CN105831546A - Winter jasmine extract and application thereof in preparation of food preservative - Google Patents
Winter jasmine extract and application thereof in preparation of food preservative Download PDFInfo
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- CN105831546A CN105831546A CN201610164311.0A CN201610164311A CN105831546A CN 105831546 A CN105831546 A CN 105831546A CN 201610164311 A CN201610164311 A CN 201610164311A CN 105831546 A CN105831546 A CN 105831546A
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
- A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
- A23L3/3454—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of liquids or solids
- A23L3/3463—Organic compounds; Microorganisms; Enzymes
- A23L3/3472—Compounds of undetermined constitution obtained from animals or plants
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Abstract
The invention discloses a winter jasmine extract and an application thereof in preparation of a food preservative containing the winter jasmine extract. The winter jasmine extract is prepared by the following steps: (a) mixing dry winter jasmine and artemisia capillaris, crushing the mixture, carrying out hot reflux extraction with an 80-90% ethanol solution, merging the extract liquids, and concentrating to have no alcohol smell, to obtain an ethanol extraction concentrated liquid; (b) diluting the ethanol extraction concentrated liquid obtained in the step (a) with water, successively extracting with petroleum ether, ethyl acetate and water saturated n-butanol, and carrying out reduced pressure concentration, to respectively obtain a petroleum ether extract, an ethyl acetate extract and an n-butanol extract; and (c) dissolving the n-butanol extract with water, filtering, enriching active ingredients with AB-8 type macroporous resin, firstly rinsing with 5-15% ethanol with the amount of 6-10 times of the column volume to remove large-polarity ingredients, then eluting with 70-80% ethanol with the amount of 8-12 times of the column volume, collecting a 70-80% ethanol eluent, and carrying out reduced pressure concentration, wherein the amount of the artemisia capillaris accounts for 5%-15% of the total weight of the winter jasmine and the artemisia capillaris.
Description
Technical field
The invention belongs to field of food, relate to preparation and the application of preservative, be specifically related to a kind of Flos Jasmini Nudiflori extract and in system
Application in standby food preservative.
Background technology
Flos Jasmini Nudiflori is the flower of Oleaceae plants Flos Jasmini Nudiflori.2～April receive adopt, dry.Former plant Flos Jasmini Nudiflori is machaka, up to 5
Rice.Branch is elongated, upright or overarch, and sprig is smooth without hair, has four ribs.Compound leaf is to life；3, lobule, avette or long ellipse
Shape is avette, long 1～3 centimetre, tip point, and there is fine, soft fur at edge, below without hair；Petiole length 5～10 millimeters.Spend faint yellow, first leaf
Bloom, on the branch being born in last year, single raw or axil life；Bennet is about 6 millimeters, is had the little bud of long and narrow green；Calyx mitriform,
Sliver 6, wire, green, with calyx letter with long or longer；Corolla pipe height foot dish, about 2 centimetres of footpath, sliver 6, long 6 millimeters,
Cylinder minister 12 millimeters；Stamen 2, and is born in cylindrical fireworks；Ovary 2 Room.Florescence 2～April.Plant in flower garden more.Distribution Shandong,
The ground such as Shaanxi, Liaoning, Jiangsu, Zhejiang, Guizhou.
For a long time, food industry is all got used to synthetic as the preservative such as benzoic acid and its esters of food, Pyrusussuriensis
Acid and its esters and parabens etc., it the most inevitably produces bad shadow to the local flavor of food
Ring, once exceed standard and human body can be produced toxic and side effects.Natural antiseptic agent has that antibiotic property is strong, safety non-toxic, good water solubility,
Heat stability is good, there is the advantages such as certain alimentary health-care function, the exploitation of natural plant source antiseptic agent and apply to spiced and stewed food
Produce and meet natural, safety, the developing direction of nutrition.
Summary of the invention
It is an object of the invention to provide the preparation method and applications of a kind of natural plant source antiseptic agent based on Flos Jasmini Nudiflori, this is prevented
Flos Jasmini Nudiflori extract in rotten agent has significant antibacterial antisepsis.
Above-mentioned purpose is achieved by the following technical solution:
A kind of Flos Jasmini Nudiflori extract with antibacterial antisepsis is prepared via a method which: (a) is by dry Flos Jasmini Nudiflori and Herba Artemisiae Scopariae
Artemisia mixes, and pulverizes, and with 80～90% ethanol solution circumfluence distillation, united extraction liquid, is concentrated into that to obtain ethanol extraction without alcohol taste dense
Contracting liquid；(b) by step (a) gained ethanol extraction concentrated solution dilute with water, successively by petroleum ether, ethyl acetate and water saturated
N-butanol extraction, concentrating under reduced pressure, respectively obtain petroleum ether extract, acetic acid ethyl ester extract and n-butyl alcohol extract；C () just
Butanol extract water dissolution, filters, with AB-8 type macroporous resin enrichment active component, first with 5～15% alcohol flushing 6～10
Individual column volume removes big polar component, then with 70～80% ethanol elution 8～12 column volumes, collection 70～80% ethanol elution,
Concentrating under reduced pressure；Wherein, Herba Artemisiae Scopariae accounts for the 5%～15% of Flos Jasmini Nudiflori and Herba Artemisiae Scopariae gross weight.
Further, the described Flos Jasmini Nudiflori extract with antibacterial antisepsis is prepared via a method which: (a) is by dry
Flos Jasmini Nudiflori and Herba Artemisiae Scopariae mixing, pulverize, with 85% ethanol solution circumfluence distillation, united extraction liquid, be concentrated into and obtain without alcohol taste
Ethanol extraction concentrated solution；B (), by step (a) gained ethanol extraction concentrated solution dilute with water, uses petroleum ether, ethyl acetate successively
With water saturated n-butanol extraction, concentrating under reduced pressure, respectively obtain petroleum ether extract, acetic acid ethyl ester extract and n-butanol extraction
Thing；C () n-butyl alcohol extract water dissolution, filters, with AB-8 type macroporous resin enrichment active component, first uses 10% ethanol
Rinse 8 column volumes and remove big polar component, then with 10 column volumes of 75% ethanol elution, collect 75% ethanol elution,
Concentrating under reduced pressure；Wherein, Herba Artemisiae Scopariae accounts for the 10% of Flos Jasmini Nudiflori and Herba Artemisiae Scopariae gross weight.
Further, the described Flos Jasmini Nudiflori extract with antibacterial antisepsis is prepared via a method which: (a) is by dry
Flos Jasmini Nudiflori and Herba Artemisiae Scopariae mixing, pulverize, with 80% ethanol solution circumfluence distillation, united extraction liquid, be concentrated into and obtain without alcohol taste
Ethanol extraction concentrated solution；B (), by step (a) gained ethanol extraction concentrated solution dilute with water, uses petroleum ether, ethyl acetate successively
With water saturated n-butanol extraction, concentrating under reduced pressure, respectively obtain petroleum ether extract, acetic acid ethyl ester extract and n-butanol extraction
Thing；C () n-butyl alcohol extract water dissolution, filters, with AB-8 type macroporous resin enrichment active component, first with 5% ethanol punching
Wash 10 column volumes and remove big polar component, then with 12 column volumes of 70% ethanol elution, collect 70% ethanol elution, subtract
Pressure concentrates；Wherein, Herba Artemisiae Scopariae accounts for the 5% of Flos Jasmini Nudiflori and Herba Artemisiae Scopariae gross weight.
Further, the described Flos Jasmini Nudiflori extract with antibacterial antisepsis is prepared via a method which: (a) is by dry
Flos Jasmini Nudiflori and Herba Artemisiae Scopariae mixing, pulverize, with 90% ethanol solution circumfluence distillation, united extraction liquid, be concentrated into and obtain without alcohol taste
Ethanol extraction concentrated solution；B (), by step (a) gained ethanol extraction concentrated solution dilute with water, uses petroleum ether, ethyl acetate successively
With water saturated n-butanol extraction, concentrating under reduced pressure, respectively obtain petroleum ether extract, acetic acid ethyl ester extract and n-butanol extraction
Thing；C () n-butyl alcohol extract water dissolution, filters, with AB-8 type macroporous resin enrichment active component, first uses 15% ethanol
Rinse 6 column volumes and remove big polar component, then with 8 column volumes of 80% ethanol elution, collect 80% ethanol elution, subtract
Pressure concentrates；Wherein, Herba Artemisiae Scopariae accounts for the 15% of Flos Jasmini Nudiflori and Herba Artemisiae Scopariae gross weight.
The application in terms of preparing food preservative of the above-mentioned Flos Jasmini Nudiflori extract.
Beneficial effects of the present invention:
The food preservative that the present invention provides mainly contains Flos Jasmini Nudiflori extract, and this extract has significant antibacterial antisepsis,
May be used for the antibacterial anticorrosion of field of food, and pure natural, without synthesis of chemicals.
Detailed description of the invention
Further illustrate the essentiality content of the present invention below in conjunction with embodiment, but do not limit scope with this.To the greatest extent
The present invention is explained in detail by pipe with reference to preferred embodiment, it will be understood by those within the art that, can be to the present invention
Technical scheme modify or equivalent, without deviating from the spirit and scope of technical solution of the present invention.
Crude drug source: medical material Flos Jasmini Nudiflori and Herba Artemisiae Scopariae are purchased from Hui nationality's Chinese Medicinal Materials Markets.
Main agents: food-grade ethanol is purchased from Shanghai Ling Feng chemical reagent company limited；AB-8 type macroporous resin is purchased from sky tunami letter
Resin company limited；Acetonitrile is HPLC level, is purchased from TEDIA；Formic acid is HPLC level, is purchased from TEDIA；Chromatographic grade is pure
Water is heartily pure water.Agents useful for same and material are the customary commercial being commercially available.
Embodiment 1: the preparation of Flos Jasmini Nudiflori extract
A Flos Jasmini Nudiflori that 5kg is dried by () and Herba Artemisiae Scopariae (accounting for gross weight 10%) co-grinding, extract 3 with 85% alcohol heat reflux
Secondary (25L × 3 time), each 2 hours, united extraction liquid, it is concentrated into and obtains concentrated solution (3L) without alcohol taste；B () is to step (a)
Concentrated solution is successively by petroleum ether (3L × 3 time), ethyl acetate (3L × 3 time) and water saturated n-butyl alcohol (3L × 3 time) extraction
Take, respectively obtain petroleum ether extract, acetic acid ethyl ester extract and n-butyl alcohol extract；(c) n-butyl alcohol extract AB-8
Type macroporous resin enrichment, first removes big polar substancess with 8 column volumes of 10% alcohol flushing, then with 75% ethanol elution 10
Column volume, collects 75% ethanol elution, concentrating under reduced pressure.
Embodiment 2: the preparation of Flos Jasmini Nudiflori extract
A Flos Jasmini Nudiflori that 5kg is dried by () and Herba Artemisiae Scopariae (accounting for gross weight 5%) co-grinding, extract 3 with 80% alcohol heat reflux
Secondary (25L × 3 time), each 2 hours, united extraction liquid, it is concentrated into and obtains concentrated solution (3L) without alcohol taste；B () is to step (a)
Concentrated solution is successively by petroleum ether (3L × 3 time), ethyl acetate (3L × 3 time) and water saturated n-butyl alcohol (3L × 3 time) extraction
Take, respectively obtain petroleum ether extract, acetic acid ethyl ester extract and n-butyl alcohol extract；(c) n-butyl alcohol extract AB-8
Type macroporous resin enrichment, first removes big polar substancess with 10 column volumes of 5% alcohol flushing, then with 70% ethanol elution 12
Column volume, collects 70% ethanol elution, concentrating under reduced pressure.
Embodiment 3: the preparation of Flos Jasmini Nudiflori extract
A Flos Jasmini Nudiflori that 5kg is dried by () and Herba Artemisiae Scopariae (accounting for gross weight 15%) co-grinding, extract 3 with 90% alcohol heat reflux
Secondary (25L × 3 time), each 2 hours, united extraction liquid, it is concentrated into and obtains concentrated solution (3L) without alcohol taste；B () is to step (a)
Concentrated solution is successively by petroleum ether (3L × 3 time), ethyl acetate (3L × 3 time) and water saturated n-butyl alcohol (3L × 3 time) extraction
Take, respectively obtain petroleum ether extract, acetic acid ethyl ester extract and n-butyl alcohol extract；(c) n-butyl alcohol extract AB-8
Type macroporous resin enrichment, first removes big polar substancess with 6 column volumes of 15% alcohol flushing, then with 8 posts of 80% ethanol elution
Volume, collects 80% ethanol elution, concentrating under reduced pressure.
Embodiment 4: the contrast of embodiment 1, without Herba Artemisiae Scopariae
A Flos Jasmini Nudiflori that 5kg is dried by () is pulverized, with 85% 3 times (25L × 3 time) of alcohol heat reflux extraction, and each 2 hours,
United extraction liquid, is concentrated into and obtains concentrated solution (3L) without alcohol taste；(b) to step (a) concentrated solution successively with petroleum ether (3L ×
3 times), ethyl acetate (3L × 3 time) and water saturated n-butyl alcohol (3L × 3 time) extraction, respectively obtain petroleum ether extract,
Acetic acid ethyl ester extract and n-butyl alcohol extract；C () n-butyl alcohol extract AB-8 type macroporous resin enrichment, first uses 10% second
Alcohol rinses 8 column volumes and removes big polar substances, then with 10 column volumes of 75% ethanol elution, collects 75% ethanol elution,
Concentrating under reduced pressure.
Embodiment 5: the contrast of embodiment 1, Herba Artemisiae Scopariae accounts for gross weight 20%
A Flos Jasmini Nudiflori that 5kg is dried by () and Herba Artemisiae Scopariae (accounting for gross weight 20%) co-grinding, extract 3 with 85% alcohol heat reflux
Secondary (25L × 3 time), each 2 hours, united extraction liquid, it is concentrated into and obtains concentrated solution (3L) without alcohol taste；B () is to step (a)
Concentrated solution is successively by petroleum ether (3L × 3 time), ethyl acetate (3L × 3 time) and water saturated n-butyl alcohol (3L × 3 time) extraction
Take, respectively obtain petroleum ether extract, acetic acid ethyl ester extract and n-butyl alcohol extract；(c) n-butyl alcohol extract AB-8
Type macroporous resin enrichment, first removes big polar substancess with 8 column volumes of 10% alcohol flushing, then with 75% ethanol elution 10
Column volume, collects 75% ethanol elution, concentrating under reduced pressure.
Embodiment 6: bacteriostatic test
Prepare Flos Jasmini Nudiflori extract 1～5 according to embodiment 1～5, investigate functions on common pollutant bacteria in Flos Jasmini Nudiflori extract 1～5 pairs of food
Bacteriostatic test, bacteriostatic test uses the method for filter paper.Flos Jasmini Nudiflori extract 1～5 is configured to concentration with deionized water dissolving respectively
Extract solution for 280mg/L.
Employing strain is as follows: Salmonella, staphylococcus aureus, Liszt mononuclear cell bacterium, escherichia coli, bacillus botulinus.
The preparation method of filter paper: with card punch, 102 type Xinhua filter paper are made the beaker putting into dried and clean of a diameter of 6mm,
Sterilizing 30 minutes, dry for standby in 121 DEG C of autoclave sterilization pots.
The mensuration of Flos Jasmini Nudiflori extract 1～5 bacteriostasis: the bacteria suspension 0.1mL drawing suitable concentration by sterile test tube adds to fall
Good plating medium surface, coating is uniformly；Respectively with micropipettor injection 20mL extract solution on filter paper, will
Filter paper is affixed on the plating medium surface of inoculated bacteria, three, every ware, in triplicate.It is inverted plate 37 DEG C cultivation 18 little
Shi Hou, measures antibacterial circle diameter with slide gauge.The results are shown in Table 1.
Inhibition zone (mm)=bacteriostatic diameter-6 (mm).
Table 1 Flos Jasmini Nudiflori extract 1～5 bacteriostasis
Result shows: Flos Jasmini Nudiflori extract 1～3 has obvious bacteriostasis.Flos Jasmini Nudiflori extract 4 and 5 fungistatic effect is poor,
Substantially not as natural Flos Jasmini Nudiflori extract 1～3；The antibacterial antiseptic effect of Flos Jasmini Nudiflori extract of the present invention is described and whether adds Herba Artemisiae Scopariae
The ratio that Artemisia and Herba Artemisiae Scopariae add is relevant.This Flos Jasmini Nudiflori extract can prepare the food preservative that antibacterial antiseptic effect is excellent.
The effect of above-described embodiment indicates that the essentiality content of the present invention, but does not limit protection scope of the present invention with this.
It will be understood by those within the art that, technical scheme can be modified or equivalent, and not take off
Essence and protection domain from technical solution of the present invention.
Claims (5)
1. a Flos Jasmini Nudiflori extract with antibacterial antisepsis, it is characterised in that be prepared via a method which: (a) will be dry
Dry Flos Jasmini Nudiflori and Herba Artemisiae Scopariae mixing, pulverize, and with 80～90% ethanol solution circumfluence distillation, united extraction liquid, is concentrated into without alcohol
Taste obtains ethanol extraction concentrated solution；B (), by step (a) gained ethanol extraction concentrated solution dilute with water, uses petroleum ether, second successively
Acetoacetic ester and water saturated n-butanol extraction, concentrating under reduced pressure, respectively obtain petroleum ether extract, acetic acid ethyl ester extract and positive fourth
Alcohol extract；C () n-butyl alcohol extract water dissolution, filters, with AB-8 type macroporous resin enrichment active component, first with 5～15%
Alcohol flushing 6～10 column volumes remove big polar components, then with 70～80% ethanol elution 8～12 column volumes, collection 70～80%
Ethanol elution, concentrating under reduced pressure；Wherein, Herba Artemisiae Scopariae accounts for the 5%～15% of Flos Jasmini Nudiflori and Herba Artemisiae Scopariae gross weight.
The Flos Jasmini Nudiflori extract with antibacterial antisepsis the most according to claim 1, it is characterised in that by such as lower section
Prepared by method: dry Flos Jasmini Nudiflori and Herba Artemisiae Scopariae are mixed by (a), pulverize, with 85% ethanol solution circumfluence distillation, united extraction
Liquid, is concentrated into and obtains ethanol extraction concentrated solution without alcohol taste；B (), by step (a) gained ethanol extraction concentrated solution dilute with water, depends on
Secondary petroleum ether, ethyl acetate and water saturated n-butanol extraction, concentrating under reduced pressure, respectively obtain petroleum ether extract, acetic acid second
Ester extract and n-butyl alcohol extract；C () n-butyl alcohol extract water dissolution, filters, live by AB-8 type macroporous resin enrichment
Property composition, first remove big polar components with 8 column volumes of 10% alcohol flushing, then with 10 column volumes of 75% ethanol elution,
Collect 75% ethanol elution, concentrating under reduced pressure；Wherein, Herba Artemisiae Scopariae accounts for the 10% of Flos Jasmini Nudiflori and Herba Artemisiae Scopariae gross weight.
The Flos Jasmini Nudiflori extract with antibacterial antisepsis the most according to claim 1, it is characterised in that by such as lower section
Prepared by method: dry Flos Jasmini Nudiflori and Herba Artemisiae Scopariae are mixed by (a), pulverize, with 80% ethanol solution circumfluence distillation, united extraction
Liquid, is concentrated into and obtains ethanol extraction concentrated solution without alcohol taste；B (), by step (a) gained ethanol extraction concentrated solution dilute with water, depends on
Secondary petroleum ether, ethyl acetate and water saturated n-butanol extraction, concentrating under reduced pressure, respectively obtain petroleum ether extract, acetic acid second
Ester extract and n-butyl alcohol extract；C () n-butyl alcohol extract water dissolution, filters, live by AB-8 type macroporous resin enrichment
Property composition, first remove big polar components with 10 column volumes of 5% alcohol flushing, then with 12 column volumes of 70% ethanol elution,
Collect 70% ethanol elution, concentrating under reduced pressure；Wherein, Herba Artemisiae Scopariae accounts for the 5% of Flos Jasmini Nudiflori and Herba Artemisiae Scopariae gross weight.
The Flos Jasmini Nudiflori extract with antibacterial antisepsis the most according to claim 1, it is characterised in that by such as lower section
Prepared by method: dry Flos Jasmini Nudiflori and Herba Artemisiae Scopariae are mixed by (a), pulverize, with 90% ethanol solution circumfluence distillation, united extraction
Liquid, is concentrated into and obtains ethanol extraction concentrated solution without alcohol taste；B (), by step (a) gained ethanol extraction concentrated solution dilute with water, depends on
Secondary petroleum ether, ethyl acetate and water saturated n-butanol extraction, concentrating under reduced pressure, respectively obtain petroleum ether extract, acetic acid second
Ester extract and n-butyl alcohol extract；C () n-butyl alcohol extract water dissolution, filters, live by AB-8 type macroporous resin enrichment
Property composition, first remove big polar components with 6 column volumes of 15% alcohol flushing, then by 8 column volumes of 80% ethanol elution, receipts
Collect 80% ethanol elution, concentrating under reduced pressure；Wherein, Herba Artemisiae Scopariae accounts for the 15% of Flos Jasmini Nudiflori and Herba Artemisiae Scopariae gross weight.
5. the application in terms of preparing food preservative of the Flos Jasmini Nudiflori extract described in Claims 1 to 4.
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| CN201610164311.0A CN105831546A (en) | 2016-03-22 | 2016-03-22 | Winter jasmine extract and application thereof in preparation of food preservative |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106963700A (en) * | 2017-05-23 | 2017-07-21 | 林燕 | A kind of extracting method of winter jasmine active ingredient |
| CN111775249A (en) * | 2020-07-08 | 2020-10-16 | 安徽昌发实业有限公司 | Mildew-proof and corrosion-proof treatment method for rubber wood |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102250174A (en) * | 2011-07-25 | 2011-11-23 | 吉首大学 | Method for extracting jasminin from winter jasmine leaves |
| CN102266469A (en) * | 2011-03-28 | 2011-12-07 | 山东大学威海分校 | Compound artemisia capillaries preparation and application thereof |
| CN105360171A (en) * | 2015-10-12 | 2016-03-02 | 邯郸学院 | Preparation method and application of plant source bacteriostatic agent |
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2016
- 2016-03-22 CN CN201610164311.0A patent/CN105831546A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102266469A (en) * | 2011-03-28 | 2011-12-07 | 山东大学威海分校 | Compound artemisia capillaries preparation and application thereof |
| CN102250174A (en) * | 2011-07-25 | 2011-11-23 | 吉首大学 | Method for extracting jasminin from winter jasmine leaves |
| CN105360171A (en) * | 2015-10-12 | 2016-03-02 | 邯郸学院 | Preparation method and application of plant source bacteriostatic agent |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106963700A (en) * | 2017-05-23 | 2017-07-21 | 林燕 | A kind of extracting method of winter jasmine active ingredient |
| CN111775249A (en) * | 2020-07-08 | 2020-10-16 | 安徽昌发实业有限公司 | Mildew-proof and corrosion-proof treatment method for rubber wood |
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Application publication date: 20160810 |