CN102860325A - Bactericidal nano-silver water gel and preparation method thereof - Google Patents
Bactericidal nano-silver water gel and preparation method thereof Download PDFInfo
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- CN102860325A CN102860325A CN2012103352319A CN201210335231A CN102860325A CN 102860325 A CN102860325 A CN 102860325A CN 2012103352319 A CN2012103352319 A CN 2012103352319A CN 201210335231 A CN201210335231 A CN 201210335231A CN 102860325 A CN102860325 A CN 102860325A
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Abstract
The invention discloses a bactericidal nano-silver water gel and a preparation method thereof. The preparation method includes the steps of:1, dissolving silver nitrate and cysteine which are taken as the raw materials in pure water to prepare cysteine-silver ion complex; and 2, taking the cysteine-silver ion complex as a precursor, reducing silver ions in a precursor solution to prepare nano silver sol through hydrated electrons and free radicals produced under the irradiation of ultraviolet light, wherein the cysteine acts with silver through sulfydryl to envelop the nano silver, and the amino of the cysteine and carboxylic acid serve as hydrophilic residues to capture hydrones so as to form water gel. In such a way, the nano-silver water gel can be prepared. Compared with the convention preparation methods of nano-silver water gel, the preparation method disclosed by the invention has the advantages that the method requires fewer raw materials, the preparation method is simple, and the water gel prepared through the method has good bactericidal effect, good stability and the like, and barely changes after exposure in air for a whole year.
Description
Technical field:
The invention belongs to the preparation method who relates to a kind of nanogel, be specifically related to that a kind of particle diameter is evenly distributed, the Nano Silver hydrogel of stability of characteristics and preparation method thereof.
Background technology:
Along with a large amount of uses of the chemicalses such as antibiotic, disinfectant and bactericide, more and more by the microbial variation population that drug resistance causes.Nano Silver is as inorganic antibacterial material, and the pathogenic microorganismss such as kill bacteria, fungi, mycoplasma have the incomparable antibacterial activity of other anti-biotic materials effectively.Nano Silver has broad-spectrum antibacterial property, high efficiency, effectiveness and lastingly, is not subjected to the advantages such as the pH value affects, safety and environmental protection, more and more is familiar with, and becomes desirable anti-biotic material.
Generally, hydrogel is to introduce a part of hydrophobic grouping and hydrophilic residue in the water soluble polymer of cross-linked network with having, and hydrophilic residue and water molecules are connected to netted inner formation with hydrone.Hydrogel mainly is by the hydrophilic macromolecule network system at present: comprise polysaccharose (starch, cellulose, alginic acid, hyaluronic acid, shitosan etc.), polypeptide class (collagen, polylysine, poly-L-GLU etc.) and synthesizing polyethylene, acrylic acid derivative (polyacrylic acid, polymethylacrylic acid, polyacrylamide, poly-N-is poly-for acrylamide etc.) consist of.
Owing to having good bio-compatibility and field of medicaments huge applications potentiality, proteins and peptides class hydrogel becomes study hotspot in recent years.Such as (Zohuriaan-Mehr, M.J., Pourjavadi, A., Salimi, H.﹠amp; Kurdtabar, M.Protein-and homo poly (amino acid)-based hydrogels with super-swelling properties.Polym Advan Technol, 2009,20,655-671.), (Seliktar, D.Designing Cell-Compatible Hydrogels for Biomedical Applications.Science, 2012,336,1124-1128.) etc. many pieces of papers are studying and are summing up proteins and peptides in great detail and forming the condition of hydrogel.In recent years, scientists is by simplifying and optimize polypeptide structure, the non-covalent hydrogel that the dipeptides that connected by oligopeptides even two amino acid has been prepared, and be applied to the field such as in-vitro antibacterial medicine controllable release.(Salick，D.A.，Kretsinger，J.K.，Pochan，D.J.&Schneider，J.P.Inherent?antibacterial?activity?of?a?peptide-based?beta-hairpin?hydrogel.J?Am?Chem?Soc，2007，129，14793-14799.)、(Liang，G.L.et?al.Supramolecular?Hydrogel?of?a?D-Amino?Acid?Dipeptide?for?Controlled?Drug?Release?in?Vivo.Langmuir，2009，25，8419-8422.)、(Ryan，D.M.&Nilsson，B.L.Self-assembled?amino?acids?and?dipeptides?as?noncovalent?hydrogels?for?tissue?engineering.Polym?Chem-Uk.2012，3，18-33.)。Scientist is also arranged at the structure condition of constantly exploring the dipeptides hydrogel, such as (Pasc, A., Akong, F.O., Cosgun, S.﹠amp simultaneously; Gerardin, C.Differences between beta-Ala and Gly-Gly in the design of amino acids-based hydrogels.Beilstein J Org Chem, 2010,6,973-977.), (Johnson, E.K., Adams, D.J.﹠amp; Cameron, P.J.Directed Self-Assembly of Dipeptides to Form Ultrathin Hydrogel Membranes.J Am Chem Soc, 2010,132,5130-5136.).
The preparation of the Nano Silver of broad-spectrum antiseptic is become hydrogel will have broad application prospects at field of medicaments.Can find out from the patent of invention of the present world and the domestic research paper of delivering and application, elementary tactics is that elder generation's reduction silver ion under the high-temperature liquid-phase condition prepares nano-Ag particles, then synthetic Nano Silver is added in the polymeric gel agent that can prepare hydrogel, as: (Roy, S.﹠amp; Banerjee, A.Amino acid based smart hydrogel:formation, characterization and fluorescence properties of silver nanoclusters within the hydrogel matrix.Soft Matter, 2011,7,5300-5308.), (Shen, J.S.﹠amp; Xu, B.In situ encapsulating silver nanocrystals into hydrogels.A " green " signaling platform for thiol-containing amino acids or small peptides.Chem Commun, 2011,47,2577-2579.), (" chitosan nano silver hydrogel adhesive and application thereof ", 200810016256.6) and (" a kind of nanometer Ag antibiotic gent for women and preparation method thereof ", number of patent application 200810123375.1) etc. number of patent application is:.Above method needs multistep synthetic, need to add a large amount of reductants, stabilizing agent, polymeric gel agent etc. when making, and has increased manufacture craft, raw material and cost.
Summary of the invention:
Patent of the present invention is for the deficiencies in the prior art, provides a kind of and adopts that raw material is few, manufacture craft simple, good antimicrobial effect and the micelle footpath narrow distribution range that makes, uniform Nano Silver hydrogel and preparation method thereof.
To achieve these goals, patent making step of the present invention is as follows:
The first step: prepare cysteine-silver ion complex in the pure water as raw material is dissolved in take silver nitrate and cysteine;
Second step: as precursor, utilize in hydrated electron that ultraviolet light irradiation produces and the radical pair precursor solution silver ion to reduce the preparation nano silver colloidal sol this complex solution; Cysteine is used for being coated with Nano Silver by sulfydryl and silver; The amino of cysteine and carboxylic acid form hydrogel as hydrophilic residue network hydrone, thereby make the Nano Silver hydrogel.
Described cysteine comprises a kind of among both of D type, L-type, and perhaps D type and L-type mixes.
The concentration conditions of described formation hydrogel is the 0.1%-0.15% that the cysteine quality accounts for the hydrogel gross mass.
The molar concentration rate of described silver nitrate and cysteine is 1.5: 1.
Described ultraviolet light, preferred 100 watts of high voltage mercury lamp irradiations.
Described exposure time is 2.5h.
Patent of the present invention is compared with existing Nano Silver hydrogel preparation method, has the following advantages:
(1) raw materials is few: cysteine is used as the complexing agent of silver ion in the precursor solution in the present invention; The sulfydryl that silver ion is reduced rear cysteine is combined with Nano Silver as the stabilizing agent of Nano Silver; The hydrophilic amino of cysteine and carboxyl are as the bond of network hydrone in the gelation process.
(2) preparation method is simple: preparation only needs uviol lamp get final product, and equipment less demanding easily realized production in enormous quantities.
(3) good antimicrobial effect, good stability: the Nano Silver particle size distribution range that makes is narrow, even, and regular shape is spheroidal; The Nano Silver hydrogel exposes 1 year without significant change in air, antibacterial consumption is few, good antimicrobial effect.
The solution generation had reproducibility under the present invention utilized and shines under the ultraviolet light
OH, H and secondary free radical become silver atoms with silver ion reduction, namely
The preparation Nano Silver; Utilization has three functions group (SH ,-NH
2The cysteine of ,-COOH) utilizes it-the interactional function nano-Ag particles of SH and noble silver; Utilization-NH
2The hydrogen bond network lock water that forms with-COOH forms hydrogel.Patent of the present invention has and adopts that raw material is few, productive rate is high, energy consumption is little, pollution-free, simple operation and other advantages.
Description of drawings:
Fig. 1 is transmission electron microscope (TEM) photo of the Nano Silver hydrogel that makes.
Fig. 2 is energy dispersive X ray (EDX) spectrogram of the Nano Silver that makes.
Fig. 3 is X-ray diffraction (XRD) figure of the Nano Silver that makes.
Fig. 4 is fourier infrared (FTIR) comparison diagram of cysteine and cysteine stabilized nanoscale silver.
Fig. 5 Nano Silver hydrogel is to the antibacterial figure of Escherichia coli (E.coli) with staphylococcus aureus (S.aureus).
Fig. 6 Nano Silver hydrogel is to the growth inhibition curve of Escherichia coli and staphylococcus aureus.
Embodiment:
Below in conjunction with specific embodiment, further set forth the present invention.
Embodiment 1:
At ambient temperature, the 0.12g cysteine is dissolved in the 100mL distilled water, forming molar concentration is the cysteine solution of 0.01mol/L; The 0.17g silver nitrate is dissolved in the 10mL distilled water, and forming molar concentration is the liquor argenti nitratis ophthalmicus of 0.1mol/L; Get 10mL cysteine solution and the 1.5mL liquor argenti nitratis ophthalmicus mixes, making its mol ratio is 1: 1.5.Mixed solution is placed on 100W under ballast fluorescent high-voltage mercury, shines 2.5h, thereby make the Nano Silver hydrogel.
Embodiment 2:
The present embodiment is the structural characterization to the antibacterial material of silver nanoparticle among the embodiment 1, specific as follows: adopt the shape and element composition of silver nano-grain in the Tecnai G2 F20 S-Twin 200 KV field transmission determination of electron microscopy Nano Silver hydrogels to characterize, result such as TEM photo (accompanying drawing 1) and EDX can spectrograms (accompanying drawing 2).Sample preparation is that the Nano Silver hydrogel is dissolved in the ultra-pure water, is dispersed on the TEM copper mesh after the absolute ethyl alcohol precipitation.Can be found out by TEM figure, the particle diameter of Nano Silver is between 5-10nm, and particle size is more even, mainly contains Ag, S, C, four kinds of elements of O in the sample.The 2 θ values that X-ray diffraction (accompanying drawing 3) records the characteristic diffraction peak of sample are followed successively by 38.2 °, 44.4 °, 64.5 °, 77.5 °, the diffraction crystal face that shows is respectively (111), (200), (220) and (311) and standard crystalline state silver card sheet (PDF#04-0783) contrast, the diffraction peak energy of the diffraction maximum that records and standard diagram is well coincide, and illustrates that prepared sample is Nano silver grain.Fourier transform infrared spectroscopy (accompanying drawing 4) is measured and is obtained containing in the Nano Silver hydrogel Cys major function group.
Embodiment 3:
The present embodiment is selected be bacillus coli and staphylococcus aureus as the representative of Gram-negative bacteria and positive bacteria, embodiment 1 has been carried out the test (accompanying drawing 5) of biocidal property.
The operating procedure of inhibition zone test is as follows: pour in the sterilized culture dish after the sterilization of LB Solid agar culture is dissolved, after the medium cooled and solidified, adding respectively 2mL concentration is 1 * 10
6Then the bacterium liquid of CFU/mL with aseptic spreading rod with its coating evenly, use aseptic nipper gripping Oxford cup again, is placed on gently dull and stereotyped centre, then it left standstill for a moment, can be fixed on the flat board.And then the Nano Silver hydrogel solution that pipettes 2mL joins in the cup of Oxford, and with sterile water as blank, every kind of thalline is done three Duplicate Samples.Medium as for cultivating 24h in 37 ℃ the incubator, is then measured respectively the diameter of inhibition zone with ruler, then average.The fungistatic effect of Nano Silver hydrogel as shown in Figure 5, result of the test such as table 1.
Table 1 Nano Silver hydrogel inhibition zone result of the test
Embodiment 4:
The minimal inhibitory concentration of Nano Silver hydrogel (MIC) and minimal bactericidal concentration (MBC) test: adopt doubling dilution and plating method to measure respectively the Nano Silver hydrogel to minimal inhibitory concentration and the minimal bactericidal concentration (accompanying drawing 6) of bacillus coli and staphylococcus aureus, concrete process of the test is as follows:
(1) minimal inhibitory concentration: get 10 sterilized test tubes, each pipe adds LB liquid nutrient medium 2mL, then adds the Nano Silver hydrogel solution 2mL of 0.70mg/mL (being 0.05mol/L) to the 1st pipe, draws 2mL behind the mixing and joins in the 2nd pipe.By that analogy, be diluted to the 9th pipe according to the method always, then abandon it with drawing 2mL in the 9th pipe, the 10th pipe adds the sterile water of 2mL as the blank group in the test tube, behind the mixing, draw 2mL, abandons it.In above-mentioned 10 test tubes, add respectively the bacillus coli suspension 0.2mL that concentration is 1 * 106CFU/mL, after shaking up, place 37 ℃ of constant incubators to cultivate 24 hours, then visually observe the result.Concentration concentration minimum and the obviously not muddy contained Nano Silver hydrogel of test tube is the minimal inhibitory concentration of this antibacterial material.Result of the test is as shown in table 2.
The minimal inhibitory concentration result of the test of table 2 Nano Silver hydrogel
As shown in Table 2, the Nano Silver hydrogel to the minimal inhibitory concentration of bacillus coli and staphylococcus aureus is: 43.75mg/L.
(2) minimal bactericidal concentration: utilize and measure above each tube culture of minimum inhibitory concentration, draw respectively 0.1mL and be coated on the sterilized LB agar medium, cultivate 24h in 37 ℃ constant incubator, the result then detects by an unaided eye.Minimum and the clump count of Nano Silver hydrogel solution consumption is less than the minimal bactericidal concentration that 5 the corresponding silver nanoparticle solution concentration of culture medium flat plate is this material.Result of the test is as shown in table 3.
The Minimum Bactericidal result of table 3 Nano Silver hydrogel
As shown in Table 3, the Nano Silver hydrogel is 350mg/L to the minimal bactericidal concentration of bacillus coli and staphylococcus aureus.
Above result shows, patent Nano Silver hydrogel of the present invention has very strong restraining and sterilizing bacteria ability, and all can produce significant inhibitory action to common gram-positive bacteria and negative bacterium; When the concentration of Nano Silver hydrogel reaches 0.35mg/mL, can kill most common bacteriums.
Claims (6)
1. sterilization Nano Silver hydrogel and preparation method thereof, it is characterized in that: making step is as follows
The first step: prepare cysteine-silver ion complex in the pure water as raw material is dissolved in take silver nitrate and cysteine;
Second step: as precursor, utilize in hydrated electron that ultraviolet light irradiation produces and the radical pair precursor solution silver ion to reduce the preparation nano silver colloidal sol this complex solution; Cysteine is used for being coated with Nano Silver by sulfydryl and silver; The amino of cysteine and carboxylic acid form hydrogel as hydrophilic residue network hydrone, thereby make the Nano Silver hydrogel.
2. a kind of sterilization Nano Silver hydrogel according to claim 1 and preparation method thereof is characterized in that: described cysteine comprises a kind of among both of D type, L-type, and perhaps D type and L-type mixes.
3. a kind of sterilization Nano Silver hydrogel according to claim 1 and preparation method thereof, it is characterized in that: the concentration conditions of described formation hydrogel is the 0.1%-0.15% that the cysteine quality accounts for the hydrogel gross mass.
4. a kind of sterilization Nano Silver hydrogel according to claim 1 and preparation method thereof, it is characterized in that: the molar concentration rate of described silver nitrate and cysteine is 1.5: 1.
5. a kind of sterilization Nano Silver hydrogel according to claim 1 and preparation method thereof is characterized in that: described ultraviolet light, preferred 100 watts of high voltage mercury lamp irradiations.
6. a kind of sterilization Nano Silver hydrogel according to claim 1 and preparation method thereof, it is characterized in that: described exposure time is 2.5h.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103125524A (en) * | 2013-01-10 | 2013-06-05 | 遵义市大丰农作物研究所 | High-efficiency nano-silver sterilizing agents without selection of media and environment and preparing method thereof |
| CN103302305A (en) * | 2013-06-09 | 2013-09-18 | 佛山市天宝利太阳能科技有限公司 | Method for preparing silver nanowires by using biomolecular amino acid as reducing agent |
| CN103461382A (en) * | 2013-08-08 | 2013-12-25 | 广东药学院 | Silver-loading modified montmorillonite antibacterial agent, preparation method and application thereof |
| CN103822889A (en) * | 2014-01-15 | 2014-05-28 | 江南大学 | Colorimetric detection method for Cl<->, Br<-> and I<-> based on silver nano-cluster hydrogel |
| CN104772469A (en) * | 2015-01-12 | 2015-07-15 | 江南大学 | Method for quickly preparing silver nanoparticles through microwave irradiation |
| CN107522875A (en) * | 2016-06-20 | 2017-12-29 | 中国科学院宁波材料技术与工程研究所 | Hydrogel, its preparation method and the application of Nano silver grain crosslinking |
| CN107823142A (en) * | 2017-10-31 | 2018-03-23 | 河南大学 | A kind of Janus structural polyethers/Ag particles and its preparation method and application |
| CN109054402A (en) * | 2018-07-20 | 2018-12-21 | 湖南工业大学 | A kind of preparation method and applications of flexibility gelatin/nano conducting powders composite material |
| CN112006978A (en) * | 2020-09-09 | 2020-12-01 | 大连民族大学 | Targeted chitosan nano-silver gel and preparation method and application thereof |
| US11291203B2 (en) * | 2019-08-20 | 2022-04-05 | Lawrence Livermore National Security, Llc | Soluble metallogels including antimicrobial silver metallogels |
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Cited By (16)
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| CN103125524A (en) * | 2013-01-10 | 2013-06-05 | 遵义市大丰农作物研究所 | High-efficiency nano-silver sterilizing agents without selection of media and environment and preparing method thereof |
| CN103125524B (en) * | 2013-01-10 | 2016-12-28 | 遵义市大丰农作物研究所 | Efficient nano silver antibacterial not selecting medium and environment and preparation method thereof |
| CN103302305A (en) * | 2013-06-09 | 2013-09-18 | 佛山市天宝利太阳能科技有限公司 | Method for preparing silver nanowires by using biomolecular amino acid as reducing agent |
| CN103302305B (en) * | 2013-06-09 | 2016-01-27 | 佛山市天宝利硅工程科技有限公司 | A kind of biomolecule amino acid that utilizes prepares the method for nano silver wire for reducing agent |
| CN103461382A (en) * | 2013-08-08 | 2013-12-25 | 广东药学院 | Silver-loading modified montmorillonite antibacterial agent, preparation method and application thereof |
| CN103461382B (en) * | 2013-08-08 | 2015-07-01 | 广东药学院 | Silver-loading modified montmorillonite antibacterial agent, preparation method and application thereof |
| CN103822889A (en) * | 2014-01-15 | 2014-05-28 | 江南大学 | Colorimetric detection method for Cl<->, Br<-> and I<-> based on silver nano-cluster hydrogel |
| CN104772469A (en) * | 2015-01-12 | 2015-07-15 | 江南大学 | Method for quickly preparing silver nanoparticles through microwave irradiation |
| CN107522875A (en) * | 2016-06-20 | 2017-12-29 | 中国科学院宁波材料技术与工程研究所 | Hydrogel, its preparation method and the application of Nano silver grain crosslinking |
| CN107823142A (en) * | 2017-10-31 | 2018-03-23 | 河南大学 | A kind of Janus structural polyethers/Ag particles and its preparation method and application |
| CN107823142B (en) * | 2017-10-31 | 2020-08-18 | 河南大学 | Janus structure polyether/Ag particle and preparation method and application thereof |
| CN109054402A (en) * | 2018-07-20 | 2018-12-21 | 湖南工业大学 | A kind of preparation method and applications of flexibility gelatin/nano conducting powders composite material |
| CN109054402B (en) * | 2018-07-20 | 2021-06-25 | 湖南工业大学 | Preparation method and application of flexible gelatin/nano conductive particle composite material |
| US11291203B2 (en) * | 2019-08-20 | 2022-04-05 | Lawrence Livermore National Security, Llc | Soluble metallogels including antimicrobial silver metallogels |
| CN112006978A (en) * | 2020-09-09 | 2020-12-01 | 大连民族大学 | Targeted chitosan nano-silver gel and preparation method and application thereof |
| CN112006978B (en) * | 2020-09-09 | 2023-04-28 | 大连民族大学 | Targeting chitosan nano silver gel and preparation method and application thereof |
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Application publication date: 20130109 |