CN103734291B - Water-soluble litchi compound nano preservative preparation method and application thereof - Google Patents

Water-soluble litchi compound nano preservative preparation method and application thereof Download PDF

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Publication number
CN103734291B
CN103734291B CN201410002678.3A CN201410002678A CN103734291B CN 103734291 B CN103734291 B CN 103734291B CN 201410002678 A CN201410002678 A CN 201410002678A CN 103734291 B CN103734291 B CN 103734291B
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antioxidant
water
soluble
filter residue
compound nano
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CN103734291A (en
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聂国朝
梁伟江
吴艳华
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Yulin Normal University
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Abstract

The present invention relates to preparation method and the application thereof of water-soluble litchi compound nano preservative.Preparation process: formation slurries smashed to pieces by caraway tissue and water machinery, sealing soak slurries after 15 ~ 30 hours suction filtration obtain filtrate and filter residue; Add 0.05% ~ 0.5% surfactant in filtrate, mix sealing and place; Filter residue is soaked in alcohol or methyl alcohol, filter residue (heap volume) and alcohol ratio=30ml:60 ~ 250ml, and sealing immersion is after 15 ~ 30 hours, and suction filtration adds antioxidant, makes antioxidant concentration be 6 ~ 12.3g/100ml, obtains antioxidant-alcoholic extract solution; Solution limit containing surfactant adds antioxidant-alcoholic extract solution 60 ~ 250ml, obtains water-soluble litchi compound nano preservative.Antistaling agent of the present invention is used for lichee, carries out fresh-keeping to it after longan fruit picking, in this antistaling agent treated water fruit 0 ~ 5 DEG C of refrigerator or freezer, and freshness-retained more than 31 days.

Description

Water-soluble litchi compound nano preservative preparation method and application thereof
Technical field
The invention belongs to antistaling agent manufacture field, be specifically related to a kind of method and the application thereof that utilize false beach wormwood tissue extract to prepare water-soluble litchi compound nano preservative.
Background technology
False beach wormwood (also Cheng Jia Betel) is the plant of Piperaceae Piper, and its fruit is called complete plectrum.Be distributed in the ground such as Yunnan, Guizhou, Fujian, Tibet, Guangdong, Guangxi of India, Vietnam, Indonesia, Philippine, Papua New Guinea, Malaysia and China's Mainland, be grown on tropical and subtropical region, normal growth is on the other wetland of sylvan life and village, in Vietnam, there is artificial growth in Laos.False beach wormwood is perennial draft of crawling, and that rubs has fragrance.Stipes expands, long-living adventitious root.Leaf alternate, nearly film quality, inhales gland point, the wealthy avette or subcircular of leaf of bottom, long 7-14cm, wide 6-13cm, the short point of tip, and base portion is heart-shaped or enter to cut shape, vein 7; The leaf on top is little, avette to ovum shape lanceolar; The long 1-5cm of petiole.Flower unisexuality, dioecism, without perianth; Cotton-shaped inflorescence; The long 1.5-2cm of male inflorescence, diameter 2-3cm, bract is oblate, diameter 0.5-0.6mm, 2 pieces, stamen; The long 6-8mm of female inflorescence, the prolongation of fruit phase reaches 2.5cm; Bract is slightly large, column cap 3-5.Berry is subsphaeroidal, tool angle rib, diameter 2.5-3cm, and bottom is embedding to be born in sequence axle.Summer at florescence.False beach wormwood can be used for stomach cold pain, and inflatable abdomen aches, rheumatism Low Back Pain, and postpartum, deficiency of vital energy pin swelled, sore pain, hemorrhoid, treating swelling and pain by traumatic injury.But up to now and find no with false beach wormwood for raw material, manufacture the report of vegetalitas antistaling agent.
Lichee is gathered due to high temperature season in full summer, adds that its structure is special, very easily brown stain and rotting after gathering.And the southern lichee collecting period, be rainy season, almost rare sunny day, existing lichee fresh-keeping process all requires that fine day is plucked, and is in fact difficult to realize.At normal temperatures, namely brown stain was rotten in 2 ~ 3 days for litchi fruits, lost commodity value.Postharvest decay is that restriction lichee stores and transports for a long time, one of the principal element that causes the short and fruit commodity value of shelf life to decline.At present, the method such as chemical preservative process, sulfur dioxide treatment, heat treatment of rotting to control for lichee has certain effect to Preservation of Litchi chinensis Fruits, but all there is the defects such as have potential hazard to human body and fresh-keeping effect is not good.Conventional chemical bactericide belongs to pesticide, and chemical bactericide has certain effect to reduction fruit rot, but its high residue harm humans is healthy and pathogen easily develops immunity to drugs to chemical bactericide, and therefore the efficient antiseptic preservation technology of research safety is imperative.The present invention develops a kind of simple and antiseptic preservation technology of lichee storing efficiently again.Fine day, rainy day all can pluck and fresh-keeping.
Antibacterial, antifungal activity that the wild caraway tool such as false beach wormwood that the antistaling agent of the present invention's exploitation adopts is good, can many excellent specific properties (Khalid Hussain, 2012) such as desinsection, antiprotozoal and nontoxicity; The antioxidant sorbic acid selected is the antisepsis antistaling agent of the highly effective and safe of international food and agricultural organization and Health Organisation recommendations, is widely used in the industry such as food, beverage; Nano particle stabilizing agent (surfactant) dialkyl quaternary ammonium salt (Huang Qiran adopted, 2007, Zhang Jinping, 2011), as: two octyl alkyl dimethyl ammonium chloride, didecyl Dimethy ammonium chloride, dodecyl benzyl dimethyl ammonium chloride or polysiloxane quaternary ammonium (HM98) they are good bactericide (Jiang Jianxiang, 2000, Li Junying, 2004), and colourless, odorless (slightly fishy smell, utilize false beach wormwood extract except it), low toxicity, safety (Yang Yanwei, 2011).
Summary of the invention
The object of the invention is to overcome the requirement that existing antistaling agent toxicity is large, meet rainy day, fine day harvesting fresh preservation, solve existing preservation method cost high, agricultural chemicals or sulfur dioxide etc. residue in the problems such as fruit surface, provide one to utilize false beach wormwood (perilla leaf, rosemary etc.) tissue extract to prepare method and the application thereof of water-soluble litchi compound nano preservative.
The solution of the present invention is by realizing like this: a kind of water-soluble litchi compound nano preservative preparation method, and this preparation method's step comprises:
Step 1): caraway tissue: water=300g:1.5 ~ 4L mixing, formation slurries smashed to pieces by machinery, sealing soak slurries after 15 ~ 30 hours suction filtration obtain filtrate and filter residue.Mode smashed to pieces by machinery with stone mill or metal mill, can wear into mud by false beach wormwood or purple perilla or the perfume (or spice) that changes.
Step 2): in the filtrate that step 1) obtains, add 0.05% ~ 0.5% surfactant, mix sealing and place.
Step 3): step 1) is obtained filter residue and be soaked in alcohol, filter residue (heap volume) and alcohol ratio=30ml:60 ~ 250ml, sealing immersion is after 15 ~ 30 hours, suction filtration, antioxidant is added in obtained wine thereby essence extract filtrate, make antioxidant concentration be 6 ~ 12.3g/100ml, obtain antioxidant-alcoholic extract solution.Alcohol-pickledly also can soak extraction with organic solvent methyl alcohol and replace, but extract obtained methyl alcohol rotary evaporation thoroughly must be eliminated after, then add the alcohol of equivalent, finally still form antioxidant-alcoholic extract solution.Methyl alcohol for the recovery rate of active ingredient in caraway tissue than alcohol height 5%-10%.
Step 4): limit whipping step 2) prepared solution limit adds antioxidant-alcoholic extract solution 60 ~ 250ml that step 3) obtains, and obtains water-soluble litchi compound nano preservative.
As further restriction of the present invention, described caraway is organized as false beach wormwood or purple perilla or repeatedly any one or their composition in fragrant tissue.
As further restriction of the present invention, described surfactant is conventional committee's ammonium salt or polysiloxane quaternary ammonium disinfection sanitizer, as any one or their composition in two octyl alkyl dimethyl ammonium chloride, didecyl Dimethy ammonium chloride, dimethyl benzyl ammonium chloride, polysiloxane quaternary ammonium (HM98).
As further restriction of the present invention, described false beach wormwood or purple perilla or be repeatedly fragrantly organized as false beach wormwood or purple perilla or repeatedly spiceleaf, false beach wormwood or purple perilla or any one or their composition repeatedly in fragrant herb.False beach wormwood or purple perilla or repeatedly fragrant herb are finish any one in plectrum or multinomial containing stem, root, fruit.Can be fresh or the false beach wormwood of drying or purple perilla or any one or their composition repeatedly in fragrant herb
As further restriction of the present invention, described antioxidant is any one or their composition in sorbic acid or sorbate.Sorbate can use potassium sorbate, sodium sorbate.
The application of the water-soluble litchi compound nano preservative described in more than one, this water-soluble litchi compound nano preservative is carried out fresh-keeping to it after being used for lichee, longan fruit picking.
For making the present invention openly abundant, the using method of antistaling agent: fresh litchi (longan) immerses this antistaling agent about 1 ~ 5 minute in batches, taking-up sets to 0 ~ and 5 DEG C, drain antistaling agent (about 10 ~ 20 minutes), evenly put into polystyrene foam case and (at the bottom of case, get out porous plastic spacer in advance, in case lichee/longan be dipped into may drip come in antistaling agent, all containers, and the equal thing of preservative film claims to soak with antistaling agent, be pre-chilled to 0 ~ 5 DEG C, with degerming), also can with the polyethylene preservative film sealing thickeied, the isolated air of sealing, bag black plastic bag lucifuge, in 0 ~ 5 DEG C of freezer or refrigerator, freshness-retained more than 31 days.This antistaling agent not only in polystyrene foam case, other closed container, be convenient to transport can.
The know-why that the present invention realizes is: employing low concentration, nontoxic cationic surfactant are emulsifying agent, false beach wormwood (perilla leaf, the rosemary etc.) extract of tropical, that subtropical zone is abundant wild caraway is utilized to be key aroma agent, antistaling agent, bactericide, antifungal agent, pesticide, with water and a small amount of edible organic matter for nano material solvent, add a small amount of antioxidant and be mixed with lichee compound nanoparticle fresh-keeping liquid, wherein diameter of nano particles is about 100-200 nm.Lichee to be immersed in this fresh-keeping liquid several minutes, can uniform fold lichee surface, protection antistaling agent slow releasing.Not only use this antistaling agent under 0-5 DEG C of environment, the ripe lichee fresh-keeping more than 31 days of 7-8 can be made, be applicable to fine day but also be applicable to the fresh fruit that the south rainy day in summer plucks.Dosing apparatus is simple and easy, simple to operate, can be mass-produced.
The present invention possesses following good result:
(1) the present invention is raw material at the false beach wormwood of creationary employing (perilla leaf, rosemary etc.), lixiviate is carried out to it and obtains false beach wormwood extract, false beach wormwood extract is utilized to prepare environment-protecting asepsis, nano compound antistaling agent that applicability is wide, this antistaling agent is under 0-5 DEG C of environment, not only the ripe lichee fresh-keeping more than 31 days of 7-8 can be made, be applicable to fine day but also be applicable to the fresh fruit that the south rainy day in summer plucks.
(2) the present invention's false basket used is suitable for growing under second shade of tree, wet environment, and easy artificial cultivation, is particluarly suitable for lichee forest interplanting, make this compound nanometer fresh-keeping agent raw material sources extensive, cost is low, nanometer fresh-keeping agent fragrant odour, nontoxic, easily wash with water.
(3) the present invention adopt antioxidant sorbic acid (salt) be a kind of unrighted acid (salt) it can by the metabolic system of human body absorb and be decomposed into rapidly carbon dioxide and water, noresidue in vivo.
Accompanying drawing explanation
Fig. 1. water-soluble litchi compound nano preservative preparation method flow chart of the present invention.
Detailed description of the invention
Below in conjunction with embodiment and description the present invention, these descriptions are not be further limited content of the present invention.
embodiment 1
The present embodiment material therefor reagent: false betel 300g, surfactant: the composition of didecyl Dimethy ammonium chloride 0.9g and dodecyl benzyl dimethyl ammonium chloride 0.6g, antioxidant: sorbic acid 8g, is prepared according to following steps.
Step 1): false betel: water=300g:3L mixing, formation slurries smashed to pieces by machinery, sealing soak slurries after 24 hours suction filtration obtain filtrate and filter residue.
Step 2): in the filtrate that step 1) obtains, add 0.05% surfactant, mix sealing and place.
Step 3): step 1) is obtained filter residue and be soaked in alcohol, filter residue (heap volume) and alcohol ratio=30ml:90ml, sealing immersion suction filtration after 20 hours, adds antioxidant in this leaching liquid 66ml, antioxidant concentration is 12.1g/100ml, obtains antioxidant-alcoholic extract solution.
Step 4): limit whipping step 2) prepared solution limit adds antioxidant-alcoholic extract solution 66ml that step 3) obtains, and obtains water-soluble litchi compound nano preservative.The compound nanometer fresh-keeping agent that the present embodiment obtains Britain's Malvern ParticleSizer detects, and Nanoparticle Size is 160 ~ 170nm about.
embodiment 2
The present embodiment material therefor reagent: perilla leaf 150g, rosemary leave 150 grams, surfactant: polysiloxane quaternary ammonium (HM98) 3g, antioxidant: potassium sorbate 4g, is prepared according to following steps.
Step 1): perilla leaf, rosemary leave: water=300g:1.5L mixing, formation slurries smashed to pieces by machinery, sealing soak slurries after 20 hours suction filtration obtain filtrate and filter residue.
Step 2): in the filtrate that step 1) obtains, add 0.2% surfactant, mix sealing and place.
Step 3): step 1) is obtained filter residue and be soaked in alcohol, filter residue (heap volume) and methyl alcohol ratio=30ml:60ml, sealing immersion is after 24 hours, suction filtration, removing filter residue, rotary evaporation reclaims methyl alcohol, and the brown paste of gained is dissolved in 100ml alcohol and adds antioxidant, antioxidant concentration is 6.0g/100ml, obtains antioxidant-alcoholic extract solution.
Step 4): limit whipping step 2) prepared solution limit adds antioxidant-alcoholic extract solution 66ml that step 3) obtains, and obtains water-soluble litchi compound nano preservative.The compound nanometer fresh-keeping agent that the present embodiment obtains Britain's Malvern ParticleSizer detects, and Nanoparticle Size is 120 ~ 130nm about.
embodiment 3
The present embodiment material therefor reagent: false beach wormwood herb (containing stem, root) 300g, surfactant: the composition of polysiloxane quaternary ammonium (HM98) 5g, dodecyl benzyl dimethyl ammonium chloride 5g, antioxidant: sorbic acid 6g, is prepared according to following steps.
Step 1): false beach wormwood herb: water=300g:3L mixing, formation slurries smashed to pieces by machinery, sealing soak slurries after 20 hours suction filtration obtain filtrate and filter residue.
Step 2): in the filtrate that step 1) obtains, add 0.33% surfactant, mix sealing and place.
Step 3): step 1) is obtained filter residue and be soaked in alcohol, filter residue (heap volume) and alcohol ratio=30ml:250ml, sealing immersion suction filtration after 24 hours, adds antioxidant in this leaching liquid 66ml, antioxidant concentration is 9.0g/100ml, obtains antioxidant-alcoholic extract solution.
Step 4): limit whipping step 2) prepared solution limit adds antioxidant-alcoholic extract solution 66ml that step 3) obtains, and obtains water-soluble litchi compound nano preservative.The compound nanometer fresh-keeping agent that the present embodiment obtains Britain's Malvern ParticleSizer detects, and Nanoparticle Size is 190 ~ 200nm about.
embodiment 4
The present embodiment material therefor reagent: repeatedly spiceleaf 150g, false betel 150g, surfactant: the composition of polysiloxane quaternary ammonium (HM98) 5g, didecyl Dimethy ammonium chloride 9g, dodecyl benzyl dimethyl ammonium chloride 6g, antioxidant: sorbic acid 6g, sodium sorbate 10g, be prepared according to following steps.
Step 1): repeatedly repeatedly spiceleaf, false betel: water=300g:4L mixing, formation slurries smashed to pieces by machinery, sealing soak slurries after 15 hours suction filtration obtain filtrate and filter residue.
Step 2): in the filtrate that step 1) obtains, add 0.5% surfactant, mix sealing and place.
Step 3): step 1) is obtained filter residue and be soaked in alcohol, filter residue (heap volume) and alcohol ratio=30ml:200ml, sealing immersion suction filtration after 30 hours, adds antioxidant in this leaching liquid 66ml, antioxidant concentration is 7.0g/ml, obtains antioxidant-alcoholic extract solution.
Step 4): limit whipping step 2) prepared solution limit adds antioxidant-alcoholic extract solution 66ml that step 3) obtains, and obtains water-soluble litchi compound nano preservative.The compound nanometer fresh-keeping agent that the present embodiment obtains Britain's Malvern ParticleSizer detects, and Nanoparticle Size is 120 ~ 130nm about.
embodiment 5
The present embodiment material therefor reagent: purple perilla herb (containing stem, root) 300g, surfactant: the composition of dodecyl benzyl dimethyl ammonium chloride 12g, antioxidant: sorbic acid 4.5g, sodium sorbate 2g, be prepared according to following steps.
Step 1): purple perilla herb: water=300g:3L mixing, formation slurries smashed to pieces by machinery, sealing soak slurries after 15 hours suction filtration obtain filtrate and filter residue.
Step 2): in the filtrate that step 1) obtains, add 0.4% surfactant, mix sealing and place.
Step 3): step 1) is obtained filter residue and be soaked in alcohol, filter residue (heap volume) and alcohol ratio=30ml:100ml, sealing immersion suction filtration after 24 hours, adds antioxidant in this leaching liquid 66ml, antioxidant concentration is 9.8g/100ml, obtains antioxidant-alcoholic extract solution.
Step 4): limit whipping step 2) prepared solution limit adds antioxidant-alcoholic extract solution 66ml that step 3) obtains, and obtains water-soluble litchi compound nano preservative.The compound nanometer fresh-keeping agent that the present embodiment obtains Britain's Malvern ParticleSizer detects, and Nanoparticle Size is 160 ~ 170nm about.
embodiment 6
The present embodiment material therefor reagent: false beach wormwood herb (containing stem, root, finish and pull out son) 150g, purple perilla herb 150g, surfactant: the composition of polysiloxane quaternary ammonium (HM98) 5g, dodecyl benzyl dimethyl ammonium chloride 5g, antioxidant: sorbic acid 8.1g, is prepared according to following steps.
Step 1): false beach wormwood herb: water=300g:3L mixing, formation slurries smashed to pieces by machinery, sealing soak slurries after 20 hours suction filtration obtain filtrate and filter residue.
Step 2): in the filtrate that step 1) obtains, add 0.33% surfactant, mix sealing and place.
Step 3): step 1) is obtained filter residue and be soaked in alcohol, filter residue (heap volume) and alcohol ratio=30ml:80ml, sealing immersion suction filtration after 24 hours, adds antioxidant in this leaching liquid 66ml, antioxidant concentration is 12.3g/100ml, obtains antioxidant-alcoholic extract solution.
Step 4): limit whipping step 2) prepared solution limit adds antioxidant-alcoholic extract solution 66ml that step 3) obtains, and obtains water-soluble litchi compound nano preservative.The compound nanometer fresh-keeping agent that the present embodiment obtains Britain's Malvern ParticleSizer detects, and Nanoparticle Size is 190 ~ 200nm about.
embodiment 7application Example
The water-soluble litchi compound nano preservative that embodiment 1 ~ 6 prepares, water-soluble litchi compound nano preservative is carried out fresh-keeping to it after can be used for lichee, longan fruit picking.
The using method of antistaling agent: fresh litchi (longan) immerses this antistaling agent about 1 ~ 5 minute in batches, taking-up sets to 0 ~ and 5 DEG C, drain antistaling agent (about 10 ~ 20 minutes), evenly put into polystyrene foam case and (at the bottom of case, get out porous plastic spacer in advance, in case lichee (longan) be dipped into may drip come in antistaling agent, all containers and the equal thing of preservative film claim to soak with antistaling agent, be pre-chilled to 0 ~ 5 DEG C, with degerming), the isolated air of sealing, bag black plastic bag lucifuge, in 0 ~ 5 DEG C of freezer or refrigerator, freshness-retained more than 31 days.

Claims (4)

1. a water-soluble litchi compound nano preservative preparation method, is characterized in that, this preparation method's step comprises:
Step 1): caraway tissue: water=300g:1.5 ~ 4L mixing, formation slurries smashed to pieces by machinery, sealing soak slurries after 15 ~ 30 hours suction filtration obtain filtrate and filter residue;
Step 2): in step 1) add 0.05% ~ 0.5% surfactant in the filtrate that obtains, mix sealing and place;
Step 3): by step 1) obtain filter residue and be soaked in alcohol, filter residue heap volume and alcohol ratio=30ml:60 ~ 250ml, sealing immersion is after 15 ~ 30 hours, suction filtration, antioxidant is added in obtained wine thereby essence extract filtrate, make antioxidant concentration be 6.0 ~ 12.3g/100ml, obtain antioxidant-alcoholic extract solution;
Step 4): at whipping step 2) prepared solution adds step 3 simultaneously) antioxidant-alcoholic extract solution 60 ~ 250ml of obtaining, obtain water-soluble litchi compound nano preservative;
Described caraway is organized as false beach wormwood or purple perilla or repeatedly any one or their composition in fragrant tissue;
Described surfactant is any one or their composition in two octyl alkyl dimethyl ammonium chloride, didecyl Dimethy ammonium chloride, dimethyl benzyl ammonium chloride, polysiloxane quaternary ammonium;
Described antioxidant is any one or their composition in sorbic acid or sorbate.
2. water-soluble litchi compound nano preservative preparation method according to claim 1, it is characterized in that, described false beach wormwood or purple perilla or be repeatedly fragrantly organized as false beach wormwood or purple perilla or repeatedly spiceleaf, false beach wormwood or purple perilla or any one or their composition repeatedly in fragrant herb.
3. a water-soluble litchi compound nano preservative preparation method, is characterized in that, this preparation method's step comprises:
Step 1): caraway tissue: water=300g:1.5 ~ 4L mixing, formation slurries smashed to pieces by machinery, sealing soak slurries after 15 ~ 30 hours suction filtration obtain filtrate and filter residue;
Step 2): in step 1) add 0.05%-0.5% surfactant in the filtrate that obtains, mix sealing and place;
Step 3): by step 1) obtain filter residue and be soaked in methyl alcohol, filter residue heap volume and methyl alcohol ratio=30ml:60 ~ 250ml, sealing immersion is after 15 ~ 30 hours, suction filtration, after the dry methyl alcohol of filtrate rotary evaporation, add equal-volume alcohol and dissolve again and obtain alcoholic extract solution, in obtained wine thereby essence extract filtrate, add antioxidant, make antioxidant concentration be 6.0 ~ 12.3g/100ml, obtain antioxidant-alcoholic extract solution;
Step 4): limit whipping step 2) prepared solution limit adds step 3) antioxidant-alcoholic extract solution 60 ~ 250ml of obtaining, obtain water-soluble litchi compound nano preservative; Described caraway is organized as false beach wormwood or purple perilla or repeatedly any one or their composition in fragrant tissue; Described false beach wormwood or purple perilla or be repeatedly fragrantly organized as false beach wormwood or purple perilla or repeatedly spiceleaf, false beach wormwood or purple perilla or any one or their composition repeatedly in fragrant herb;
Described surfactant is any one or their composition in two octyl alkyl dimethyl ammonium chloride, didecyl Dimethy ammonium chloride, dimethyl benzyl ammonium chloride, polysiloxane quaternary ammonium;
Described antioxidant is any one or their composition in sorbic acid or sorbate.
4. an application for the water-soluble litchi compound nano preservative described in any one of claims 1 to 3, is characterized in that, this water-soluble litchi compound nano preservative is carried out fresh-keeping to it after being used for lichee, longan fruit picking.
CN201410002678.3A 2014-01-03 2014-01-03 Water-soluble litchi compound nano preservative preparation method and application thereof Expired - Fee Related CN103734291B (en)

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CN105767129B (en) * 2016-03-17 2020-07-28 广东海洋大学 Piper sarmentosum roxb leaf extract and application thereof in fresh keeping of pitaya
CN107343532A (en) * 2017-07-05 2017-11-14 广西南宁乐蕊生物科技有限责任公司 A kind of antistaling agent of Han Jia Betel extracts and Prochloraz

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