary evaporator, freeze drying, obtains persimmon leaf flavone.
A composite preservative containing persimmon leaf flavone, raw material is:
Persimmon leaf flavone extract 1.3 parts, CMC 10 parts, glycerine 40 parts, 10 parts, calcium chloride, polyethylene glycol (molecular weight is 600) 15 parts, polysorbas20 0.5 part, 1000 parts, water.
Preparation method is with embodiment 1.
comparative example 1
A composite preservative containing persimmon leaf flavone, raw material composition is with embodiment 1.
Preparation method is as follows:
(1) each raw material of weight portion is directly stirred, mix, obtain compositional liquor;
(2) compositional liquor is carried out bubble-free in vacuum outgas to compositional liquor under vacuum conditions.
comparative example 2
An antistaling agent containing persimmon leaf flavone, raw material is:
Persimmon leaf flavone (extracting method is with embodiment 3) 1.5 parts, glycerine 40 parts, 10 parts, calcium chloride, polyethylene glycol 14 parts, Tween-20 0.5 part, 1000 parts, water.
The preparation method of antistaling agent is as follows:
(1) weight portion calcium chloride, polyethylene glycol, polysorbas20 are mixed with water, ultrasonic wave added dissolves, and stirs, obtains base fluid;
(2) parts by weight of glycerin is mixed with persimmon leaf flavone, after stirring, obtain flavones-glycerine mixed liquor;
(3) flavones-glycerine mixed liquor is mixed with base fluid, stir, obtain compositional liquor;
(4) compositional liquor is carried out bubble-free in vacuum outgas to compositional liquor under vacuum conditions.
comparative example 3
A kind of coating antistaling agent, raw material is:
CMC 30 parts, glycerine 40 parts, 10 parts, calcium chloride, polyethylene glycol 14 parts, Tween-20 0.5 part, 1000 parts, water.
Preparation method: raw material is mixed, then degassed to bubble-free in compositional liquor.
Effect test:
1. the composite preservative that embodiment 1 is prepared with comparative example 2-3 is carried out total number of bacteria evaluation.
Test method: select 5 groups just to pluck, intact pleurotus eryngii, wherein do not do any process for blank for one group, wherein 3 groups of composite preservatives utilizing embodiment 3 and comparative example 2-3 to prepare respectively are processed, pleurotus eryngii is put into antistaling agent 1-2s, pull out and naturally to dry afterwards, then at room temperature (20 ± 2 DEG C) are preserved, last group is only by glycerine 40 parts, 10 parts, calcium chloride, polyethylene glycol 14 parts, polysorbas20 0.5 part, soaks 1-2s in the base fluid of 1000 parts, water composition, contrasts as base fluid group.Concrete outcome is in table 1.
Table 1
2.. composite preservative embodiment 1-3 and comparative example 1 prepared is to the fresh-keeping test of honey peach.
Test method: select 5 groups of intact honey peach, antistaling agent prepared by embodiment 1-3 and comparative example 1 is evenly sprayed the White mushroom surface in 1-4 group, 5th group is blank group, do not carry out any process, natural air drying, every 1L composite preservative process honey peach 35kg, deposits 14d at average room temperature is 20 ± 2 DEG C.To healthy fruit, weight-loss ratio and honey peach quality are added up, and concrete outcome is in table 2.
Table 2
3. composite preservative embodiment 1-3 and comparative example 1 prepared is to the fresh-keeping test of White mushroom.
Test method is: the intact White mushroom just plucked is equally divided into 5 groups, antistaling agent prepared by embodiment 1-3 and comparative example 1 is evenly sprayed the White mushroom surface in 1-4 group, 5th group is blank group, do not carry out any process, natural air drying, every 1L composite preservative process White mushroom 40kg, after all packing with polyethylene packaging bag, under room temperature, (20 ± 2 DEG C) carry out preservation, carry out effect assessment to color, smell, form, hardness in total number of bacterial colonies.Evaluation criterion is as follows:
Color: full marks 2 points; Milky or slightly yellow, khaki: 1-2 divides; Yellow, color and luster is dim: 0.5-1 divides; Yellowish-brown, dark brown: less than 0.5 point.
Smell: full marks 1.2 points; Normal mushroom taste, free from extraneous odour: 0.8-1.2 divides; Lighter mushroom taste, slight tart flavour or musty: 0.4-0.8 divides; Acid smell: less than 0.4 point.
Form: full marks 2 points; Institutional framework is good, and anhydrous or a small amount of water flows out, without mould generation: 1-2 divides; Institutional framework is better, and more moisture flows out, a small amount of mould generation: 0.5-1 divides; Institutional framework is poor, and large quantity of moisture flows out, a large amount of mould generation: less than 0.5.
Hardness: full marks 1.2 points; Mushroom umbrella soft durometer is moderate, and mushroom stalk has the toughness of normal mushroom: 0.8-1.2 divides; Mushroom umbrella soft durometer is poor, and the toughness of mushroom umbrella is general: 0.4-0.8 divides; Mushroom umbrella is soft rotten, and mushroom stalk is immalleable: less than 0.4.
Total number of bacteria: full marks 3.6 points; Less than 5000: 2.4-3.6 divides; 5000-10000:1.2-2.4; Less than more than 10000: 1.2.
Carry out effect assessment to the White mushroom of Preservation Treatment at 2d, 4d, 6d, concrete evaluation result is in table 3.
Table 3
Above-described embodiment is the present invention's preferably embodiment; but embodiments of the present invention are not by the restriction of embodiment; other is any do not deviate from Spirit Essence of the present invention and principle under make change, modification, combination, substitute, simplify and all should be equivalent substitute mode, be included within protection scope of the present invention.

Claims (7)

1. the composite preservative containing persimmon leaf flavone, is characterized in that, be made up of following raw material:
Persimmon leaf flavone 0.5-1.5 part, CMC 10-30 part, glycerine 30-40 part, calcium chloride 5-10 part, polyethylene glycol 10-20 part, polysorbas20 0.3-0.5 part, 1000 parts, water.
2. composite preservative according to claim 1, is characterized in that, the molecular weight of described polyethylene glycol is 200-600.
3. composite preservative according to claim 1, is characterized in that, the extraction of described persimmon leaf flavone adopts following methods to obtain:
(1) by the powder of persimmon leaf with 45vol% ethanolic solution according to solid-liquid ratio 1:35(g/mL) mix, then add acetic acid adjust ph, add in supersonic extractors after stirring, be warming up to 50 DEG C with the heating rate of 3-5 DEG C/min, under power is 500W condition, re-extract three times;
(2) merge extract and filter, filtrate to during close to Transparent color, removes ethyl acetate layer with separatory funnel through extraction into ethyl acetate, then after concentrating in a rotary evaporator, freeze drying, obtains persimmon leaf flavone.
4. composite preservative according to claim 3, is characterized in that: in step (1), described in add acetic acid adjust ph be 4-5.
5. the extraction of persimmon leaf flavone according to claim 3, is characterized in that, the time of described extraction is 20min.
6. a preparation method for the composite preservative as described in any one of claim 1-5, is characterized in that, comprises the following steps:
(1) weight portion CMC, calcium chloride, polyethylene glycol, polysorbas20 are mixed with water, ultrasonic wave added dissolves, and stirs, obtains CMC base fluid;
(2) parts by weight of glycerin is mixed with persimmon leaf flavone, after stirring, obtain flavones-glycerine mixed liquor;
(3) flavones-glycerine mixed liquor is mixed with CMC base fluid, stir, obtain compositional liquor;
(4) compositional liquor is carried out bubble-free in vacuum outgas to compositional liquor under vacuum conditions.
7. the application of the composite preservative as described in any one of claim 1-5 in fresh agricultural products is fresh-keeping.
CN201510580604.2A 2015-09-14 2015-09-14 Composite coating film fresh keeping agent containing persimmon leaf flavones as well as preparation method and application of composite coating film fresh keeping agent Pending CN105285077A (en)

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Cited By (3)

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Publication number Priority date Publication date Assignee Title
CN107183076A (en) * 2017-06-07 2017-09-22 天津中智科技发展有限公司 A kind of plants antimicrobial additive and preparation method thereof
CN108077410A (en) * 2017-12-15 2018-05-29 黄照强 A kind of persimmon antistaling agent and preparation method thereof
CN108497057A (en) * 2018-03-28 2018-09-07 华南理工大学 Composite coating preservative of the chromocor extract containing tartary buckwheat bran and its preparation method and application

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107183076A (en) * 2017-06-07 2017-09-22 天津中智科技发展有限公司 A kind of plants antimicrobial additive and preparation method thereof
CN108077410A (en) * 2017-12-15 2018-05-29 黄照强 A kind of persimmon antistaling agent and preparation method thereof
CN108497057A (en) * 2018-03-28 2018-09-07 华南理工大学 Composite coating preservative of the chromocor extract containing tartary buckwheat bran and its preparation method and application

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Application publication date: 20160203