CN101130085A - Nano montmorillonite for restraining bacterium and method of preparing the same - Google Patents
Nano montmorillonite for restraining bacterium and method of preparing the same Download PDFInfo
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- CN101130085A CN101130085A CNA2007101377683A CN200710137768A CN101130085A CN 101130085 A CN101130085 A CN 101130085A CN A2007101377683 A CNA2007101377683 A CN A2007101377683A CN 200710137768 A CN200710137768 A CN 200710137768A CN 101130085 A CN101130085 A CN 101130085A
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Abstract
The invention provides nano bacterium-resisting montmorillonite, which comprises montmorillonite 100 weight parts and antibacterial drugs 10-45 weight parts. The preparing process comprises steps of mixing Na-montmorillonite and antibacterial drugs, charging solvent and stirring, forming stable suspension, filtering, removing the solvent, finally drying and ball-grinding.
Description
The applying date of original application is 2005.9.27, and application number is 200510037525.3, and denomination of invention is inflammation-resistant modified imvite and preparation method thereof
Technical field
The present invention relates to a kind of medicinal preparation, be specifically related to infection material modified montmorillonoid and preparation method thereof.
Background technology
Montorillonite clay (Montmorillonite) claim bentonite again, is a kind of phyllosilicate, and its molecule space has bigger hole, and its construction unit is by two silicon-oxy tetrahedrons, and silica of sandwich is octahedra to be constituted, and its chemical formula is (M+nH
2O) (Al
4-yMgy) Si
8O
20(OH)
4(M=Na wherein
+, Ca
2+, Mg
2+Or the like), its structure lamella is a nanoscale, about 1 nanometer of elementary layer spacing is wherein carried out exchange reaction with inorganic, alkyl quaternary ammonium salts or other organic cations and neutral molecule easily and is generated organo montmorillonite.
One piece of paper that is entitled as " preparation of organo montmorillonite and structural characterization thereof " of Wang Ke etc. page has been published in " Beijing Institute of Technology's journal " the 22nd volume the 2nd phase 2002.4.P240～241, the cation exchange capacity that discloses the various nano imvites that form after the modification in this article is different, more helps carrying out organically-modified to montorillonite clay.There is researcher Xi Li to fly to add the stirring of 0.2g montorillonite clay powder in the NaOH aqueous solution of 20ml 0.1ml/l down again, at room temperature stirred 1 hour, standing over night, ultra-sonic dispersion takes by weighing 0.36g acyclovir powder again and puts in the 60ml montmorillonite suspension liquid reaction and make acyclovir/montorillonite clay slow-releasing system (" medicine/preparation of montorillonite clay slow-releasing system and the research of release in vitro " Xi Li fly to the sky Tianjin college of materials science and engineering 2004.1.P16 of university～29).Researcher Xi Li flies the slow release of obtained acyclovir/montorillonite clay slow-releasing system by montorillonite clay control acyclovir, and has certain directionality, thereby has improved bioavailability of medicament.Just as described herein, the intercalation of acyclovir and montorillonite clay is actually cation in drug molecule and the montmorillonite layer (as Na
+, Mg
2+And Ca
2+) exchange, and be inserted in the montmorillonite layer to form modes such as hydrogen bond, coordinate bond or complexation.Yet the infection material is of a great variety, the chemical constitution of every kind of medicine, character are all different, be not that all anti-infectives can both insert and anchor in the lamella of montorillonite clay, therefore can't fly disclosed technical scheme by Xi Li knows antibacterials/montorillonite clay slow-releasing system by inference, more can't predict its technique effect.
Summary of the invention
The object of the present invention is to provide a kind of nano montmorillonite for restraining bacterium.
Another object of the present invention provides a kind of preparation method of nano montmorillonite for restraining bacterium.
Nano montmorillonite for restraining bacterium of the present invention is made up of the component of following mass parts:
Na-montorillonite clay: 100;
Antibacterial medicines: 10～45;
Wherein, described antibacterial medicines is: tetracycline or doxycycline.
Montorillonite clay of the present invention is the Na-montorillonite clay.The Na-montorillonite clay can prepare with following method: the raw material montorillonite clay (is mainly contained Na
+, Ca
2+, Mg
2+Ion) stirs in 10 parts of saturated deionized water solutions of the NaCl at 100～300 parts, form steady suspension; Suspension stirred 5～6 hours down at 30～40 ℃; Sucking filtration is filtered thing with deionized water wash then; To constant weight, ball milling to particle diameter is 20～30 μ m to the filter thing, promptly obtains the Na-montorillonite clay at 70 ℃ of following vacuum dryings.
Antibacterial medicines of the present invention is for medically using antibacterial medicines always.Antibacterial medicines of the present invention can be antifungal such as miconazole nitrate, econazole nitrate; Can be aminoglycosides antibacterial medicines such as amikacin sulfate, gentamycin; Can be Tetracyclines antibacterial medicines such as tetracycline, doxycycline; Can also be quinolione antibiotics and chlorhexidine acetate, rifampicin.Antibacterial medicines used in the present invention preferably miconazole nitrate, chlorhexidine acetate, tetracycline, amikacin sulfate wherein one or more.Preferably 20～45 parts of antibacterial medicines consumptions of the present invention (mass parts/100 mass parts Na-montorillonite clays).
Nano montmorillonite for restraining bacterium preparation method of the present invention be under solution condition with the antibacterial medicines intercalation in montorillonite clay, modification is carried out in montorillonite clay.
Nano montmorillonite for restraining bacterium preparation method of the present invention may further comprise the steps:
Na-montorillonite clay and antibacterial medicines are mixed, Na-montorillonite clay quality=5: 1～20: 1) or deionized water (deionized water quality: Na-montorillonite clay quality=5: 1～20: 1) or chloroform (chloroform quality: Na-montorillonite clay quality=5: 1～20: 1) stir and form stable suspension add dehydrated alcohol (dehydrated alcohol quality:, at room temperature (or constant temperature 40 ℃) stirred 2～6 hours, filter, remove dehydrated alcohol or deionized water or chloroform; With dehydrated alcohol or deionized water or chloroform washing filter thing, dry, ball milling obtain the nano montmorillonite for restraining bacterium that particle diameter is 20～30 μ m then.
In the nano montmorillonite for restraining bacterium preparation method of the present invention, the intercalation modifying time better is 3～5 hours behind the adding antibacterial medicines, preferably 4 hours.
In the nano montmorillonite for restraining bacterium preparation method of the present invention, form dehydrated alcohol or the deionized water or the chloroform quality of suspension with the Na-montorillonite clay: the Na-montorillonite clay is best in quality to be 8: 1.
For a better understanding of the present invention, the infection of following description of test nano montmorillonite for restraining bacterium of the present invention, slow releasing effect.
1, the slow releasing effect of antibacterial medicines in the nano montmorillonite for restraining bacterium
3 parts of the nano montmorillonite for restraining bacterium of quality such as take by weighing,, be suspended in 0.9% normal saline (perhaps coordinative solvent), soak 2h with the filter paper parcel, 6h, 12h, 24h, 48h, 72h ... take out, with ultraviolet spectrophotometer test antibacterial medicines release time be 2～48 hours.
The slow release result of table 1 UV spectrophotometer measuring miconazole nanometer
| Time (h) | 2 | 6 | 12 | 24 | 48 |
| Miconazole release concentration (mg/ml) miconazole burst size (mg) | 0.15 1.5 | 0.23 2.3 | 0.38 2.8 | 0.30 3.0 | 0.35 3.5 |
2, the fungistatic effect of nano montmorillonite for restraining bacterium
On different MH culture medium, inoculate escherichia coli, staphylococcus aureus, Candida albicans respectively.On the MH culture medium, beat the hole of 2mm diameter according to the sterile working, the nano montmorillonite for restraining bacterium of quality such as precision takes by weighing and the powder of montorillonite clay (in contrast), click and enter respectively in the hole of MH culture medium, in incubator 37 ℃ cultivate 24h after, observe the bacterial growth situation, parallel test 3 times is write down its antibacterial ring size respectively, calculating mean value.
The biocidal property effect of table 2 nano montmorillonite for restraining bacterium
| The montorillonite clay kind | Colibacillary antibacterial ring size (mm) | The antibacterial ring size of staphylococcus aureus (mm) | The antibacterial ring size of Candida albicans (mm) |
| MMT | 0 | 0 | 0 |
| Miconazole nitrate/MMT | 0 | 18±2.34 | 26±1.38 |
| Tetracycline/miconazole/MMT | 20±3.45 | 23±1.66 | 22±1.89 |
| Tetracycline/MMT | 21±4.01 | 14±1.00 | 0 |
| Amikacin sulfate/MMT | 22±4.89 | 17±4.55 | 0 |
3. the miconazole nano imvite is to the adsorption of antibacterial
Get conical flask and add a certain amount of miconazole nano imvite, the Na-montorillonite clay adds a certain amount of Escherichia coli bacteria liquid respectively again as blank, jolting 20 minutes, leave standstill after 6 hours and draw supernatant, behind the doubling dilution on the MH culture medium viable bacteria plate count, calculate average clump count.Be calculated as follows both adsorption rates: adsorption rate=(bacterial concentration in bacterial concentration in the 1-developmental tube supernatant/blank pipe supernatant) * 100% to the escherichia coli growth.
Table 3MMT and nanometer miconazole/MMT are to colibacillary absorption
| Group | Supernatant bacterium amount (cfu/ml) | Adsorption rate (%) |
| Control tube MMT narrows health azoles/MMT | 5.60×10 4 2.16×10 4 0.25×10 4 | 61.4 87.7 |
The result: experimental results show that Na-montorillonite clay, the montorillonite clay of nanometer miconazole do not have biocidal property to escherichia coli, the montorillonite clay of nanometer miconazole to the adsorption rate of antibacterial apparently higher than the Na-montorillonite clay to the antibacterial adsorption rate.
Use the antibacterial medicines modified montmorillonoid, with the antibacterial medicines intercalation in montorillonite clay.The Na-montorillonite clay is as the antibacterial medicines carrier, and the slow release of control antibacterial medicines by the absorption of antibacterial medicines modified Nano montorillonite clay to antibacterial, increases local drug concentration simultaneously, strengthens the anti-infective action effect.In addition, antibacterial medicines is released gradually, reduces the side effect of antibacterial medicines to human body.
Description of drawings
Fig. 1 is the XRD figure of montorillonite clay.Curve 1 is the XRD figure of Na-montorillonite clay among the figure; Curve 2 is XRD figure of amikacin sulfate modified montmorillonoid; Curve 3 is XRD figure of miconazole modified montmorillonoid; Curve 4 is XRD figure of tetracycline modified montmorillonoid; Curve 5 is XRD figure of hibitane modified montmorillonoid.
Fig. 2 is the infrared spectrogram of montorillonite clay.Curve 1 is the infrared spectrogram of Na-montorillonite clay among the figure: curve 2 is infrared spectrograms of amikacin sulfate modified montmorillonoid; Curve 3 is infrared spectrograms of miconazole modified montmorillonoid; Curve 4 is infrared spectrograms of tetracycline modified montmorillonoid; Curve 5 is infrared spectrograms of hibitane modified montmorillonoid.
Fig. 3 is the inhibition escherichia coli grown cultures result of montorillonite clay.1,2,3,4,5 is respectively hibitane modified montmorillonoid, amikacin sulfate modified montmorillonoid, tetracycline modified montmorillonoid, rifampicin modified montmorillonoid, montorillonite clay bacteria growing inhibiting cultivation results among the figure.
The specific embodiment
Following examples make those skilled in the art more fully understand the present invention, but do not limit the present invention in any way.
Embodiment 1
1. preparation Na-montorillonite clay: the raw material montorillonite clay (is mainly contained Na
+, Ca
2+, Mg
2+Ion) 20g stirs in the saturated deionized water solution of 500mL NaCl, forms steady suspension; Suspension stirred 5 hours down at 35 ℃.Sucking filtration is used the deionized water wash filtrate 4 times then.Be deposited in 70 ℃ of following vacuum dryings to constant weight, ball milling to particle diameter is 20～30 μ m, promptly obtains Na-montorillonite clay (its XRD figure is seen Fig. 1, and its infrared spectrum is seen Fig. 2).
2. preparation miconazole nitrate modification Na-montorillonite clay: get above-mentioned gained Na-montorillonite clay 10g and mix with the 6g miconazole nitrate, adding dehydrated alcohol 200ml is with mixed liquor stirring reaction 5 hours at room temperature.Sucking filtration uses the absolute ethanol washing filtrate for several times then, and the UV spectrophotometer measuring filtrate does not have miconazole nitrate, is deposited in 60 ℃ of following vacuum dryings to constant weight, and ball milling to particle diameter is 20-30 μ m, promptly gets the miconazole nitrate modified montmorillonoid.Collect all filtrates,, get an amount of filtrate and use Biomat-5 type ultraviolet spectrophotometer mensuration ultraviolet light light absorption value, calculate residual drug 4.8g with the filtering with microporous membrane of 0.45um.Be miconazole nitrate at 10g Na-montmorillonite intercalation 1.2g, confirmed that with XRD test and IR test and ultraviolet spectrometry gravimetric analysis 20% miconazole nitrate inserts between montmorillonite layer.
Embodiment 2
1. preparation Na-montorillonite clay: with embodiment 1.
2. preparation miconazole nitrate modification Na-montorillonite clay: get above-mentioned gained Na-montorillonite clay 10g and mix with the 8g miconazole nitrate, adding dehydrated alcohol 200ml is with mixed liquor stirring reaction 2 hours at room temperature.Sucking filtration uses the absolute ethanol washing filtrate for several times then, and the UV spectrophotometer measuring filtrate does not have miconazole nitrate, is deposited in 60 ℃ of following vacuum dryings to constant weight, and ball milling to particle diameter is 20-30 μ m, promptly gets the miconazole nitrate modified montmorillonoid.Collect all filtrates,, get an amount of filtrate and use Biomat-5 type ultraviolet spectrophotometer mensuration ultraviolet light light absorption value, calculate residual drug 6g with the filtering with microporous membrane of 0.45um.Be miconazole nitrate at 10g Na-montmorillonite intercalation 2g, confirmed 25% miconazole nitrate insertion montmorillonite-based nano sheet interlayer with XRD test and IR test and ultraviolet spectrometry gravimetric analysis.
Embodiment 3
1. preparation Na-montorillonite clay: with embodiment 1.
2. preparation miconazole nitrate modification Na-montorillonite clay: get above-mentioned gained Na-montorillonite clay 10g and mix with 10g nitric acid flavor health azoles, adding dehydrated alcohol 200ml is with mixed liquor stirring reaction 5 hours at room temperature.Sucking filtration uses the absolute ethanol washing filtrate for several times then, and the UV spectrophotometer measuring filtrate does not have miconazole nitrate, is deposited in 60 ℃ of following vacuum dryings to constant weight, and ball milling to particle diameter is 20-30 μ m, promptly gets the miconazole nitrate modified montmorillonoid.Collect all filtrates,, get an amount of filtrate and use Biomat-5 type ultraviolet spectrophotometer mensuration ultraviolet light light absorption value, calculate residual drug 6g with the filtering with microporous membrane of 0.45um.Be miconazole nitrate at 10g Na-montmorillonite intercalation 4g, confirmed 40% miconazole nitrate insertion montmorillonite-based nano sheet interlayer with XRD test and IR test and ultraviolet spectrometry gravimetric analysis.
Embodiment 4
1. preparation Na-montorillonite clay: with embodiment 1.
2. preparation chlorhexidine acetate modification Na-montorillonite clay: get 10g Na-montorillonite clay and mix with the 4g chlorhexidine acetate, adding dehydrated alcohol 50ml is with mixed liquor stirring reaction 5 hours at room temperature.Sucking filtration uses the absolute ethanol washing filtrate for several times then, and the UV spectrophotometer measuring filtrate does not have chlorhexidine acetate, is deposited in 60 ℃ of following vacuum dryings to constant weight, and ball milling to particle diameter is 20-30 μ m, promptly obtains the chlorhexidine acetate modified montmorillonoid.Collect all filtrates,, get an amount of filtrate and use Biomat-5 type ultraviolet spectrophotometer mensuration ultraviolet light light absorption value, calculate residual drug 2.8g with the filtering with microporous membrane of 0.45um.Be chlorhexidine acetate at 10g Na-montmorillonite intercalation 1.2g, confirmed 30% chlorhexidine acetate insertion montmorillonite-based nano sheet interlayer with XRD test and IR test and ultraviolet spectrometry gravimetric analysis.
Embodiment 5
1. preparation Na-montorillonite clay: with embodiment 1.
2. preparation chlorhexidine acetate modification Na-montorillonite clay: get 10g Na-montorillonite clay and mix with the 6g chlorhexidine acetate, adding dehydrated alcohol 100ml is with mixed liquor stirring reaction 3 hours at room temperature.Sucking filtration uses the absolute ethanol washing filtrate for several times then, and the UV spectrophotometer measuring filtrate does not have chlorhexidine acetate, is deposited in 60 ℃ of following vacuum dryings to constant weight, and ball milling to particle diameter is 20-30 μ m, promptly obtains the chlorhexidine acetate modified montmorillonoid.Collect all filtrates,, get an amount of filtrate and use Biomat-5 type ultraviolet spectrophotometer mensuration ultraviolet light light absorption value, calculate residual drug 4.9g with the filtering with microporous membrane of 0.45um.Be chlorhexidine acetate at 10g Na-montmorillonite intercalation 2.1g, confirmed 35% chlorhexidine acetate insertion montmorillonite-based nano sheet interlayer with XRD test and IR test and ultraviolet spectrometry gravimetric analysis.
Embodiment 6
1. preparation Na-montorillonite clay: with embodiment 1.
2. preparation chlorhexidine acetate modification Na-montorillonite clay: get 10g Na-montorillonite clay and mix with the 8g chlorhexidine acetate, adding dehydrated alcohol 150ml is with mixed liquor stirring reaction 4 hours at room temperature.Sucking filtration uses the absolute ethanol washing filtrate for several times then, and the UV spectrophotometer measuring filtrate does not have chlorhexidine acetate, is deposited in 60 ℃ of following vacuum dryings to constant weight, and ball milling to particle diameter is 20-30 μ m, promptly obtains the chlorhexidine acetate modified montmorillonoid.Collect all filtrates,, get an amount of filtrate and use Biomat-5 type ultraviolet spectrophotometer mensuration ultraviolet light light absorption value, calculate residual drug 5.6g with the filtering with microporous membrane of 0.45um.Be chlorhexidine acetate at 10g Na-montmorillonite intercalation 2.4g, confirmed 30% chlorhexidine acetate insertion montmorillonite-based nano sheet interlayer with XRD test and IR test and ultraviolet spectrometry gravimetric analysis.
Embodiment 7
3. preparation Na-montorillonite clay: with embodiment 1.
2. preparation chlorhexidine acetate modification Na-montorillonite clay: get the 10gNa-montorillonite clay and mix with the 10g chlorhexidine acetate, adding dehydrated alcohol 80ml is with mixed liquor stirring reaction 4 hours at room temperature.Sucking filtration uses the absolute ethanol washing filtrate for several times then, and the UV spectrophotometer measuring filtrate does not have chlorhexidine acetate, is deposited in 60 ℃ of following vacuum dryings to constant weight, and ball milling to particle diameter is 20-30 μ m, promptly obtains the chlorhexidine acetate modified montmorillonoid.Collect all filtrates,, get an amount of filtrate and use Biomat-5 type ultraviolet spectrophotometer mensuration ultraviolet light light absorption value, calculate residual drug 7g with the filtering with microporous membrane of 0.45um.Be chlorhexidine acetate at 10g Na-montmorillonite intercalation 3g, confirmed 30% chlorhexidine acetate insertion montmorillonite-based nano sheet interlayer with XRD test and IR test and ultraviolet spectrometry gravimetric analysis.
Embodiment 8
3. preparation Na-montorillonite clay: with embodiment 1.
2. preparation tetracycline modification Na-montorillonite clay: above-mentioned gained 10gNa-montorillonite clay is mixed with the 6g tetracycline, and adding dehydrated alcohol 80ml is with mixed liquor stirring reaction 6 hours at room temperature.Sucking filtration uses the absolute ethanol washing filtrate for several times then, and the UV spectrophotometer measuring filtrate does not have tetracycline, is deposited in 60 ℃ of following vacuum dryings to constant weight, and ball milling to particle diameter is 20-30 μ m, promptly obtains the tetracycline modified montmorillonoid.Collect all filtrates,, get an amount of filtrate and use Biomat-5 type ultraviolet spectrophotometer mensuration ultraviolet light light absorption value, calculate residual drug 4.2g with the filtering with microporous membrane of 0.45um.Be that tetracycline is at 10g Na-montmorillonite intercalation 1.8g; Confirmed 30% tetracycline insertion montmorillonite-based nano sheet interlayer with XRD test and IR test and ultraviolet spectrometry gravimetric analysis.
Embodiment 9
3. preparation Na-montorillonite clay: with embodiment 1.
2. preparation tetracycline modification Na-montorillonite clay: above-mentioned gained 10gNa-montorillonite clay is mixed with the 8g tetracycline, and adding dehydrated alcohol 150ml is with mixed liquor stirring reaction 4 hours at room temperature.Sucking filtration uses the absolute ethanol washing filtrate for several times then, and the UV spectrophotometer measuring filtrate does not have tetracycline, is deposited in 60 ℃ of following vacuum dryings to constant weight, and ball milling to particle diameter is 20-30 μ m, promptly obtains the tetracycline modified montmorillonoid.Collect all filtrates,, get an amount of filtrate and use Biomat-5 type ultraviolet spectrophotometer mensuration ultraviolet light light absorption value, calculate residual drug 5.44g with the filtering with microporous membrane of 0.45um.Be that tetracycline is at 10g Na-montmorillonite intercalation 2.56g; Confirmed 32% tetracycline insertion montmorillonite-based nano sheet interlayer with XRD test and IR test and ultraviolet spectrometry gravimetric analysis.
Embodiment 10
3. preparation Na-montorillonite clay: with embodiment 1.
2. preparation tetracycline modification Na-montorillonite clay: above-mentioned gained 10gNa-montorillonite clay is mixed with the 10g tetracycline, and adding dehydrated alcohol 100ml is with mixed liquor stirring reaction 4 hours at room temperature.Sucking filtration uses the absolute ethanol washing filtrate for several times then, and the UV spectrophotometer measuring filtrate does not have tetracycline, is deposited in 60 ℃ of following vacuum dryings to constant weight, and ball milling to particle diameter is 20-30 μ m, promptly obtains the tetracycline modified montmorillonoid.Collect all filtrates,, get an amount of filtrate and use Biomat-5 type ultraviolet spectrophotometer mensuration ultraviolet light light absorption value, calculate residual drug 6.2g with the filtering with microporous membrane of 0.45um.Be that tetracycline is at 10g Na-montmorillonite intercalation 3.8g; Confirmed 38% tetracycline insertion montmorillonite-based nano sheet interlayer with XRD test and IR test and ultraviolet spectrometry gravimetric analysis.
Embodiment 11
3. preparation Na-montorillonite clay: with embodiment 1.
2. preparation amikacin sulfate modification Na-montorillonite clay: above-mentioned gained 10gNa-montorillonite clay is mixed with the 6g amikacin sulfate, adding deionized water 80ml, with mixed liquor 40 ℃ of following stirring reactions 3 hours.Sucking filtration uses the deionized water wash filtrate for several times then, and the UV spectrophotometer measuring filtrate does not have amikacin sulfate, is deposited in 60 ℃ of following vacuum dryings to constant weight, and ball milling to particle diameter is 20-30 μ m, promptly obtains the amikacin sulfate modified montmorillonoid.Collect all filtrates,, get an amount of filtrate and use Biomat-5 type ultraviolet spectrophotometer mensuration ultraviolet light light absorption value, calculate residual drug 4.5g with the filtering with microporous membrane of 0.45um.Be that amikacin sulfate is at 10g Na-montmorillonite intercalation 1.5g; Confirmed 25% amikacin sulfate insertion montmorillonite-based nano sheet interlayer with XRD test and IR test and ultraviolet spectrometry gravimetric analysis.
Embodiment 12
3. preparation Na-montorillonite clay: with embodiment 1.
2. preparation amikacin sulfate modification Na-montorillonite clay: above-mentioned gained 10gNa-montorillonite clay is mixed with the 10g amikacin sulfate, adding deionized water 100ml, with mixed liquor 40 ℃ of following stirring reactions 6 hours.Sucking filtration uses the deionized water wash filtrate for several times then, and the UV spectrophotometer measuring filtrate does not have amikacin sulfate, is deposited in 60 ℃ of following vacuum dryings to constant weight, and ball milling to particle diameter is 20-30 μ m, promptly obtains the amikacin sulfate modified montmorillonoid.Collect all filtrates,, get an amount of filtrate and use Biomat-5 type ultraviolet spectrophotometer mensuration ultraviolet light light absorption value, calculate residual drug 7g with the filtering with microporous membrane of 0.45um.Be that amikacin sulfate is at 10g Na-montmorillonite intercalation 3g; Confirmed 30% amikacin sulfate insertion montmorillonite-based nano sheet interlayer with XRD test and IR test and ultraviolet spectrometry gravimetric analysis.
Embodiment 13
3. preparation Na-montorillonite clay: with embodiment 1.
2. preparation rifampicin modification Na-montorillonite clay: above-mentioned gained 10gNa-montorillonite clay and 5g rifampicin powder are added in the 150ml chloroform, stirred 4 hours under the room temperature, sucking filtration is used chloroform washing and filtering thing 4 times then.Be deposited in 60 ℃ of following vacuum dryings to constant weight, ball milling to particle diameter is 20-30 μ m, promptly obtains the rifampicin modified montmorillonoid.Collect all filtrates,, get an amount of filtrate and use Biomat-5 type ultraviolet spectrophotometer mensuration ultraviolet light light absorption value, calculate residual drug 3.75g with the filtering with microporous membrane of 0.45um.Be that rifampicin is at 10g Na-montmorillonite intercalation 1.25g; Confirmed 25% rifampicin insertion montmorillonite-based nano sheet interlayer with XRD test and IR test and ultraviolet spectrometry gravimetric analysis.
Embodiment 14
3. preparation Na-montorillonite clay: with embodiment 1.
2. preparation rifampicin modification Na-montorillonite clay: above-mentioned gained 10gNa-montorillonite clay and 10g rifampicin powder are added in the 150ml chloroform, stirred 3 hours under the room temperature, sucking filtration is used chloroform washing and filtering thing 4 times then.Be deposited in 60 ℃ of following vacuum dryings to constant weight, ball milling to particle diameter is 20-30 μ m, promptly obtains the rifampicin modified montmorillonoid.Collect all filtrates,, get an amount of filtrate and use Biomat-5 type ultraviolet spectrophotometer mensuration ultraviolet light light absorption value, calculate residual drug 6.5g with the filtering with microporous membrane of 0.45um.Be that rifampicin is at 10g Na-montmorillonite intercalation 3.5g; Confirmed 35% rifampicin insertion montmorillonite-based nano sheet interlayer with XRD test and IR test and ultraviolet spectrometry gravimetric analysis.
Embodiment 15
1. preparation Na-montorillonite clay: with embodiment 1.
2. preparation tetracycline/miconazole modification Na-montorillonite clay: above-mentioned gained 10gNa-montorillonite clay is mixed with 3g tetracycline, 3g miconazole, and adding dehydrated alcohol 150ml is with mixed liquor stirring reaction 4 hours at room temperature.Sucking filtration uses the absolute ethanol washing filtrate for several times then, and the UV spectrophotometer measuring filtrate does not have tetracycline, miconazole, is deposited in 60 ℃ of following vacuum dryings to constant weight, and ball milling to particle diameter is 20-30 μ m, promptly obtains tetracycline/miconazole modified montmorillonoid.Collect all filtrates,, get an amount of filtrate and use Biomat-5 type ultraviolet spectrophotometer mensuration ultraviolet light light absorption value, calculate residual drug 3.6g with the filtering with microporous membrane of 0.45um.Be that medicine is at 10g Na-montmorillonite intercalation 2.4g; Confirmed 40% medicine insertion montmorillonite-based nano sheet interlayer with XRD test and IR test and ultraviolet spectrometry gravimetric analysis.
Embodiment 16
1. preparation Na-montorillonite clay: with embodiment 1.
2. preparation tetracycline/miconazole modification Na-montorillonite clay: above-mentioned gained 10gNa-montorillonite clay is mixed with 4g tetracycline, 4g miconazole, and adding dehydrated alcohol 200ml is with mixed liquor stirring reaction 4 hours at room temperature.Sucking filtration uses the absolute ethanol washing filtrate for several times then, and the UV spectrophotometer measuring filtrate does not have tetracycline, miconazole, is deposited in 60 ℃ of following vacuum dryings to constant weight, and ball milling to particle diameter is 20-30 μ m, promptly obtains tetracycline/miconazole modified montmorillonoid.Collect all filtrates,, get an amount of filtrate and use Biomat-5 type ultraviolet spectrophotometer mensuration ultraviolet light light absorption value, calculate residual drug 5.2g with the filtering with microporous membrane of 0.45um.Be that medicine is at 10g Na-montmorillonite intercalation 2.8g; Confirmed 35% medicine insertion montmorillonite-based nano sheet interlayer with XRD test and IR test and ultraviolet spectrometry gravimetric analysis.
Embodiment 17
1. preparation Na-montorillonite clay: with embodiment 1.
2. preparation tetracycline/hibitane modification Na-montorillonite clay: above-mentioned gained 10gNa-montorillonite clay is mixed with 3g tetracycline, 3g hibitane, and adding dehydrated alcohol 100ml is with mixed liquor stirring reaction 3 hours at room temperature.Sucking filtration uses the absolute ethanol washing filtrate for several times then, and the UV spectrophotometer measuring filtrate does not have tetracycline, hibitane, is deposited in 60 ℃ of following vacuum dryings to constant weight, and ball milling to particle diameter is 20-30 μ m, promptly obtains tetracycline/hibitane modified montmorillonoid.Collect all filtrates,, get an amount of filtrate and use Biomat-5 type ultraviolet spectrophotometer mensuration ultraviolet light light absorption value, calculate residual drug 3.9g with the filtering with microporous membrane of 0.45um.Be that medicine is at 10g Na-montmorillonite intercalation 2.1g; Confirmed 35% medicine insertion montmorillonite-based nano sheet interlayer with XRD test and IR test and ultraviolet spectrometry gravimetric analysis.
Embodiment 18
1. preparation Na-montorillonite clay: with embodiment 1.
2. preparation tetracycline/hibitane modification Na-montorillonite clay: above-mentioned gained 10gNa-montorillonite clay is mixed with 5g tetracycline, 5g hibitane, and adding dehydrated alcohol 200ml is with mixed liquor stirring reaction 4 hours at room temperature.Sucking filtration uses the absolute ethanol washing filtrate for several times then, and the UV spectrophotometer measuring filtrate does not have tetracycline, hibitane, is deposited in 60 ℃ of following vacuum dryings to constant weight, and ball milling to particle diameter is 20-30 μ m, promptly obtains tetracycline/hibitane modified montmorillonoid.Collect all filtrates,, get an amount of filtrate and use Biomat-5 type ultraviolet spectrophotometer mensuration ultraviolet light light absorption value, calculate residual drug 6g with the filtering with microporous membrane of 0.45um.Be that medicine is at 10g Na-montmorillonite intercalation 4g; Confirmed 40% medicine insertion montmorillonite-based nano sheet interlayer with XRD test and IR test and ultraviolet spectrometry gravimetric analysis.
Embodiment 19
1. preparation Na-montorillonite clay: with embodiment 1.
2. preparation tetracycline/hibitane/miconazole modification Na-montorillonite clay: above-mentioned gained 10gNa-montorillonite clay is mixed with 2g tetracycline, 2g hibitane and 2g miconazole, and adding ethanol 100ml is with mixed liquor stirring reaction 5 hours at room temperature.Sucking filtration, use the washing with alcohol filtrate for several times then, the UV spectrophotometer measuring filtrate does not have tetracycline, hibitane, miconazole, is deposited in 60 ℃ of following vacuum dryings to constant weight, ball milling to particle diameter is 20-30 μ m, promptly obtains tetracycline/hibitane/miconazole modified montmorillonoid.Collect all filtrates,, get an amount of filtrate and use Biomat-5 type ultraviolet spectrophotometer mensuration ultraviolet light light absorption value, calculate residual drug 3.3g with the filtering with microporous membrane of 0.45um.Be that medicine is at 10g Na-montmorillonite intercalation 2.7g; Confirmed 45% medicine insertion montmorillonite-based nano sheet interlayer with XRD test and IR test and ultraviolet spectrometry gravimetric analysis.
Embodiment 20
1. preparation Na-montorillonite clay: with embodiment 1.
2. preparation tetracycline/hibitane/miconazole modification Na-montorillonite clay: above-mentioned gained 10gNa-montorillonite clay is mixed with 3g tetracycline, 3g hibitane and 3g miconazole, and adding ethanol 150ml is with mixed liquor stirring reaction 4 hours at room temperature.Sucking filtration, use the washing with alcohol filtrate for several times then, the UV spectrophotometer measuring filtrate does not have tetracycline, hibitane, miconazole, is deposited in 60 ℃ of following vacuum dryings to constant weight, ball milling to particle diameter is 20-30m, promptly obtains tetracycline/hibitane/miconazole modified montmorillonoid.Collect all filtrates,, get an amount of filtrate and use Biomat-5 type ultraviolet spectrophotometer mensuration ultraviolet light light absorption value, calculate residual drug 4.5g with the filtering with microporous membrane of 0.45um.Be that medicine is at 10g Na-montmorillonite intercalation 4.5g; Confirmed 50% medicine insertion montmorillonite-based nano sheet interlayer with XRD test and IR test and ultraviolet spectrometry gravimetric analysis.
Claims (8)
1. nano montmorillonite for restraining bacterium, it is made up of the component of following mass parts:
Na-montorillonite clay: 100;
Antibacterial medicines: 10～45;
Wherein, described antibacterial medicines is: tetracycline or doxycycline.
2. the described nano montmorillonite for restraining bacterium of claim 1, wherein the consumption of antibacterial medicines is 20～45 parts/100 parts Na-montorillonite clays.
3. the preparation method of claim 1 or 2 described nano montmorillonite for restraining bacterium, contain following steps:
Na-montorillonite clay and antibacterial medicines are mixed, add dehydrated alcohol or the deionized water or the chloroform stirring formation stable suspension of 5～20 times of quality, stirred 2～6 hours down for 40 ℃, filter, remove dehydrated alcohol or deionized water or chloroform in room temperature or constant temperature; With dehydrated alcohol or deionized water or chloroform washing filter thing, dry, ball milling obtains the nano montmorillonite for restraining bacterium that particle diameter is 20 ~ 30 μ m then.
4. the described nano montmorillonite for restraining bacterium preparation method of claim 3, wherein mixing time is 3～5 hours.
5. the described nano montmorillonite for restraining bacterium preparation method of claim 3, wherein mixing time is 4 hours.
6. the described nano montmorillonite for restraining bacterium preparation method of claim 3, wherein whipping temp is 40 ℃ of constant temperature.
7. the described nano montmorillonite for restraining bacterium preparation method of claim 3, wherein whipping temp is a room temperature.
8. the described nano montmorillonite for restraining bacterium preparation method of claim 3, wherein form ethanol or the deionized water or the chloroform quality of suspension with the Na-montorillonite clay: Na-montorillonite clay quality is 8: 1.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102440982A (en) * | 2011-09-16 | 2012-05-09 | 南京师范大学 | Chlorhexidine acetate-copper/imvite nano antibacterial composite material and preparation method thereof |
| CN105418972A (en) * | 2016-01-25 | 2016-03-23 | 郑叶芳 | Organic antimicrobial agent intercalation modified montmorillonite and application thereof |
| CN105454232A (en) * | 2016-01-25 | 2016-04-06 | 郑叶芳 | Montmorillonite-based antibacterial agent and preparation method thereof |
| CN110694073A (en) * | 2019-10-21 | 2020-01-17 | 南通大学附属医院 | Drug-loaded long-circulation modified nano-montmorillonite material and preparation method thereof |
-
2005
- 2005-09-27 CN CN2007101377683A patent/CN101130085B/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102440982A (en) * | 2011-09-16 | 2012-05-09 | 南京师范大学 | Chlorhexidine acetate-copper/imvite nano antibacterial composite material and preparation method thereof |
| CN102440982B (en) * | 2011-09-16 | 2014-05-28 | 南京师范大学 | Chlorhexidine acetate-copper/imvite nano antibacterial composite material and preparation method thereof |
| CN105418972A (en) * | 2016-01-25 | 2016-03-23 | 郑叶芳 | Organic antimicrobial agent intercalation modified montmorillonite and application thereof |
| CN105454232A (en) * | 2016-01-25 | 2016-04-06 | 郑叶芳 | Montmorillonite-based antibacterial agent and preparation method thereof |
| CN105418972B (en) * | 2016-01-25 | 2018-08-21 | 郑叶芳 | A kind of organic antibacterial agent intercalation modifying montmorillonite and its application |
| CN110694073A (en) * | 2019-10-21 | 2020-01-17 | 南通大学附属医院 | Drug-loaded long-circulation modified nano-montmorillonite material and preparation method thereof |
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