CN105497959A - A preparing method of a graphene oxide antibacterial mildew-resistant medical bandage - Google Patents

A preparing method of a graphene oxide antibacterial mildew-resistant medical bandage Download PDF

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CN105497959A
CN105497959A CN201510828217.6A CN201510828217A CN105497959A CN 105497959 A CN105497959 A CN 105497959A CN 201510828217 A CN201510828217 A CN 201510828217A CN 105497959 A CN105497959 A CN 105497959A
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graphene oxide
antibacterial
mouldproof
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bandage
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CN105497959B (en
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张建刚
张重静
王兰芳
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
    • A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
    • A61L15/22—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing macromolecular materials
    • A61L15/26—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
    • A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
    • A61L15/18—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing inorganic materials
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
    • A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
    • A61L15/20—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing organic materials
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
    • A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
    • A61L15/22—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing macromolecular materials
    • A61L15/24—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
    • A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
    • A61L15/42—Use of materials characterised by their function or physical properties
    • A61L15/46—Deodorants or malodour counteractants, e.g. to inhibit the formation of ammonia or bacteria
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
    • C07C41/01—Preparation of ethers
    • C07C41/34—Separation; Purification; Stabilisation; Use of additives
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/10—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing inorganic materials
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/20—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing organic materials
    • A61L2300/216—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing organic materials with other specific functional groups, e.g. aldehydes, ketones, phenols, quaternary phosphonium groups
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
    • A61L2300/404—Biocides, antimicrobial agents, antiseptic agents

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Abstract

The invention relates to a preparing method of a graphene oxide antibacterial mildew-resistant medical bandage. The method includes evenly spraying gauze with a prepared antibacterial mildew-resistant agent through a spraying process to obtain the antibacterial mildew-resistant medical bandage. Antibacterial mildew-resistant and peculiar smell-removing effects of the bandage are significantly improved through synergistic effects of nanometer graphene oxide, a wild lily bulb extract and nanometer metal-supported graphene oxide. The mildew-resistant level of the bandage is the zero level. The bacteriostatic rate of the bandage for staphylococcus aureus is 99.91%, the bacteriostatic rate of the bandage for escherichia coli is 99.23%, the bacteriostatic rate of the bandage for helicobacter pylori is 99.0%, the bacteriostatic rate of the bandage for candida albicans is 98%, and the bacteriostatic rate of the bandage for mould is 100%. For the gauze sprayed with the antibacterial mildew-resistant agent, nanometer particles penetrate into the gauze and inner cohesiveness of the gauze is enhanced, and therefore hairiness is greatly reduced, and secondary wounds when the bandage is used by a patient are avoided.

Description

A kind of preparation method of graphene oxide antibacterial and mouldproof medical bandage
Technical field
The present invention relates to a kind of preparation method, be specifically related to a kind of preparation method of graphene oxide antibacterial and mouldproof medical bandage.Belong to new material technology field.
Background technology
Medical bandage be come into vogue early 1980s use there is certain elastic wrapper material.Medical bandage has good elasticity and comfortableness, multiplex at athletic protective and medical field.Because medical bandage has continuous elastic and not easily slippage performance that conventional bandages do not possess, medical bandage is made to have indispensable status on medical nursing and treatment.But the phenomenons such as the medical bandage used at present exists filoplume, allergy, go mouldy, be easily adhered, infected wound, cause secondary insult.
Functionalized graphene (grapheneoxide) is the oxide of Graphene, and its color is brown color, and product common on the market has Powdered, lamellar and solution shape.Because of after oxidation, it on oxygen-containing functional group increase and make character comparatively Graphene more vivaciously, nature can be improved via various with the reaction of oxygen-containing functional group.Graphene oxide thin slice is powdered graphite through chemical oxidation and the product after peeling off, graphene oxide is single atomic layer, can expand to some tens of pm at any time on lateral dimension, therefore, and its construct trans typical size of general chemistry and material science.Graphene oxide can be considered a kind of flexible material of non-traditional kenel, has polymer, colloid, thin film, and amphiphilic characteristic.Graphene oxide is regarded as hydroaropic substance for a long time, because it has superior dispersibility in water, but related experiment result shows, in fact graphene oxide has amphipathic, presents hydrophilic to hydrophobic property distribution from graphene platelet edge to central authorities.Therefore, graphene oxide can as interfacial agent Presence of an interface, and reduce the energy between interface.
Herba Crotalariae sessiliflorae is the herb of leguminous plant Herba Crotalariae sessiliflorae.Summer, autumn gather.Another name Herba Sedi Multicaulis (" Zhiwu Mingshi Tukao "), leopard cat bean (" botany voluminous dictionary "), Canis familiaris L. bell grass, blue flower Herba Crotalariae sessiliflorae (" Chinese main plant figure says pulse family "), Folium Trematis Dielsianae, Herba lamii barbati, Semen Sesami jingle bell bell (" Zhejiang conventional medical herbs among the people "), Herba Crotalariae sessiliflorae (" full exhibition a collection of selected materials tumor ").Former plant Herba Crotalariae sessiliflorae is annual upright draft, high 20 ~ 100 centimetres, and be close to slightly long hair, hair is slightly coarse.Dan Ye, linear or lanceolar, leaf blade size alters a great deal, long 2.5 ~ 8 centimetres, wealthy 0.5 ~ 1 centimetre, the narrow point in two ends, and tip has pencil hair usually, above slightly by hair or several without hair, drapes over one's shoulders mercerising matter hair below; Several without petiole; Stipule is superfine little, setiform.Raceme, top is raw or axil is raw, and spend 2 ~ 20, flower is together intensive.Bract and squamella fairly similar, linear; Squamella and is born in bennet top, is all become mildewed by roughish; Bennet is extremely short, sagging during result: calyx is long 10 ~ 15 millimeters, is closely become mildewed by brown color, calyx tooth tip point; Corolla butterfly, hyacinthine or light blue, about isometric with calyx, vexil is circular, and ala is short compared with vexil, the shape of falling ovum square circle, fossil fragments and ala isometric, inflection, tool beak; Stamen 10, monomer, flower pesticide 2 type; Ovary stockless, style is elongated.Pod without hair, Long Circle, about isometric with calyx; 10 ~ 15, seed.Florescence JIUYUE.Be born in the weeds of wasteland.Distribution northeast, East China, south China and southwestern various places.Be common in the application of Herba Crotalariae sessiliflorae extract and field of medicaments, but its extract be applied to the antibacterial and mouldproof medical instruments field of medical bandage, rarely have report.
Summary of the invention
The object of the invention is the deficiency existed for overcoming above-mentioned prior art, a kind of preparation method of graphene oxide antibacterial and mouldproof medical bandage is provided.
For achieving the above object, the present invention adopts following technical proposals:
A preparation method for graphene oxide antibacterial and mouldproof medical bandage, the method comprises: be evenly distributed on gauze by the antibacterial mildew inhibitor of preparation through spray processing, obtains antibacterial and mouldproof medical bandage.
The agent of described antibacterial and mouldproof enzyme, with weight portion, it comprises: nano graphene oxide 0.5-1.55 part, nano load burning Graphene 0.05-0.55 part, nano-calcium carbonate 1.3-9.5 part, Herba Crotalariae sessiliflorae extract compound 0.02-0.65 part, Polyethylene Glycol 1.0-5.5 part, polyvinylpyrrolidone 0.2-1.8 part, water 50-120 part.
Described nano graphene oxide, its purity >=99%, lamellar spacing 0.5-2nm, lamella length is 500-900nm.
The carried metal of described nano load burning Graphene can be one or more in silver, copper, palladium.
The structural formula that described Herba Crotalariae sessiliflorae extracts compound is:
Described Herba Crotalariae sessiliflorae extracts the preparation method of compound, comprise following operating procedure: the dry herb of Herba Crotalariae sessiliflorae is pulverized by (a), extract with 75 ~ 85% alcohol heat reflux, merge extractive liquid, be concentrated into without alcohol taste, use petroleum ether, ethyl acetate and water saturated n-butanol extraction successively, obtain petroleum ether extract, acetic acid ethyl ester extract and n-butyl alcohol extract respectively; Acetic acid ethyl ester extract macroporous resin remove impurity in (b) step (a), first use 10% ethanol elution, 8 column volumes, then use 75% ethanol elution, 10 column volumes, collect 75% ethanol elution, concentrating under reduced pressure obtains 75% ethanol elution thing extractum; C in () step (b), 75% ethanol elution extractum purification on normal-phase silica gel is separated, obtain 5 components successively with the methylene chloride-methanol gradient elution that volume ratio is 85: 1,40: 1,20: 1,12: 1 and 1: 1; D in () step (c), component 4 is separated further by purification on normal-phase silica gel, obtain 3 components successively with the methylene chloride-methanol gradient elution that volume ratio is 20: 1,12: 1 and 5: 1; E in () step (d), component 2 reverse phase silica gel of octadecylsilane bonding is separated, with the methanol aqueous solution isocratic elution that concentration expressed in percentage by volume is 70%, collect 8 ~ 10 column volume eluents, namely eluent concentrating under reduced pressure obtains Herba Crotalariae sessiliflorae and extracts compound.
Described antibacterial and mouldproof enzyme agent preparation method, specifically comprise following operating procedure: under (a) ul-trasonic irradiation, successively the Polyethylene Glycol of weight portion, polyvinylpyrrolidone and nano-calcium carbonate are added to the water, ul-trasonic irradiation 25-75min, ultrasonic power: 200-600W system temperature: 10-30 DEG C; (2) room temperature mechanical stirring action, extracts nano graphene oxide, nano load burning Graphene, Herba Crotalariae sessiliflorae compound and adds in step (1) system, rotating speed: 300-12000r/min, time: 10-50min successively.
The sprinkling ratio of described antibacterial mildew inhibitor is 0.5-3.5g/m 2gauze.
Beneficial effect of the present invention: (1) preparation technology proposed by the invention is simple and easy to operate, does not use chemical drugs and with low cost, reduces its production cycle, is easy to realize industrial-scale production.
Medical bandage obtained by the present invention, owing to the addition of nano graphene oxide simultaneously, nano metal load graphene oxide, Herba Crotalariae sessiliflorae extract, this medical bandage is had antibacterial, mildew-resistant, the functionality advantage such as eliminate the unusual smell, this is because graphene oxide bactericidal property is remarkable, the physics " antibiotic " not having drug resistance, graphene oxide not only can by cutting the insertion of bacterial cell membrane, directly can also be extracted by the extensive of phospholipid molecule in cell membrane, destroy cell membrane thus kill antibacterial, the two-dimensional structure of Graphene uniqueness makes it with the phospholipid molecule on bacterial cell membrane, superpower interaction can occur, thus cause a large amount of phospholipid molecule to depart from cell membrane, Herba Crotalariae sessiliflorae extract of the present invention is a kind of new compound, research finds it, and to antibacterial, particularly mycete is very responsive, under the synergism of nano graphene oxide, Herba Crotalariae sessiliflorae extract and nano metal load graphene oxide, considerably improve the effect that its antibacterial and mouldproof eliminates the unusual smell, its mildew-resistant grade is 0 grade, be 99.91% to the bacteriostasis rate of staphylococcus aureus, be 99.23% to colibacillary bacteriostasis rate, to the bacteriostasis rate of helicobacter pylori be 99.0%, bacteriostasis rate 98% to Candida albicans, for being 100% to the bacteriostasis rate of mycete.
(2) gauze of spray antimicrobial mildew-resistant, nanoparticle immerses in yarn, strengthens yarn interior cohesiveness, greatly reduces the generation of filoplume phenomenon, secondary insult when avoiding patient to use.
Accompanying drawing explanation
Fig. 1 is compound (I) structural formula figure;
Fig. 2 is the theoretical ECD value of compound (I) and experiment ECD value comparison diagram.
Detailed description of the invention
Further illustrate essentiality content of the present invention below in conjunction with embodiment, but do not limit scope with this.Although be explained in detail the present invention with reference to preferred embodiment, those of ordinary skill in the art should be appreciated that and can modify to technical scheme of the present invention or equivalent replacement, and does not depart from essence and the scope of technical solution of the present invention.
Embodiment 1:
Herba Crotalariae sessiliflorae extracts compound separation preparation and structural identification:
Preparation method: the dry herb (10kg) of (a) Herba Crotalariae sessiliflorae is pulverized, (25L × 3 time) are extracted with 80% alcohol heat reflux, merge extractive liquid, be concentrated into without alcohol taste (3L), use petroleum ether (3L × 3 time), ethyl acetate (3L × 3 time) and water saturated n-butyl alcohol (3L × 3 time) to extract successively, obtain petroleum ether extract, acetic acid ethyl ester extract (398g) and n-butyl alcohol extract respectively; Acetic acid ethyl ester extract AB-8 type macroporous resin remove impurity in (b) step (a), first use 10% ethanol elution, 8 column volumes, use 75% ethanol elution, 10 column volumes again, collect 75% ethanol elution, concentrating under reduced pressure obtains 75% ethanol elution thing extractum (163g); C in () step (b), 75% ethanol elution extractum 200-300 order purification on normal-phase silica gel is separated, successively with volume ratio be 85: 1 (8 column volumes), the methylene chloride-methanol gradient elution of 40: 1 (8 column volumes), 20: 1 (8 column volumes), 12: 1 (10 column volumes) and 1: 1 (5 column volumes) obtains 5 components; D component 4 (49g) 200-300 order purification on normal-phase silica gel is separated further in () step (c), successively with volume ratio be 20: 1 (8 column volumes), the methylene chloride-methanol gradient elution of 12: 1 (10 column volumes) and 5: 1 (5 column volumes) obtains 3 components; E in () step (d), component 2 (25g) the reverse phase silica gel ODS-C18 of octadecylsilane bonding is separated, with the methanol aqueous solution isocratic elution that concentration expressed in percentage by volume is 70%, collect 8 ~ 10 column volume eluents, eluent concentrating under reduced pressure obtains pure compound (I) (44mg).
Structural identification: Yellow amorphous powder; HR-ESIMS shows [M+Na] +for m/z549.2314, can obtain molecular formula in conjunction with nuclear-magnetism feature is C 33h 34o 6, degree of unsaturation is 17.Hydrogen nuclear magnetic resonance modal data δ h(ppm, DMSO-d 6, 500MHz): H-4 (6.33, d, J=1.8), H-6 (6.55, d, J=1.8), H-α (6.85, d, J=16.0), H-β (6.61, d, J=16.0), H-2 ', 6 ' (7.04, d, J=8.2), H-3 ', 5 ' (6.64, d, J=8.2) H-3 " (6.24, d, J=2.3), H-5 " (6.14, dd, J=8.2, 2.3), H-6 " (6.62, d, J=8.2), H-α ' (2.38, 2H, m), H-β ' (2.20, 2H, m), H-γ ' (4.45, br, s), H-2 " ', 6 " ' (7.04, d, J=8.2), H-3 " ', 5 " ' (6.64, d, J=8.2), 3-OCH 3(3.58, s), 2 "-OCH 3(3.52, s), 4 "-OCH 3(3.62, s), 4 " '-OCH 3(3.59, s), carbon-13 nmr spectra data δ c(ppm, DMSO-d 6, 125MHz): 139.9 (C, 1-C), 124.7 (C, 2-C), 160.0 (C, 3-C), 98.5 (CH, 4-C), 159.6 (C, 5-C), 103.7 (CH, 6-C), 125.8 (CH, α-C), 130.6 (CH, β-C), 130.1 (C, 1 '-C), 128.2 (CH, 2 ', 6 '-C), 116.0 (CH, 3 ', 5 '-C), 157.5 (C, 4 '-C), 122.3 (C, 1 "-C), 159.3 (C, 2 "-C), 99.2 (CH, 3 "-C), 156.9 (C, 4 "-C), 106.8 (CH, 5 "-C), 130.6 (CH, 6 "-C), 28.5 (CH 2, α '-C), 33.4 (CH 2, β '-C), 39.6 (CH, γ '-C), 138.0 (C, 1 " '-C), 129.1 (CH, 2 " ', 6 " '-C), 113.6 (CH, 3 " ', 5 " '-C), 158.1 (C, 4 " '-C), 55.2 (CH 3, 3-OCH 3), 55.2 (CH 3, 2 " and-OCH 3), 55.4 (CH 3, 4 " and-OCH 3), 55.2 (CH 3, 4 " '-OCH 3), carbon atom labelling is see Fig. 1. 1hNMR and 1h- 1hCOSY spectrum demonstrates two couples of bimodal [δ H7.04 (2H, d, J=8.2Hz) of diproton, 6.64 (2H, d, J=8.2Hz), 7.04 (2H, d, J=8.2Hz), 6.64 (2H, d, J=8.2Hz)], show that this compound contains two Isosorbide-5-Nitraes-di-substituted aryl ring.In addition, the coupled signal δ H6.62 (1H, d, J=8.2Hz) of one group of ABX is observed, 6.24 (1H, d, J=2.3Hz) and 6.14 (1H, dd, J=8.2,2.3Hz), show that this compound contains 1,2, a 4-trisubstituted aromatic ring.Coupled signal δ H6.55 (1H, d, J=1.8Hz) and 6.33 (1H, d, J=1.8Hz) between another two, illustrates also containing 1,2,3, a 5-tetra-substituted aroma ring.Except aromatic protons, also have two trans olefins proton signal δ H6.85 (1H, d, J=16.0Hz) and 6.61 (1H, d, J=16.0Hz), two methylene aliphatic proton signals [δ H2.20 (2H, m), 2.38 (2H, m)], methine signals [d4.45 (1H, a br, ] and four methoxyl group signals [δ H3.62,3.59,3.58 s), 3.52, (3H, s)]. 13cNMR and hsqc spectrum show composes 11 consistent fragrant quaternary carbons with hydrogen, comprises six containing oxygen quaternary carbon, 13 aromatic series methine carbons, three aliphatic methine carbons, two aliphatic mesomethylene carbons, four methoxyl group carbon.In HMBC spectrum, the dependency of trans olefins sp2 spin proton and p-hydroxy benzenes and four substituted benzene rings shows that this compound is conjugation stilbenes compound. 1h- 1hCOSY Correlated Spectroscopy indicates aliphatic chain carbon signal C-α ', the existence of C-β ', C-γ ', and in HMBC spectrum, H-α ' and the dependency of aromatic series carbon show that C-α ' is connected with 2,4-Dimethoxyphenyls.In NOESY spectrum, the dependency of H-γ ' signal and trans olefins unit and 3-methoxyl group-5-hydroxyl phenyl ring shows, above-mentioned stilbene unit is connected with C-γ '.Comprehensive hydrogen spectrum, carbon spectrum, HMBC spectrum and NOESY spectrum, and document is about correlation type nuclear magnetic data, can substantially determine this compound as shown in Figure 1, spatial configuration is determined further by ECD test, theoretical value and experiment value basically identical (Fig. 2).
Embodiment 2:
A preparation method for graphene oxide antibacterial and mouldproof medical bandage, the method comprises: be evenly distributed on gauze by the antibacterial mildew inhibitor of preparation through spray processing, obtains antibacterial and mouldproof medical bandage.
The agent of described antibacterial and mouldproof enzyme, with weight portion, it comprises: nano graphene oxide 0.5 part, nano load burning Graphene 0.05 part, nano-calcium carbonate 1.3 parts, Herba Crotalariae sessiliflorae extract compound 0.02 part, Polyethylene Glycol 1.0 parts, polyvinylpyrrolidone 0.2 part, 50 parts, water.
Described nano graphene oxide, its purity >=99%, lamellar spacing 0.5nm, lamella length is 500nm.
The carried metal of described nano load burning Graphene can be silver.
Described Herba Crotalariae sessiliflorae extracts structural formula of compound and preparation method thereof, with embodiment 1.
Described antibacterial and mouldproof enzyme agent preparation method, specifically comprise following operating procedure: under (a) ul-trasonic irradiation, successively the Polyethylene Glycol of weight portion, polyvinylpyrrolidone and nano-calcium carbonate are added to the water, ul-trasonic irradiation 25min, ultrasonic power: 200W system temperature: 10 DEG C; (2) room temperature mechanical stirring action, extracts nano graphene oxide, nano load burning Graphene, Herba Crotalariae sessiliflorae compound and adds in step (1) system, rotating speed: 300r/min, time: 50min successively.
The sprinkling ratio of described antibacterial mildew inhibitor is 0.5g/m 2gauze.
Through antibacterial test, being 99.91% to the bacteriostasis rate of staphylococcus aureus, is 99.23% to colibacillary bacteriostasis rate, to the bacteriostasis rate of helicobacter pylori be 99.0%, bacteriostasis rate 98% to Candida albicans, for being 100% to the bacteriostasis rate of mycete.
Embodiment 3:
A preparation method for graphene oxide antibacterial and mouldproof medical bandage, the method comprises: be evenly distributed on gauze by the antibacterial mildew inhibitor of preparation through spray processing, obtains antibacterial and mouldproof medical bandage.
The agent of described antibacterial and mouldproof enzyme, with weight portion, it comprises: nano graphene oxide 1.55 parts, nano load burning Graphene 0.55 part, nano-calcium carbonate 9.5 parts, Herba Crotalariae sessiliflorae extract compound 0.65 part, Polyethylene Glycol 5.5 parts, polyvinylpyrrolidone 1.8 parts, 120 parts, water.
Described nano graphene oxide, its purity >=99%, lamellar spacing 2nm, lamella length is 900nm.
The carried metal of described nano load burning Graphene can be copper.
Described Herba Crotalariae sessiliflorae extracts structural formula of compound and preparation method thereof, with embodiment 1.
Described antibacterial and mouldproof enzyme agent preparation method, specifically comprise following operating procedure: under (a) ul-trasonic irradiation, successively the Polyethylene Glycol of weight portion, polyvinylpyrrolidone and nano-calcium carbonate are added to the water, ul-trasonic irradiation 75min, ultrasonic power: 600W system temperature: 30 DEG C; (2) room temperature mechanical stirring action, extracts nano graphene oxide, nano load burning Graphene, Herba Crotalariae sessiliflorae compound and adds in step (1) system, rotating speed: 12000r/min, time: 10min successively.
The sprinkling ratio of described antibacterial mildew inhibitor is 3.5g/m 2gauze.
Through antibacterial test, being 99.95% to the bacteriostasis rate of staphylococcus aureus, is 99.98% to colibacillary bacteriostasis rate, to the bacteriostasis rate of helicobacter pylori be 99.23%, bacteriostasis rate 99.12% to Candida albicans, for being 100% to the bacteriostasis rate of mycete.
Embodiment 4:
A preparation method for graphene oxide antibacterial and mouldproof medical bandage, the method comprises: be evenly distributed on gauze by the antibacterial mildew inhibitor of preparation through spray processing, obtains antibacterial and mouldproof medical bandage.
The agent of described antibacterial and mouldproof enzyme, with weight portion, it comprises: nano graphene oxide 1.0 parts, nano load burning Graphene 0.1 part, nano-calcium carbonate 1.8 parts, Herba Crotalariae sessiliflorae extract compound 0.12 part, Polyethylene Glycol 1.8 parts, polyvinylpyrrolidone 0.8 part, 40 parts, water.
Described nano graphene oxide, its purity >=99%, lamellar spacing 1.0nm, lamella length is 600nm.
The carried metal of described nano load burning Graphene can be silver and palladium.
Described Herba Crotalariae sessiliflorae extracts structural formula of compound and preparation method thereof, with embodiment 1.
Described antibacterial and mouldproof enzyme agent preparation method, specifically comprise following operating procedure: under (a) ul-trasonic irradiation, successively the Polyethylene Glycol of weight portion, polyvinylpyrrolidone and nano-calcium carbonate are added to the water, ul-trasonic irradiation 45min, ultrasonic power: 350W system temperature: 25 DEG C; (2) room temperature mechanical stirring action, extracts nano graphene oxide, nano load burning Graphene, Herba Crotalariae sessiliflorae compound and adds in step (1) system, rotating speed: 800r/min, time: 15min successively.
The sprinkling ratio of described antibacterial mildew inhibitor is 1.5g/m 2gauze.
Through antibacterial test, being 99.99% to the bacteriostasis rate of staphylococcus aureus, is 99.98% to colibacillary bacteriostasis rate, to the bacteriostasis rate of helicobacter pylori be 99.95%, bacteriostasis rate 99.98% to Candida albicans, for being 100% to the bacteriostasis rate of mycete.
Embodiment 5:
A preparation method for graphene oxide antibacterial and mouldproof medical bandage, the method comprises: be evenly distributed on gauze by the antibacterial mildew inhibitor of preparation through spray processing, obtains antibacterial and mouldproof medical bandage.
The agent of described antibacterial and mouldproof enzyme, with weight portion, it comprises: nano graphene oxide 1.45 parts, nano load burning Graphene 0.45 part, nano-calcium carbonate 8.5 parts, Herba Crotalariae sessiliflorae extract compound 0.35 part, Polyethylene Glycol 4.5 parts, polyvinylpyrrolidone 1.3 parts, 100 parts, water.
Described nano graphene oxide, its purity >=99%, lamellar spacing 1.5nm, lamella length is 850nm.
The carried metal of described nano load burning Graphene can be silver, copper and palladium.
Described Herba Crotalariae sessiliflorae extracts structural formula of compound and preparation method thereof, with embodiment 1.
Described antibacterial and mouldproof enzyme agent preparation method, specifically comprise following operating procedure: under (a) ul-trasonic irradiation, successively the Polyethylene Glycol of weight portion, polyvinylpyrrolidone and nano-calcium carbonate are added to the water, ul-trasonic irradiation 65min, ultrasonic power: 550W system temperature: 28 DEG C; (2) room temperature mechanical stirring action, extracts nano graphene oxide, nano load burning Graphene, Herba Crotalariae sessiliflorae compound and adds in step (1) system, rotating speed: 9000r/min, time: 25min successively.
The sprinkling ratio of described antibacterial mildew inhibitor is 3.2g/m 2gauze.
Through antibacterial test, being 99.99% to the bacteriostasis rate of staphylococcus aureus, is 99.68% to colibacillary bacteriostasis rate, to the bacteriostasis rate of helicobacter pylori be 99.98%, bacteriostasis rate 97% to Candida albicans, for being 100% to the bacteriostasis rate of mycete.
Although above-mentioned, the specific embodiment of the present invention is described; but not limiting the scope of the invention; on the basis of technical scheme of the present invention, those skilled in the art do not need to pay various amendment or distortion that creative work can make still within protection scope of the present invention.

Claims (8)

1. a preparation method for graphene oxide antibacterial and mouldproof medical bandage, the method comprises: be evenly distributed on gauze by the antibacterial mildew inhibitor of preparation through spray processing, obtains antibacterial and mouldproof medical bandage.
2. the preparation method of graphene oxide antibacterial and mouldproof medical bandage according to claim 1, it is characterized in that: the agent of described antibacterial and mouldproof enzyme, with weight portion, it comprises: nano graphene oxide 0.5-1.55 part, nano load burning Graphene 0.05-0.55 part, nano-calcium carbonate 1.3-9.5 part, Herba Crotalariae sessiliflorae extract compound 0.02-0.65 part, Polyethylene Glycol 1.0-5.5 part, polyvinylpyrrolidone 0.2-1.8 part, water 50-120 part.
3. the preparation method of graphene oxide antibacterial and mouldproof medical bandage according to claim 2, is characterized in that: described nano graphene oxide, its purity >=99%, lamellar spacing 0.5-2nm, and lamella length is 500-900nm.
4. the preparation method of graphene oxide antibacterial and mouldproof medical bandage according to claim 2, is characterized in that: the carried metal of described nano load burning Graphene can be one or more in silver, copper, palladium.
5. the preparation method of graphene oxide antibacterial and mouldproof medical bandage according to claim 2, is characterized in that: the structural formula that described Herba Crotalariae sessiliflorae extracts compound is:
6. the preparation method of graphene oxide antibacterial and mouldproof medical bandage according to claim 2, it is characterized in that: described Herba Crotalariae sessiliflorae extracts the preparation method of compound, comprise following operating procedure: the dry herb of Herba Crotalariae sessiliflorae is pulverized by (a), extract with 75 ~ 85% alcohol heat reflux, merge extractive liquid, be concentrated into without alcohol taste, use petroleum ether, ethyl acetate and water saturated n-butanol extraction successively, obtain petroleum ether extract, acetic acid ethyl ester extract and n-butyl alcohol extract respectively; Acetic acid ethyl ester extract macroporous resin remove impurity in (b) step (a), first use 10% ethanol elution, 8 column volumes, then use 75% ethanol elution, 10 column volumes, collect 75% ethanol elution, concentrating under reduced pressure obtains 75% ethanol elution thing extractum; C in () step (b), 75% ethanol elution extractum purification on normal-phase silica gel is separated, obtain 5 components successively with the methylene chloride-methanol gradient elution that volume ratio is 85: 1,40: 1,20: 1,12: 1 and 1: 1; D in () step (c), component 4 is separated further by purification on normal-phase silica gel, obtain 3 components successively with the methylene chloride-methanol gradient elution that volume ratio is 20: 1,12: 1 and 5: 1; E in () step (d), component 2 reverse phase silica gel of octadecylsilane bonding is separated, with the methanol aqueous solution isocratic elution that concentration expressed in percentage by volume is 70%, collect 8 ~ 10 column volume eluents, namely eluent concentrating under reduced pressure obtains Herba Crotalariae sessiliflorae and extracts compound.
7. the preparation method of graphene oxide antibacterial and mouldproof medical bandage according to claim 2, it is characterized in that: described antibacterial and mouldproof enzyme agent preparation method, specifically comprise following operating procedure: under (a) ul-trasonic irradiation, successively the Polyethylene Glycol of weight portion, polyvinylpyrrolidone and nano-calcium carbonate are added to the water, ul-trasonic irradiation 25-75min, ultrasonic power: 200-600W system temperature: 10-30 DEG C; (2) room temperature mechanical stirring action, extracts nano graphene oxide, nano load burning Graphene, Herba Crotalariae sessiliflorae compound and adds in step (1) system, rotating speed: 300-12000r/min, time: 10-50min successively.
8. the preparation method of graphene oxide antibacterial and mouldproof medical bandage according to claim 1, is characterized in that: the sprinkling ratio of described antibacterial mildew inhibitor is 0.5-3.5g/m 2gauze.
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CN105963073A (en) * 2016-04-22 2016-09-28 济南圣泉集团股份有限公司 Microcurrent band-aid
CN107050633A (en) * 2017-06-14 2017-08-18 成都润泰智通科技有限公司 Destroy the debridement system of bacterial biof iotalm
CN107938021A (en) * 2017-10-18 2018-04-20 福建恒安卫生材料有限公司 A kind of anti-bacterial fibre, preparation method and disposable absorbent article surface layer antibacterial non-woven
CN108641995A (en) * 2018-05-21 2018-10-12 山东省科创食用菌产业技术研究院 A kind of formula and method improving liquid spawn yield using bark diffusion juice
CN109042724A (en) * 2018-08-15 2018-12-21 广州康滤净化科技有限公司 A kind of graphene is compound except net wind material of musty and preparation method thereof
CN114775019A (en) * 2022-05-25 2022-07-22 西南医科大学附属医院 Preparation method of medical metal implant surface antibacterial coating
CN115428805A (en) * 2022-09-26 2022-12-06 常州大学 Graphene oxide-based composite antibacterial material and preparation method of antibacterial solution

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CN104248520A (en) * 2013-06-25 2014-12-31 王平 Caper euphorbia seed Crotalaria sessiliflora L. Chinese medicinal mask

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US20100160887A1 (en) * 2008-09-10 2010-06-24 Ruby Lee Brown Lily pad panty
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CN104248520A (en) * 2013-06-25 2014-12-31 王平 Caper euphorbia seed Crotalaria sessiliflora L. Chinese medicinal mask
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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105963073A (en) * 2016-04-22 2016-09-28 济南圣泉集团股份有限公司 Microcurrent band-aid
CN105968903A (en) * 2016-06-08 2016-09-28 西安科技大学 Composition for metallic oxide thin film transistor coating
CN107050633A (en) * 2017-06-14 2017-08-18 成都润泰智通科技有限公司 Destroy the debridement system of bacterial biof iotalm
CN107938021A (en) * 2017-10-18 2018-04-20 福建恒安卫生材料有限公司 A kind of anti-bacterial fibre, preparation method and disposable absorbent article surface layer antibacterial non-woven
CN108641995A (en) * 2018-05-21 2018-10-12 山东省科创食用菌产业技术研究院 A kind of formula and method improving liquid spawn yield using bark diffusion juice
CN109042724A (en) * 2018-08-15 2018-12-21 广州康滤净化科技有限公司 A kind of graphene is compound except net wind material of musty and preparation method thereof
CN114775019A (en) * 2022-05-25 2022-07-22 西南医科大学附属医院 Preparation method of medical metal implant surface antibacterial coating
CN115428805A (en) * 2022-09-26 2022-12-06 常州大学 Graphene oxide-based composite antibacterial material and preparation method of antibacterial solution
CN115428805B (en) * 2022-09-26 2024-04-30 常州大学 Preparation method of graphene oxide-based composite antibacterial material and antibacterial solution

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