WO2017158626A1 - Nanocomposites hybrides de nio-nanocellulose à activités antibactériennes et antifongiques - Google Patents
Nanocomposites hybrides de nio-nanocellulose à activités antibactériennes et antifongiques Download PDFInfo
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- WO2017158626A1 WO2017158626A1 PCT/IN2017/050099 IN2017050099W WO2017158626A1 WO 2017158626 A1 WO2017158626 A1 WO 2017158626A1 IN 2017050099 W IN2017050099 W IN 2017050099W WO 2017158626 A1 WO2017158626 A1 WO 2017158626A1
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- 229920001046 Nanocellulose Polymers 0.000 title claims abstract description 109
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 60
- 230000000843 anti-fungal effect Effects 0.000 title claims abstract description 23
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 41
- 235000007164 Oryza sativa Nutrition 0.000 claims abstract description 25
- 235000009566 rice Nutrition 0.000 claims abstract description 25
- 239000010902 straw Substances 0.000 claims abstract description 25
- 241000222122 Candida albicans Species 0.000 claims abstract description 19
- 229940095731 candida albicans Drugs 0.000 claims abstract description 19
- 230000002538 fungal effect Effects 0.000 claims abstract description 19
- 241000222199 Colletotrichum Species 0.000 claims abstract description 16
- LAIZPRYFQUWUBN-UHFFFAOYSA-L nickel chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Ni+2] LAIZPRYFQUWUBN-UHFFFAOYSA-L 0.000 claims abstract description 15
- 241000894006 Bacteria Species 0.000 claims abstract description 13
- 241000588724 Escherichia coli Species 0.000 claims abstract description 13
- 241000589776 Pseudomonas putida Species 0.000 claims abstract description 13
- 241000191967 Staphylococcus aureus Species 0.000 claims abstract description 13
- 230000000845 anti-microbial effect Effects 0.000 claims abstract description 12
- 230000001580 bacterial effect Effects 0.000 claims abstract description 10
- 241000730682 Bacillus toyonensis BCT-7112 Species 0.000 claims abstract description 9
- 241000192125 Firmicutes Species 0.000 claims abstract description 8
- 240000007594 Oryza sativa Species 0.000 claims abstract 2
- 239000011541 reaction mixture Substances 0.000 claims description 34
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- 239000012153 distilled water Substances 0.000 claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 229910000480 nickel oxide Inorganic materials 0.000 claims description 14
- 241000193755 Bacillus cereus Species 0.000 claims description 13
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 12
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 10
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 8
- 238000002360 preparation method Methods 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 8
- 230000001476 alcoholic effect Effects 0.000 claims description 7
- 239000006227 byproduct Substances 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 239000002154 agricultural waste Substances 0.000 claims description 4
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 2
- 239000000920 calcium hydroxide Substances 0.000 claims description 2
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 abstract description 19
- 238000003786 synthesis reaction Methods 0.000 abstract description 19
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 238000005580 one pot reaction Methods 0.000 abstract description 5
- 241001660259 Cereus <cactus> Species 0.000 abstract description 2
- 241000209094 Oryza Species 0.000 description 23
- 230000005764 inhibitory process Effects 0.000 description 23
- 229920002678 cellulose Polymers 0.000 description 17
- 239000001913 cellulose Substances 0.000 description 17
- 235000010980 cellulose Nutrition 0.000 description 17
- 239000000243 solution Substances 0.000 description 17
- 239000000047 product Substances 0.000 description 16
- 238000012360 testing method Methods 0.000 description 14
- 239000002253 acid Substances 0.000 description 13
- 229910052500 inorganic mineral Inorganic materials 0.000 description 10
- 239000011707 mineral Substances 0.000 description 10
- 239000000203 mixture Substances 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 238000002828 disc diffusion antibiotic sensitivity testing Methods 0.000 description 8
- 235000013305 food Nutrition 0.000 description 8
- 229940125898 compound 5 Drugs 0.000 description 7
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 7
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 6
- 230000003389 potentiating effect Effects 0.000 description 6
- 238000000638 solvent extraction Methods 0.000 description 6
- 239000002028 Biomass Substances 0.000 description 5
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 5
- 238000005904 alkaline hydrolysis reaction Methods 0.000 description 5
- 239000003153 chemical reaction reagent Substances 0.000 description 5
- 230000002401 inhibitory effect Effects 0.000 description 5
- 239000012454 non-polar solvent Substances 0.000 description 5
- 239000002798 polar solvent Substances 0.000 description 5
- 241000012248 Bacillus toyonensis Species 0.000 description 4
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 4
- 239000001965 potato dextrose agar Substances 0.000 description 4
- 241000193830 Bacillus <bacterium> Species 0.000 description 3
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 244000005700 microbiome Species 0.000 description 3
- 239000003208 petroleum Substances 0.000 description 3
- 239000002574 poison Substances 0.000 description 3
- 231100000614 poison Toxicity 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 239000001117 sulphuric acid Substances 0.000 description 3
- 235000011149 sulphuric acid Nutrition 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- 239000003899 bactericide agent Substances 0.000 description 2
- 230000004071 biological effect Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- MYSWGUAQZAJSOK-UHFFFAOYSA-N ciprofloxacin Chemical compound C12=CC(N3CCNCC3)=C(F)C=C2C(=O)C(C(=O)O)=CN1C1CC1 MYSWGUAQZAJSOK-UHFFFAOYSA-N 0.000 description 2
- 238000000338 in vitro Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002609 medium Substances 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 235000015097 nutrients Nutrition 0.000 description 2
- 244000052769 pathogen Species 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- NQTSTBMCCAVWOS-UHFFFAOYSA-N 1-dimethoxyphosphoryl-3-phenoxypropan-2-one Chemical compound COP(=O)(OC)CC(=O)COC1=CC=CC=C1 NQTSTBMCCAVWOS-UHFFFAOYSA-N 0.000 description 1
- 229920001817 Agar Polymers 0.000 description 1
- 241000697872 Bactria Species 0.000 description 1
- 241000222120 Candida <Saccharomycetales> Species 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 241001269238 Data Species 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 241000233866 Fungi Species 0.000 description 1
- 229920000168 Microcrystalline cellulose Polymers 0.000 description 1
- 229920002522 Wood fibre Polymers 0.000 description 1
- 239000008272 agar Substances 0.000 description 1
- 229940121375 antifungal agent Drugs 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 229960003405 ciprofloxacin Drugs 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000000855 fungicidal effect Effects 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 239000001963 growth medium Substances 0.000 description 1
- 238000011534 incubation Methods 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 238000011081 inoculation Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 239000002608 ionic liquid Substances 0.000 description 1
- 238000009630 liquid culture Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 235000019813 microcrystalline cellulose Nutrition 0.000 description 1
- 239000008108 microcrystalline cellulose Substances 0.000 description 1
- 229940016286 microcrystalline cellulose Drugs 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000006916 nutrient agar Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000000101 transmission high energy electron diffraction Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002025 wood fiber Substances 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
Definitions
- This invention particularly relates to novel process for synthesis of a new class of
- NiO-Nanocellulose Hybrid Nanocomposites of formula 5 having Antibacterial and Antifungal activities and possess overall yield 90% after purification.
- This invention also relates to the Antimicrobial Activities against (03) three gram positive; (02) two gram negative bacterial strains and fungal strain Candida albicans MTCC 3017.
- Gram positive bacteria are Staphylococcus aureus MTCC 6908, Bacillus toyonensis BCT 7112 and Bacillus cereus MTCC 1272; Gram negative bacteria are Pseudomonas putida ATCC 17642 and Escherichia coli MTCC 739 and Fungal strain are Candida albicans MTCC 3017 and their Antifungal activity against plant pathogenic fungus Colletotrichum gleosporioides.
- the present invention relates to the synthesis of a new class of NiO-
- this invention relates to the synthesis of Nanocellulose from renewable agrowaste i.e. rice straw.
- the process of the present invention does not involve the use of any costly and environmentally toxic reagents and catalysts and has been developed using a non-toxic reagents under mild reaction conditions.
- the present invention provides for the production of nanocellulose in a very cost-effective and convenient method from a renewable agriculture resource, rice straw.
- Nanocomposites is recently gaining importance owing to their potent biological activity. So far, no literature reported on NiO-NC, which has potent antibacterial and antifungal activity against bacterial strains and fungal strain such as Candida albicans MTCC3007, Gram positive bacteria Staphylococcus aureus MTCC 6908, Bacillus toyonensis BCT 7112 and Bacillus cereus MTCC 1272; and Gram negative bacteria such as Pseudomonas putida ATCC 17642 and Escherichia coli MTCC 739; Fungal strain Candida albicans MTCC 3017 and plant pathogenic fungus Colletotrichum gleosporioides.
- bacterial strains and fungal strain such as Candida albicans MTCC3007, Gram positive bacteria Staphylococcus aureus MTCC 6908, Bacillus toyonensis BCT 7112 and Bacillus cereus MTCC 1272; and Gram negative bacteria such as Ps
- Nanocellulose was carried out from renewable agrowaste i.e. rice straw.
- the hitherto known prior art generally related is referred to herein below:
- Nanocellulose Composite which describes the method of nanocellulose composites and a method of manufacturing nanocellulose composites which comprise nanocellulose material mixed with a polymer.
- Patent number CN102505546A entitled “Method for preparing nanocellulose by using homogeneous method” discloses a method for preparing nanocellulose by using a homogeneous method, relating to a method for preparing modified cellulose, i.e., the nanocellulose.
- the method comprises the following steps of adding ionic liquid into crushed wood fibers to ensure that the mass percentage of the cellulose is 1-15%.
- CNCs/ZnO cellulose nanocrystals/zinc oxide
- PVA poly(vinyl alcohol)
- Cs chitosan
- Nano and nanocomposite antimicrobial materials for food packaging applications Paulraj Kanmani & Jong -Whan Rhim, Progress in Nanomaterials for Food Packaging, 2014, 34-48” describes the antimicrobial function of some nano and nanocomposite materials.
- NiO-Nanocellulose (NiO-NC) Hybrid Nanocomposites of the formula 5 described in the present invention is completely new and has not been reported so far by any other workers.
- the main objective of the present invention is to provide a novel process to synthesize a new class of NiO-Nanocellulose (NiO-NC) Hybrid Nanocomposites of formula 5 starting from nickel chloride hexahydrate (N1CI 2 .6H 2 O) and nanocellulose (NC).
- NiO-NC NiO-Nanocellulose
- the size of this new class of NiO-Nanocellulose (NiO-NC) Hybrid Nanocomposites is in the range of 0.4 nm shown in Figure 4.
- Yet another objective of the present invention is to provide antimicrobial activities against (03) three gram positive; (02) two gram negative bacterial strains and fungal strain Candida albicans MTCC 3017.
- Gram positive bacteria are Staphylococcus aureus MTCC 6908, Bacillus toyonensis BCT 7112 and Bacillus cereus MTCC 1272;
- Gram negative bacteria are Pseudomonas putida ATCC 17642 and Escherichia coli MTCC 739; and Fungal strain Candida albicans MTCC 3017 are shown in Figure 1.
- Yet another objective of the present invention is to provide a general method of preparation of a new class of NiO-Nanocellulose (NiO-NC) Hybrid Nanocomposites of the formula 5 starting from Nickel oxide (NiO) and nano cellulose (NC) with one step reaction which could be useful as potent antifungal inhibitors against plant pathogenic fungus Colletotrichum gleosporioides shown in Figure 2.
- NiO-NC NiO-Nanocellulose
- NC nano cellulose
- Still another objective of the present invention is to provide a one pot process for synthesis or construct a new class of NiO-Nanocellulose (NiO-NC) Hybrid Nanocomposites of formula 5.
- the present invention provides a NiO-Nanocellulose hybrid nanocomposites having antibacterial and antifungal activity, wherein the said hybrid nanocomposite exhibit the particle size ranging from 04-10 nm.
- the hybrid nanocomposites exhibit good antimicrobial activity viz. antibacterial activity against Gram+ve ,Gram-ve bacterial strains and Fungal strain Candida albicans MTCC 3017, wherein Gram positive bacteria are Staphylococcus aureus MTCC 6908, Bacillus toyonensis BCT 7112 and Bacillus cereus MTCC 1272; Gram negative bacteria are Pseudomonas putida ATCC 17642 and Escherichia coli MTCC 739.
- step (iii) centrifuged the reaction mixture of step (ii) to separate nickel oxide nanocellulose nanocomposites (NiO-NC), washing with distilled water for several times to remove the byproducts;
- base solution used for the reaction is selected from the group consisting of potassium hydroxide, sodium hydroxide, calcium hydroxide and sodium carbonate and in the range of 100 ml of 2 mol/L - 100 ml of 10 mol/L per 1 gm of nanocellulose used.
- the renewable agrowaste rice straw was used.
- the new class of NiO- Nanocellulose (NiO-NC) Hybrid Nanocomposites of formula 5 possess overall yield 90% after purification and have been found to show good antibacterial activity in general determined by disc diffusion method as shown in Figure 1.
- Nanocellulose (NiO-NC) Hybrid Nanocomposites of formula 5 also has been found to show potent antifungal activity against plant pathogenic fungus Colletotrichum gleosporioides determined by using the poisoned food technique as shown in Figure 2. Colletotrichum gleosporioides with the inhibition percentage 98% as depicted in the Figure 2 which was determined by the standard antifungal activity test, viz., Poison Food Technique.
- Antibacterial test was performed on four different types of the pathogens and all were found to be sensitive to compound 5 with inhibition zones varying from 2.67-15 mm.
- the product of formula 5 derived from nanocellulose with nickel chloride hexahydrate (N1CI 2 .6H 2 O) of the formula 1 and 2 were show highest inhibition against Candida albicans of 15+00 mm at concentration 50 ⁇ / ⁇ 1 followed by Bacillus toyonensis of 7+1 mm.
- Pseudomonas putida and Staphylococcus aureus inhibition zones were 4.67+0.57 mm and 5.33+1.15 mm respectively at concentration of 50 ⁇ / ⁇ 1.
- a little inhibition zones were detected against Escherichia coli and Bacillus cereus. From the analyzed result, these NiO-Nanocellulose (NiO-NC) Hybrid Nanocomposites of the formula 5 has been found to be the most promising bactericide against both Gram positive and Gram negative bacteria with MIC values 0.05-2 ⁇ g respectively.
- Figure 1 Zone of inhibition of compound against 1) Pseudomonas putida 2) Escherichia coli 3) Bacillus toyonensis 4) Staphylococcus aureus 5) Bacillus cereus and 6) Candida albicans
- Figure 2 Antifungal activity against plant pathogenic fungus Colletotrichum gleosporioides.
- Figure 3 TEM image of nanocellulose.
- This invention relates to the process for synthesis of a new and novel compound of formula 5 NiO-Nanocellulose Hybrid Nanocomposites prepared from nickel chloride hexahydrate (NiCl 2 .6H 2 0) and nanocellulose
- NC Nickel chloride hexahydrate NiO-Nanocellulose Hybrid Nanocomposites
- NC Nano cellulose
- NiCl 2 .6H 2 0 Nickel chloride hexahydrate
- Ethanol (EtOH) 4 Sodium hydroxide (NaOH)
- This invention also relates to the process for synthesis of new class of NiO- Nanocellulose Hybrid Nanocomposites and their Antifungal Activity against plant pathogenic fungus Colletotrichum gleosporioid.es.
- This invention particularly relates to the process for synthesis of new class of NiO- Nanocellulose Hybrid Nanocomposites and their Antimicrobial Activities against (03) three gram positive and (02) two gram negative bacterial strains and fungal strain Candida albicans MTCC 3017.
- Gram positive bacteria are Staphylococcus aureus MTCC 6908, Bacillus toyonensis BCT7112 and Bacillus cereus MTCC 1272;
- Gram negative bacteria are Pseudomonas putida ATCC 17642 and Escherichia coli MTCC 739.
- Fungal strain is Candida albicans MTCC 3017.
- the process of invention is found to have an overall yield 90% after purification.
- the process of the present invention does not involve the use of any costly and environmentally toxic reagents and catalysts and has been developed using a non-toxic reagents under mild reaction conditions.
- the present invention provides for the production of nanocellulose in a very cost-effective and convenient method from a renewable agriculture resource, rice straw of North East India.
- the present investigation is to provide an one pot process for synthesizing or constructing a new class of NiO-Nanocellulose Hybrid Nanocomposites of the formula 5 with yield of 90% from nickel chloride hexahydrate (NiCl 2 .6H 2 0) of the formula 1 and nanocellulose of the formula 2 accompanying this specification which comprises the following steps :-
- Step I Solvent extraction of rice straw plant material is done with the help of Soxhlet apparatus using non polar solvent (petroleum ether/hexane) and polar solvent (methanol/ethanol) .
- non polar solvent petroleum ether/hexane
- polar solvent methanol/ethanol
- Step II After solvent extraction rice straw was dried in an oven in a period of 3-6 hrs at the temperature range 40-60 °C. Alkaline hydrolysis was done using base in the range of 100-250 ml of NaOH and Na 2 C0 3 and stirred the mixture for a period of 6-12 hours. The reaction mixture was then cooled and neutralized with mineral acid selected from the group consisting of hydrochloric acid, sulphuric acid or perchloric acid etc, particularly hydrochloric acid and in the range of 10-20 % per 10 gm of pretreated rice straw used.
- mineral acid selected from the group consisting of hydrochloric acid, sulphuric acid or perchloric acid etc, particularly hydrochloric acid and in the range of 10-20 % per 10 gm of pretreated rice straw used.
- Step III Cellulose was acid hydrolysed with mineral acid selected from the group consisting of sulphuric acid, hydrochloric acid or perchloric acid etc, particularly sulphuric acid in the range of 4-6% per 10 gm of cellulose. Refluxed the reaction mixture in a period of 4-6 hrs at the temperature range 60-80 °C. Then the reaction mixture was filtered and washed with distilled water for several times to get the desired product nanocellulose .
- mineral acid selected from the group consisting of sulphuric acid, hydrochloric acid or perchloric acid etc, particularly sulphuric acid in the range of 4-6% per 10 gm of cellulose. Refluxed the reaction mixture in a period of 4-6 hrs at the temperature range 60-80 °C. Then the reaction mixture was filtered and washed with distilled water for several times to get the desired product nanocellulose .
- Step IV Nickel oxide nanocellulose hybrid nanocomposites were synthesized by using nanocellulose with nickel chloride hexahydrate (NiCl 2 -6H 2 0) mixing in alcoholic solvent with weight ratio of N1CI 2 .6H 2 O : nanocellulose was 1:2.
- Antimicrobial test was performed on four different types of the pathogens and all were found to be sensitive to compound 5 with inhibition zones varying from 2.67-15 mm. The highest inhibition was calculated against Candida albicans of 15+00 mm at concentration 50 ⁇ / ⁇ 1 followed by Bacillus toyonensis of 7+1 mm. In Pseudomonas putida and Staphylococcus aureus inhibition zones were 4.67+0.57 mm and 5.33+1.15 mm respectively at concentration of 50 ⁇ / ⁇ 1. A little inhibition zones were detected against Escherichia coli and Bacillus cereus. From the analyzed result, these NiO-Nanocellulose (NiO-NC) Hybrid Nanocomposites of the formula 5 has been found to be the most promising bactericide against both Gram positive and Gram negative bacteria with MIC values 0.05-2 ⁇ g respectively.
- NiO-NC NiO-Nanocellulose
- NiO-NC NiO-Nanocellulose
- the new and novel class of NiO-Nanocellulose (NiO-NC) Hybrid Nanocomposites of formula 5 also has been found to show potent antifungal activity against plant pathogenic fungus Colletotrichum gleosporioides determined by using the poisoned food technique as shown in Figure 2. Colletotrichum gleosporioides with the inhibition percentage 98% as depicted in the Figure 2 which was determined by the standard antifungal activity test, viz., Poison Food Technique.
- Step A Preparation of nanocellulose:
- Step I Dry powdered RS sample was extracted with non polar solvent -petroleum ether and polar solvent -methanol with the help of Soxhlet apparatus for 15 hrs at 45 °C to remove oil/wax etc.
- Step II After solvent extraction rice straw was dried in an oven for 4 hrs at 40 °C. Alkaline hydrolysis was done using mixture of 5% NaOH of 150 ml and 5% Na 2 C0 3 of 150 ml and stirred the mixture for 7 hours. The reaction mixture was then cooled and neutralized with 10% mineral acid - 10 ml HC1 per 10 gm of pretreated rice straw. Filtered the biomass and treated with 20% H 2 0 2 solution of 10 ml per 10 gm of pretreated rice straw and stirred for 6 hrs at 45 °C. The reaction mixture was then cooled and filtered and then washed with distilled water for several times to get the desired product cellulose with the yield of 75%.
- Step III Cellulose was acid hydrolysed with 5% mineral acid- 5 ml H 2 S0 4 per 10 gm of cellulose. Reaction mixture was refluxed for 5 hrs at 70 °C. After that reaction mixture was filtered and washed with distilled water for several times to get the desired product nanocellulose with the yield 90%.
- Step B Synthesis of NiO-Nanocellulose (NiO-NC) Hybrid Nanocomposites :
- Nickel oxide nanocellulose hybrid nanocomposites were synthesized by mixing nanocellulose with nickel chloride hexahydrate (NiCl 2 .6H 2 0) in alcoholic solvent -EtOH and further stirring the reaction for a period of 3 hrs at 45 °C to get transparent solution with weight ratio of NiCl 2 .6H 2 0 : nanocellulose as 1:2. After that sodium hydroxide solution was added dropwise to the above reaction mixture with gentle stirring for 12 hrs at 75 °C and allowing to settle down, centrifuging the reaction mixture to separate nickel oxide nanocellulose nanocomposites (NiO-NC) and washing with distilled water for several times to remove the byproducts. Sample was dried for 2 hrs at 70 °C to get the compound 5 with yield 90%.
- Step A Preparation of nanocellulose:
- Step I Dry powdered RS sample was extracted with non polar solvent - hexane and polar solvent -ethanol with the help of Soxhlet apparatus for 18 hrs at 50 °C to remove oil/wax etc.
- Step II After solvent extraction rice straw was dried in an oven for 6 hrs at 45°C. Alkaline hydrolysis was done using mixture of 5% KOH of 150 ml and 5% Na 2 C0 3 of 150 ml and stirred the mixture for 9 hours. The reaction mixture was then cooled and neutralized with 10% mineral acid -10 ml H 2 S0 4 per 10 gm of pretreated rice straw. Filtered the biomass and treated with 20% H 2 0 2 solution of 10 ml per 10 gm of pretreated rice straw and stirred for 8 hrs at 55 °C. The reaction mixture was then cooled and filtered and then washed with distilled water for several times to get the desired product cellulose with the yield of 60%.
- Step III Cellulose was acid hydrolysed with 10% mineral acid -10 ml HC1 per 10 gm of cellulose. Reaction mixture was refluxed for 7 hrs at 90 °C. After that reaction mixture was filtered and washed with distilled water for several times to get the desired product nanocellulose with the yield 80%.
- Step B Synthesis of NiO-Nanocellulose (NiO-NC) Hybrid Nanocomposites: Nickel oxide nanocellulose hybrid nanocomposites were synthesized by mixing nanocellulose with nickel chloride hexahydrate (NiCl 2 .6H 2 0) in alcoholic solvent -MeOH and stirred the reaction for a period of 2 hrs at 40 °C to get transparent solution with weight ratio of NiCl 2 .6H 2 0 : nanocellulose as 1:2.
- Step A Preparation of nanocellulose:
- Step I Dry powdered RS sample was extracted with non polar solvent - hexane and polar solvent - propanol with the help of Soxhlet apparatus for 10 hrs at 45 °C to remove oil/wax etc.
- Step II After solvent extraction rice straw was dried in an oven for 8 hrs at 55 °C. Alkaline hydrolysis was done using mixture of 3% NaOH of 150 ml and 3% Na 2 C0 3 of 200 ml and stirred the mixture for 10 hours. The reaction mixture was then cooled and neutralized with 10% mineral acid- 10 ml HC10 4 per 10 gm of pretreated rice straw. Filtered the biomass and treated with 15% H 2 0 2 solution of 20 ml per 10 gm of pretreated rice straw and stirred for 10 hrs at 60 °C. The reaction mixture was then cooled and filtered and then washed with distilled water for several times to get the desired product cellulose with yield of 50%.
- Step III Cellulose was acid hydrolysed with 10% mineral acid -10 ml HC10 4 10 ml per 10 gm of cellulose used. Reaction mixture was refluxed for 9 hrs at 90 °C. After that reaction mixture was filtered and washed with distilled water for several times to get the desired product nanocellulose with yield 65%.
- Step B Synthesis of NiO-Nanocellulose (NiO-NC) Hybrid Nanocomposites :
- Nickel oxide nanocellulose hybrid nanocomposites were synthesized by mixing nanocellulose with nickel chloride hexahydrate (NiCl 2 .6H 2 0) in alcoholic solvent-propanol and stirred the reaction for a period of 3 hrs at 43 °C to get transparent solution with weight ratio of NiCl 2 .6H 2 0 : nanocellulose as 1:2. After that sodium carbonate solution was added dropwise to the above reaction mixture with gentle stirring for 14 hrs at 82 °C and allowed to settle down. Centrifuging the reaction mixture to separate nickel oxide nanocellulose nanocomposites (NiO-NC) and washing with distilled water for several times to remove the byproducts. Sample was dried for 3 hrs at 92 °C to get the compound 5 with yield 65%.
- Step A Preparation of nanocellulose :
- Step I Dry powdered RS sample was extracted with non polar solvent - petroleum ether and polar solvent - propanol with the help of Soxhlet apparatus for 20 hrs at 56 °C to remove oil/wax etc.
- Step II After solvent extraction rice straw was dried in an oven for 1 hrs at 60 °C. Alkaline hydrolysis was done using mixture of 2% NaOH of 150 ml and 5% Na 2 C0 3 of 150 ml and stirred the mixture for 12 hours. The reaction mixture was then cooled and neutralized with 10% mineral acid -10 ml HC1 per 10 gm of pretreated rice straw. Filtered the biomass and treated with 10% H 2 0 2 solution of 20 ml per 10 gm of pretreated rice straw and stirred for 10 hrs at 45 °C. The reaction mixture was then cooled and filtered and then washed with distilled water for several times to get the desired product cellulose with the yield of 55%.
- Step III Cellulose was acid hydrolysed with 10% mineral acid -10 ml HC10 4 per 10 gm of cellulose. Reaction mixture was refluxed for 8 hrs at 85 °C. After that reaction mixture was filtered and washed with distilled water for several times to get the desired product nanocellulose with yield 50%.
- Step B Synthesis of NiO-Nanocellulose (NiO-NC) Hybrid Nanocomposites :
- Nickel oxide nanocellulose hybrid nanocomposites were synthesized by mixing nanocellulose with nickel chloride hexahydrate (NiCl 2 .6H 2 0) in alcoholic solvent and stirred the reaction for a period of 2 hrs at 42 °C to get transparent solution with weight ratio of NiCl 2 .6H 2 0 : nanocellulose as 1:2. After that sodium carbonate solution was added dropwise to the above reaction mixture with gentle stirring for 12 hrs at 72 °C and allowed to settle down, centrifuging the reaction mixture to separate nickel oxide nanocellulose nanocomposites (NiO-NC) and washing with distilled water for several times to remove the byproducts. Sample was dried for 2 hrs at 98 °C to get the compound 5 with yield 55%.
- NiO-Nanocellulose Hybrid Nanocomposites of formula 5:
- NiO-Nanocellulose (NiO-NC) Hybrid Nanocomposites of the formula 5 has shown good antimicrobial activity in general, which was determined by disc diffusion method as shown in Figure 1. a. Test microorganisms:
- Gram positive bacterias are Staphylococcus aureus MTCC
- Fungal strain Candida albicans MTCC3017 was also used to study. The bacterial strains were grown in nutrient broth at 30°C for 24 hours and the fungal strain was grown on potato dextrose broth at 30°C for 24 hours. Stocks were prepared by transferring 300 ⁇ 1 of liquid culture into test tubes containing 700 ⁇ 1 of 50% sterile glycerol and stored at -20-30°C.
- Nanocomposites were suspended in DMSO to make a concentration of 50 ⁇ g/ml and then diluted to 10 ⁇ g/ml and 5 ⁇ g/ml.20 ⁇ of these test samples were impregnated to 6 mm diameter sterile filter paper discs and allowed to air dry. Dried discs were placed under UV light for 30 mins. 100 ⁇ of the test bacteria were grown in 10 ml of nutrient broth at
- MNC showed inhibition zone against all tested microorganisms with the highest inhibition against Candida albicans (Fig.lA) of 15+lmm at concentration 50 ⁇ g/ml followed by bacillus toyonensis (Fig. IB) of 7+1 mm.
- Fig. lA Candida albicans
- Fig. IB bacillus toyonensis
- Pseudomonas putida (Fig. lC) and Staphylococcus aureus inhibition zones were 4.67+lmm and 5.33+lmm respectively at concentration of 50 ⁇ / ⁇ 1.
- a little inhibition zones were detected against Escherichia coli and Bacillus cereus. Zone of inhibition in millimeters is tabulated in Table 1.
- toyonensis and Bacillus cereus were 0.5 mg/ml and 2mg/ml. The remaining two bacteria under study showed inhibition at concentration of 1 mg/ml.
- Table 1 Zone of inhibition in millimeters of the product in disc diffusion method.
- Table 2 Minimum inhibitory concentration and sensitivity test against the strains.
- NiO-NC NiO-Nanocellulose
- the new and novel class of NiO-Nanocellulose (NiO-NC) Hybrid Nanocomposites of the formula 5 has also shown potent antifungal activity against plant pathogenic fungus Colletotrichum gleosporioides determined by using the poisoned food technique as shown in Figure 2. Colletotrichum gleosporioides with the inhibition percentage 98% as depicted in the Figure 2 which was determined by the standard antifungal activity test, viz., Poison Food Technique.
- Poisoned Food Technique was used to test the antifungal activity of the product of the formula 5 with six different concentrations of sample at 100, 200, 300, 400, 500, 600 ppm prepared in the particular solvent and used 1ml of each concentration was mixed with the freshly prepared, sterilized potato-dextrose agar media in petriplates (each 1ml sample was added to 20 ml of media), allowed them to mix homogeneously and to be solidified.
- Control growth medium contained equivalent amounts solvent and sterilized distilled water.
- Fungal disks of 5 mm in diameter from a 8-day-old pure culture were placed in the center of the Petri dish containing medium under aseptic condition, incubated at 27 +1 °C for 7 days. The experiments were carried out in three replicates per treatment. Fungal growth was observed at every 24 hrs. interval. At the end of the incubation period the mycelial growth was measured. The fungicidal nature of the sample was determined by testing revival of growth following transfer of the mycelial disk to an appropriate agar plate without sample. Percentage inhibition of mycelial growth was evaluated using the poisoned food techniques .
- NiO-NC NiO-Nanocellulose
- Synthesized nanocomposites have been found to possess good antimicrobial activity against (03) three gram positive and (02) two gram negative bacterial strains and fungal strain Candida albicans MTCC 3017.
- Gram positive bacteria are Staphylococcus aureus MTCC 6908, Bacillus toyonensis BCT 7112 and Bacillus cereus MTCC 1272; Gram negative bacteria are Pseudomonas putida ATCC 17642 and Escherichia coli MTCC 739.
- the invention provides for the production of nanocellulose in a very cost-effective and convenient method from a renewable agriculture resource, rice straw.
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Abstract
La présente invention concerne la synthèse d'une classe de nanocomposites hybrides de NiO-nanocellulose (NiO-NC) par un procédé monotope commode et la détermination de leurs activités antibactériennes et antifongiques. La présente invention concerne également un procédé de synthèse d'une nouvelle classe de nanocomposites hybrides de NiO-nanocellulose à partir de l'hexahydrate de chlorure de nickel (NiCl2.6H2O) de formule 1 et de nanocellulose (NC) de formule 2. La présente invention concerne en outre des activités antimicrobiennes contre (03) trois souches bactériennes à Gram positif et (02) deux souches bactériennes à Gram négatif et une souche fongique Candida albicans MTCC 3017. Les bactéries à Gram positif sont Staphylococcus aureus MTCC 6908, Bacillus toyonensis BCT 7112 et Bacillus cereus MTCC 1272, les bactéries à Gram négatif sont Pseudomonas putida ATCC 17642 et Escherichia coli MTCC 739, et la souche fongique est Candida albicans MTCC 3017 et une activité antifongique contre le champignon pathogène des plantes Colletotrichum gleosporioides. La présente invention concerne également la production d'une nanocellulose d'une manière très économique et commode à partir d'une ressource agricole renouvelable, la paille de riz.
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KR20220153373A (ko) * | 2021-05-11 | 2022-11-18 | 광운대학교 산학협력단 | 생물활성이 높고 세포 독성이 낮은 항균특성을 갖는 Si 기반 NiOOH 나노플라워의 제조 방법, MRSA, 녹농균, 폐렴간균에 대한 항균성 Si 기반 NiOOH 나노플라워, 및 이의 살균 방법 |
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
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WO2020059864A1 (fr) * | 2018-09-21 | 2020-03-26 | 丸紅株式会社 | Agent de lutte contre des pathogènes de plantes |
JPWO2020059864A1 (ja) * | 2018-09-21 | 2021-01-07 | 丸紅株式会社 | 植物病原菌防除剤 |
CN114711253A (zh) * | 2021-01-06 | 2022-07-08 | 合肥杰事杰新材料股份有限公司 | 抗菌剂及其制备方法和抗菌组合物 |
CN114711253B (zh) * | 2021-01-06 | 2024-02-20 | 合肥杰事杰新材料股份有限公司 | 抗菌剂及其制备方法和抗菌组合物 |
KR20220153373A (ko) * | 2021-05-11 | 2022-11-18 | 광운대학교 산학협력단 | 생물활성이 높고 세포 독성이 낮은 항균특성을 갖는 Si 기반 NiOOH 나노플라워의 제조 방법, MRSA, 녹농균, 폐렴간균에 대한 항균성 Si 기반 NiOOH 나노플라워, 및 이의 살균 방법 |
KR102620112B1 (ko) | 2021-05-11 | 2023-12-29 | 광운대학교 산학협력단 | 생물활성이 높고 세포 독성이 낮은 항균특성을 갖는 Si 기반 NiOOH 나노플라워의 제조 방법, MRSA, 녹농균, 폐렴간균에 대한 항균성 Si 기반 NiOOH 나노플라워, 및 이의 살균 방법 |
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