CN105497959B - A kind of preparation method of graphene oxide antibacterial and mouldproof medical bandage - Google Patents

A kind of preparation method of graphene oxide antibacterial and mouldproof medical bandage Download PDF

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CN105497959B
CN105497959B CN201510828217.6A CN201510828217A CN105497959B CN 105497959 B CN105497959 B CN 105497959B CN 201510828217 A CN201510828217 A CN 201510828217A CN 105497959 B CN105497959 B CN 105497959B
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graphene oxide
antibacterial
mouldproof
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preparation
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CN105497959A (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

Abstract

The present invention relates to a kind of preparation method of graphene oxide antibacterial and mouldproof medical bandage, this method includes：The antibacterial mildew inhibitor of preparation is evenly distributed on gauze through spray processing, up to antibacterial and mouldproof medical bandage.Under the synergistic effect of nano graphene oxide, rattlebush extract and nano metal load graphene oxide, considerably improve the effect that its antibacterial and mouldproof eliminates the unusual smell, its mould proof grade is 0 grade, bacteriostasis rate to staphylococcus aureus is 99.91%, bacteriostasis rate to Escherichia coli is 99.23%, bacteriostasis rate to helicobacter pylori is 99.0%, the bacteriostasis rate 98% to Candida albicans, to be 100% to the bacteriostasis rate of mould.The mould proof gauze of spray antimicrobial, nano-particle are immersed in yarn, are strengthened yarn interior cohesiveness, are greatly reduced the generation of filoplume phenomenon, secondary insult when avoiding the patient from using.

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, and in particular to a kind of graphene oxide doctor antibacterial and mouldproof treats the preparation side of bandage Method.Belong to new material technology field.
Background technology
Medical bandage is the wrapper material with certain elasticity used that comes into vogue early 1980s.Medical bandage With good elasticity and comfort, it is used in athletic protective and medical field more.Since there are medical bandage conventional bandages not have Standby continuous elastic and it is not easy to slip performance so that medical bandage has indispensable status on medical nursing and treatment. But the medical bandage used at present there are filoplume, allergy, go mouldy phenomena such as, be easily adhered, infected wound, cause secondary insult.
Graphite alkene (graphene oxide) is the oxide of graphene, its color is brown color, common on the market Product has powdered, sheet and solution shape.After oxidized, oxygen-containing functional group increases and makes property compared with graphene more thereon Add vivaciously, nature can be improved via the various and reaction of oxygen-containing functional group.Graphene oxide thin slice is powdered graphite warp Product after chemical oxidation and stripping, graphene oxide is single atomic layer, can expand to number on lateral dimension at any time Ten microns, therefore, the typical size of the general chemistry of its construct trans and material science.Graphene oxide can be considered a kind of non-biography The flexible material for kenel of uniting, has polymer, colloid, film, and the characteristic of amphiphatic molecule.Graphene oxide for a long time by It is considered as hydroaropic substance, because it has superior dispersiveness in water, still, related experiment is the results show that graphene oxide It is of virtually amphipathic, hydrophilic to hydrophobic property distribution is presented from graphene platelet edge to center.Therefore, graphite oxide Alkene can generally there are interface such as interfacial agent, and reduce the energy between interface.
Rattlebush is the herb of legume rattlebush.Summer, autumn collection.Alias manystem stonecrop leaf (《The Illustrated Book on Plants》), Leopard cat beans (《Botany voluminous dictionary》), the colored rattlebush of dog bell grass, indigo plant (《Chinese main plant figure says pulse family》), abelmosehus moschatus, wild sesame Numb, sesame jingle bell bell (《Zhejiang common herbal medicine among the people》), crotalaria seesiliflora (《Full exhibition a collection of selected materials tumour》).Former plant rattlebush is 1 year Raw upright draft, 20~100 centimetres high, the hair for being close to slightly grow, hair are slightly coarse.Dan Ye, linear or lanceolar, leaf blade size become Change is very big, and 2.5~8 centimetres long, wealthy 0.5~1 centimetre, the narrow point in both ends, apex usually has pencil hair, omits hair or a few nothings above Hair, drapes over one's shoulders mercerising matter hair below；Several no petioles；Stipule is superfine small, setiform.Raceme, basidixed or axillary, spend 2~20, Flower is intensive together.Bract and squamella are extremely similar, linear；Squamella is born in bennet top, is become mildewed by roughish；Flower Obstruct it is extremely short, as a result when it is sagging：Calyx grows 10~15 millimeters, close to be become mildewed by brown color, calyx tooth apex point；Corolla butterfly, hyacinthine Or it is light blue, about isometric with calyx, vexil is circular, and ala is short compared with vexil, and the square of falling ovate is circular, and fossil fragments are isometric with ala, interior It is curved, have beak；Stamen 10, monomer, 2 type of flower pesticide；Ovary stockless, style are elongated.Pod is hairless, oval, about isometric with calyx；Kind Son 10~15.Florescence September.It is born in the weeds of wasteland.It is distributed northeast, East China, south China and southwestern various regions.It is common in open country hundred Extract application and field of medicaments are closed, but its extract is applied to the antibacterial and mouldproof medical instruments field of medical bandage, is rarely had Report.
The content of the invention
The purpose of the present invention is to overcome above-mentioned the shortcomings of the prior art, there is provided an a kind of graphene oxide medical treatment is taut The preparation method of band.
To achieve the above object, the present invention uses following technical proposals：
A kind of preparation method of graphene oxide antibacterial and mouldproof medical bandage, this method include：By the antibacterial and mouldproof of preparation Agent is evenly distributed on gauze through spray processing, up to antibacterial and mouldproof medical bandage.
The antibacterial and mouldproof enzyme agent, with parts by weight, it includes：0.5-1.55 parts of nano graphene oxide, nano load metal 0.05-0.55 parts of graphene oxide, 1.3-9.5 parts of nano-calcium carbonate, 0.02-0.65 parts of compound of rattlebush extraction, poly- second two 1.0-5.5 parts of alcohol, 0.2-1.8 parts of polyvinylpyrrolidone, 50-120 parts of water.
The nano graphene oxide, its purity >=99%, lamellar spacing 0.5-2nm, lamella length are 500-900nm.
The carried metal of the nano load metal graphene oxide can be the one or more in silver, copper, palladium.
The structural formula of described rattlebush extraction compound is：
The preparation method of the rattlebush extraction compound, includes following operating procedure：(a) by the drying herb of rattlebush Crush, with 75~85% alcohol heat reflux extract, merge extracting solution, be concentrated into no alcohol taste, successively with petroleum ether, ethyl acetate and Water saturated extracting n-butyl alcohol, respectively obtains petroleum ether extract, acetic acid ethyl ester extract and n-butyl alcohol extract；(b) step (a) acetic acid ethyl ester extract is cleaned with macroreticular resin in, first with 10% ethanol elution, 8 column volumes, then with 75% ethanol elution 10 column volumes, collect 75% ethanol eluate, be concentrated under reduced pressure to obtain 75% ethanol elution thing medicinal extract；(c) 75% second in step (b) Alcohol elution medicinal extract is separated with purification on normal-phase silica gel, successively with dichloromethane-first that volume ratio is 85: 1,40: 1,20: 1,12: 1 and 1: 1 Alcohol gradient elution obtains 5 components；(d) component 4 is further separated with purification on normal-phase silica gel in step (c), is successively 20 with volume ratio: 1st, 12: 1 and 5: 1 methylene chloride-methanol gradient elution obtains 3 components；(e) component 2 uses octadecylsilane in step (d) The reverse phase silica gel separation of bonding, with the methanol aqueous solution isocratic elution that concentration expressed in percentage by volume is 70%, collects 8~10 column volumes Eluent, eluent, which is concentrated under reduced pressure, obtains rattlebush extraction compound.
The antibacterial and mouldproof enzyme agent preparation method, specifically includes following operating procedure：(a) under ul-trasonic irradiation, successively will Polyethylene glycol, polyvinylpyrrolidone and the nano-calcium carbonate of parts by weight are added to the water, ul-trasonic irradiation 25-75min, ultrasound Power：200-600W system temperatures：10-30℃；(2) room temperature mechanical stirring action, successively bears nano graphene oxide, nanometer Carry metal graphene oxide, rattlebush extraction compound is added in step (1) system, rotating speed：300-12000r/min, time： 10-50min。
The sprinkling ratio of the antibacterial mildew inhibitor is 0.5-3.5g/m2Gauze.
Beneficial effects of the present invention：(1) preparation process proposed by the invention is simple and easy to operate, without using chemicals and It is of low cost, reduce its production cycle, it is easy to accomplish industrial-scale production.
Medical bandage obtained by the present invention, due to the addition of nano graphene oxide, nano metal load oxidation stone at the same time Black alkene, rattlebush extract so that the medical bandage has antibacterial, mould proof, the functionality advantage such as eliminate the unusual smell, this is because oxidation stone Black alkene bactericidal property is remarkable, is the physics " antibiotic " of no drug resistance, graphene oxide not only can be by bacterial cell The insertion of film is cut, can also by cell membrane phospholipid molecule it is extensive directly extract, come destroy cell membrane from And bacterium is killed, it is superpower mutual that the two-dimensional structure of graphene uniqueness allows it to occur with the phospholipid molecule on bacterial cell membrane Effect, so as to cause a large amount of phospholipid molecules to depart from cell membrane；The rattlebush extract of the present invention is a kind of new compound, research It was found that it is extremely sensitive to bacterium particularly mould, nano graphene oxide, rattlebush extract and nano metal load oxygen Under the synergistic effect of graphite alkene, the effect that its antibacterial and mouldproof eliminates the unusual smell is considerably improved, its mould proof grade is 0 grade, to gold The bacteriostasis rate of staphylococcus aureus is 99.91%, and the bacteriostasis rate to Escherichia coli is 99.23%, to the antibacterial of helicobacter pylori Rate is 99.0%, the bacteriostasis rate 98% to Candida albicans, to be 100% to the bacteriostasis rate of mould.
(2) the mould proof gauze of spray antimicrobial, nano-particle are immersed in yarn, are strengthened yarn interior cohesiveness, are greatly reduced The generation of filoplume phenomenon, secondary insult when avoiding the patient from using.
Brief description of the drawings
Fig. 1 is compound (I) structural formula figure；
Fig. 2 is compound (I) theory ECD values figure compared with testing ECD values.
Embodiment
The essentiality content of the present invention is further illustrated with reference to embodiment, but present invention protection model is not limited with this Enclose.Although being explained in detail with reference to preferred embodiment to the present invention, it will be understood by those of ordinary skill in the art that, can be right Technical scheme technical scheme is modified or replaced equivalently, without departing from the spirit and scope of technical solution of the present invention.
Embodiment 1：
Rattlebush extraction compound separation prepares and structural identification：
Preparation method：(a) the drying herb (10kg) of rattlebush crushes, and (25L × 3 are extracted with 80% alcohol heat reflux It is secondary), merge extracting solution, be concentrated into no alcohol taste (3L), satisfied successively with petroleum ether (3L × 3 time), ethyl acetate (3L × 3 time) and water N-butanol (3L × 3 time) extraction of sum, respectively obtains petroleum ether extract, acetic acid ethyl ester extract (398g) and extracting n-butyl alcohol Thing；(b) acetic acid ethyl ester extract is cleaned with AB-8 types macroreticular resin in step (a), first with 10% ethanol elution, 8 column volumes, Again with 75% ethanol elution, 10 column volumes, 75% ethanol eluate is collected, be concentrated under reduced pressure to obtain 75% ethanol elution thing medicinal extract (163g)；(c) 75% ethanol elution medicinal extract is separated with 200-300 mesh purification on normal-phase silica gel in step (b), is successively 85: 1 with volume ratio (8 column volumes), 40: 1 (8 column volumes), 20: 1 (8 column volumes), 12: 1 (10 column volumes) and 1: 1 (5 column volumes) Methylene chloride-methanol gradient elution obtain 5 components；(d) component 4 (49g) 200-300 mesh purification on normal-phase silica gel in step (c) Further separation, successively with two that volume ratio is 20: 1 (8 column volumes), 12: 1 (10 column volumes) and 5: 1 (5 column volumes) Chloromethanes-methanol elution gradient obtains 3 components；(e) in step (d) component 2 (25g) be bonded with octadecylsilane it is anti-phase Silica gel ODS-C18 is separated, and with the methanol aqueous solution isocratic elution that concentration expressed in percentage by volume is 70%, is collected 8~10 column volumes and is washed De- liquid, eluent are concentrated under reduced pressure to give pure compound (I) (44mg).
Structural identification：Yellow amorphous powder；HR-ESIMS is shown [M+Na]+For m/z 549.2314, with reference to nuclear-magnetism feature It is C that molecular formula, which can be obtained,33H34O6, degree of unsaturation 17.Hydrogen nuclear magnetic resonance modal data δH(ppm, DMSO-d6, 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-OCH3(3.58, s), 2 "-OCH3 (3.52, s), 4 "-OCH3(3.62, s), 4 " '-OCH3(3.59, s)；Carbon-13 nmr spectra data δC(ppm, DMSO-d6, 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 (CH2, α '-C), 33.4 (CH2, 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 (CH3, 3-OCH3), 55.2 (CH3, 2 "-OCH3), 55.4 (CH3, 4 "-OCH3), 55.2 (CH3, 4 " '-OCH3)； Carbon atom is marked referring to Fig. 1.1H NMR and1H-1H COSY spectrums show two pairs of diprotons bimodal [δ H7.04 (2H, d, J= 8.2Hz), 6.64 (2H, d, J=8.2Hz), 7.04 (2H, d, J=8.2Hz), 6.64 (2H, d, J=8.2Hz)], show the change Compound contains two Isosorbide-5-Nitraes-di-substituted aryl ring.It was furthermore observed that the coupled signal δ H6.62 (1H, d, J=8.2Hz) of one group of ABX, 6.24 (1H, d, J=2.3Hz) and 6.14 (1H, dd, J=8.2,2.3Hz), show that the compound contains one 1,2,4- tri- and takes The aromatic ring in generation.Coupled signal δ H6.55 (1H, d, J=1.8Hz) and 6.33 (1H, d, J=1.8Hz), illustrate also to contain between another two There are 1,2,3, a 5- tetra- substituted aroma rings.Except aromatic protons, there are 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)], a methine signals [d4.45 (1H, br, s)] and four methoxyl group signals [δ H3.62,3.59,3.58, 3.52, (3H, s)].13C NMR and hsqc spectrum show the fragrant quaternary carbons of 11 consistent with hydrogen spectrum, including six oxygen-containing quaternary carbons, ten Three aromatic series methine carbons, three aliphatic methine carbons, two aliphatic mesomethylene carbons, four methoxyl group carbon.In HMBC spectrums, instead The correlation of formula alkene sp2 spin protons and p- hydroxy benzenes and four substituted benzene rings shows the compound for conjugation stilbenes compound 。1H-1H COSY Correlated Spectroscopies indicate the presence of aliphatic chain carbon signal C- α ', C- β ', C- γ ', H- α ' and aromatic series during HMBC is composed The correlation of carbon shows that C- α ' are connected with 2,4- Dimethoxyphenyls.H- γ ' signals and trans olefins unit and 3- in NOESY spectrums The correlation of methoxyl group -5- hydroxyl phenyl ring shows that above-mentioned talan unit is connected with C- γ '.Comprehensive hydrogen spectrum, carbon spectrum, HMBC Spectrum and NOESY spectrums, and document can determine the compound as shown in Figure 1, spatial configuration substantially on correlation type nuclear magnetic data Further tested and determined by ECD, theoretical value and experiment value are basically identical (Fig. 2).
Embodiment 2：
A kind of preparation method of graphene oxide antibacterial and mouldproof medical bandage, this method include：By the antibacterial and mouldproof of preparation Agent is evenly distributed on gauze through spray processing, up to antibacterial and mouldproof medical bandage.
The antibacterial and mouldproof enzyme agent, with parts by weight, it includes：0.5 part of nano graphene oxide, the oxidation of nano load metal 0.05 part of graphene, 1.3 parts of nano-calcium carbonate, 0.02 part of compound of rattlebush extraction, 1.0 parts of polyethylene glycol, polyvinyl pyrrole 0.2 part of alkanone, 50 parts of water.
The nano graphene oxide, its purity >=99%, lamellar spacing 0.5nm, lamella length are 500nm.
The carried metal of the nano load metal graphene oxide can be silver.
Described structural formula of rattlebush extraction compound and preparation method thereof, with embodiment 1.
The antibacterial and mouldproof enzyme agent preparation method, specifically includes following operating procedure：(a) under ul-trasonic irradiation, successively will Polyethylene glycol, polyvinylpyrrolidone and the nano-calcium carbonate of parts by weight are added to the water, ul-trasonic irradiation 25min, ultrasonic work( Rate：200W system temperatures：10℃；(2) room temperature mechanical stirring action, successively by nano graphene oxide, nano load metal oxygen Graphite alkene, rattlebush extraction compound are added in step (1) system, rotating speed：300r/min, time：50min.
The sprinkling ratio of the antibacterial mildew inhibitor is 0.5g/m2Gauze.
Through antibacterial test, the bacteriostasis rate to staphylococcus aureus is 99.91%, and the bacteriostasis rate to Escherichia coli is 99.23%, the bacteriostasis rate to helicobacter pylori is 99.0%, the bacteriostasis rate 98% to Candida albicans, for the antibacterial of mould Rate is 100%.
Embodiment 3：
A kind of preparation method of graphene oxide antibacterial and mouldproof medical bandage, this method include：By the antibacterial and mouldproof of preparation Agent is evenly distributed on gauze through spray processing, up to antibacterial and mouldproof medical bandage.
The antibacterial and mouldproof enzyme agent, with parts by weight, it includes：1.55 parts of nano graphene oxide, the oxidation of nano load metal 0.55 part of graphene, 9.5 parts of nano-calcium carbonate, 0.65 part of compound of rattlebush extraction, 5.5 parts of polyethylene glycol, polyvinyl pyrrole 1.8 parts of alkanone, 120 parts of water.
The nano graphene oxide, its purity >=99%, lamellar spacing 2nm, lamella length are 900nm.
The carried metal of the nano load metal graphene oxide can be copper.
Described structural formula of rattlebush extraction compound and preparation method thereof, with embodiment 1.
The antibacterial and mouldproof enzyme agent preparation method, specifically includes following operating procedure：(a) under ul-trasonic irradiation, successively will Polyethylene glycol, polyvinylpyrrolidone and the nano-calcium carbonate of parts by weight are added to the water, ul-trasonic irradiation 75min, ultrasonic work( Rate：600W system temperatures：30℃；(2) room temperature mechanical stirring action, successively by nano graphene oxide, nano load metal oxygen Graphite alkene, rattlebush extraction compound are added in step (1) system, rotating speed：12000r/min, time：10min.
The sprinkling ratio of the antibacterial mildew inhibitor is 3.5g/m2Gauze.
Through antibacterial test, the bacteriostasis rate to staphylococcus aureus is 99.95%, and the bacteriostasis rate to Escherichia coli is 99.98%, the bacteriostasis rate to helicobacter pylori is 99.23%, the bacteriostasis rate 99.12% to Candida albicans, for mould Bacteriostasis rate is 100%.
Embodiment 4：
A kind of preparation method of graphene oxide antibacterial and mouldproof medical bandage, this method include：By the antibacterial and mouldproof of preparation Agent is evenly distributed on gauze through spray processing, up to antibacterial and mouldproof medical bandage.
The antibacterial and mouldproof enzyme agent, with parts by weight, it includes：1.0 parts of nano graphene oxide, the oxidation of nano load metal 0.1 part of graphene, 1.8 parts of nano-calcium carbonate, 0.12 part of compound of rattlebush extraction, 1.8 parts of polyethylene glycol, polyvinylpyrrolidine 0.8 part of ketone, 40 parts of water.
The nano graphene oxide, its purity >=99%, lamellar spacing 1.0nm, lamella length are 600nm.
The carried metal of the nano load metal graphene oxide can be silver and palladium.
Described structural formula of rattlebush extraction compound and preparation method thereof, with embodiment 1.
The antibacterial and mouldproof enzyme agent preparation method, specifically includes following operating procedure：(a) under ul-trasonic irradiation, successively will Polyethylene glycol, polyvinylpyrrolidone and the nano-calcium carbonate of parts by weight are added to the water, ul-trasonic irradiation 45min, ultrasonic work( Rate：350W system temperatures：25℃；(2) room temperature mechanical stirring action, successively by nano graphene oxide, nano load metal oxygen Graphite alkene, rattlebush extraction compound are added in step (1) system, rotating speed：800r/min, time：15min.
The sprinkling ratio of the antibacterial mildew inhibitor is 1.5g/m2Gauze.
Through antibacterial test, the bacteriostasis rate to staphylococcus aureus is 99.99%, and the bacteriostasis rate to Escherichia coli is 99.98%, the bacteriostasis rate to helicobacter pylori is 99.95%, the bacteriostasis rate 99.98% to Candida albicans, for mould Bacteriostasis rate is 100%.
Embodiment 5：
A kind of preparation method of graphene oxide antibacterial and mouldproof medical bandage, this method include：By the antibacterial and mouldproof of preparation Agent is evenly distributed on gauze through spray processing, up to antibacterial and mouldproof medical bandage.
The antibacterial and mouldproof enzyme agent, with parts by weight, it includes：1.45 parts of nano graphene oxide, the oxidation of nano load metal 0.45 part of graphene, 8.5 parts of nano-calcium carbonate, 0.35 part of compound of rattlebush extraction, 4.5 parts of polyethylene glycol, polyvinyl pyrrole 1.3 parts of alkanone, 100 parts of water.
The nano graphene oxide, its purity >=99%, lamellar spacing 1.5nm, lamella length are 850nm.
The carried metal of the nano load metal graphene oxide can be silver, copper and palladium.
Described structural formula of rattlebush extraction compound and preparation method thereof, with embodiment 1.
The antibacterial and mouldproof enzyme agent preparation method, specifically includes following operating procedure：(a) under ul-trasonic irradiation, successively will Polyethylene glycol, polyvinylpyrrolidone and the nano-calcium carbonate of parts by weight are added to the water, ul-trasonic irradiation 65min, ultrasonic work( Rate：550W system temperatures：28℃；(2) room temperature mechanical stirring action, successively by nano graphene oxide, nano load metal oxygen Graphite alkene, rattlebush extraction compound are added in step (1) system, rotating speed：9000r/min, time：25min.
The sprinkling ratio of the antibacterial mildew inhibitor is 3.2g/m2Gauze.
Through antibacterial test, the bacteriostasis rate to staphylococcus aureus is 99.99%, and the bacteriostasis rate to Escherichia coli is 99.68%, the bacteriostasis rate to helicobacter pylori is 99.98%, the bacteriostasis rate 97% to Candida albicans, for the antibacterial of mould Rate is 100%.
Although the above-mentioned embodiment to the present invention is described, not to the limit of the scope of the present invention System, on the basis of technical scheme, those skilled in the art need not make the creative labor can make it is each Kind modification is deformed still within protection scope of the present invention.

Claims (6)

1. a kind of preparation method of graphene oxide antibacterial and mouldproof medical bandage, this method include：By the antibacterial mildew inhibitor of preparation It is evenly distributed on through spray processing on gauze, up to antibacterial and mouldproof medical bandage；The antibacterial mildew inhibitor, with its bag of parts by weight Include：0.5-1.55 parts of nano graphene oxide, 0.05-0.55 parts of nano load metal graphene oxide, nano-calcium carbonate 1.3- 9.5 parts, rattlebush extraction 0.02-0.65 parts of compound, 1.0-5.5 parts of polyethylene glycol, 0.2-1.8 parts of polyvinylpyrrolidone, 50-120 parts of water.
2. the preparation method of graphene oxide antibacterial and mouldproof medical bandage according to claim 1, it is characterised in that：It is described Nano graphene oxide, its purity >=99%, lamellar spacing 0.5-2nm, lamella length are 500-900nm.
3. the preparation method of graphene oxide antibacterial and mouldproof medical bandage according to claim 2, it is characterised in that：It is described The carried metal of nano load metal graphene oxide can be the one or more in silver, copper, palladium.
4. the preparation method of graphene oxide antibacterial and mouldproof medical bandage according to claim 1, it is characterised in that：It is described Rattlebush extraction compound structural formula be：
5. the preparation method of graphene oxide antibacterial and mouldproof medical bandage according to claim 1, it is characterised in that：It is described Antibacterial mildew inhibitor preparation method, specifically includes following operating procedure：(a) under ul-trasonic irradiation, successively by the poly- second two of parts by weight Alcohol, polyvinylpyrrolidone and nano-calcium carbonate are added to the water, ul-trasonic irradiation 25-75min, ultrasonic power：200-600W System temperature：10-30℃；(2) room temperature mechanical stirring action, successively by nano graphene oxide, nano load metal oxygen fossil Black alkene, rattlebush extraction compound are added in step (1) system, rotating speed：300-12000r/min, time：10-50min.
6. the preparation method of graphene oxide antibacterial and mouldproof medical bandage according to claim 1, it is characterised in that：It is described The sprinkling ratio of antibacterial mildew inhibitor is 0.5-3.5g/m2Gauze.
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