研究目的
To develop a permanent photo-antimicrobial cellulosic material by covalently linking protoporphyrin IX onto Lyocell fibers using azide-alkyne click chemistry for applications in antimicrobial textiles.
研究成果
The covalent attachment of protoporphyrin IX to Lyocell fibers via click chemistry successfully imparted permanent photo-antibacterial activity, effective against Staphylococcus aureus and Bacillus subtilis under light illumination. This approach offers a durable antimicrobial treatment for cellulosic materials, with potential applications in healthcare and textiles.
研究不足
The low surface area of Lyocell fibers limits grafting yield and reactivity. The modification process requires multiple steps and specific conditions, which may not be scalable. Antimicrobial testing was only against two bacterial strains and under specific light conditions, potentially limiting generalizability.
1:Experimental Design and Method Selection:
The study employed an azide-alkyne click chemistry approach for covalent modification. Lyocell fibers were pre-modified with (3-azidopropyl)triethoxysilane to introduce azide groups, and protoporphyrin IX was alkynylated via Steglich esterification. A copper-catalyzed azide-alkyne cycloaddition (CuAAC) was used for covalent linkage.
2:Sample Selection and Data Sources:
Lyocell fibers (TENCEL VR) were provided by Lenzing AG. Bacterial strains (Staphylococcus aureus and Bacillus subtilis) were used for antimicrobial testing.
3:List of Experimental Equipment and Materials:
Equipment included FTIR spectrometer (PerkinElmer Frontier), NMR spectrometers (Bruker Avance III HD 400 and Bruker Avance II 400), UV/Vis spectrophotometer (PerkinElmer Lambda 35), SEM (FEI INSPECT S50), elemental analyzer (EURO EA 3000 CHNS-O), and LED panels (Optonica DL2352). Materials included protoporphyrin IX, propargyl alcohol, EDC hydrochloride, DMAP, (3-chloropropyl)triethoxysilane, sodium azide, TBAB, copper(II) sulfate pentahydrate, L-ascorbic acid, and various solvents.
4:2). Materials included protoporphyrin IX, propargyl alcohol, EDC hydrochloride, DMAP, (3-chloropropyl)triethoxysilane, sodium azide, TBAB, copper(II) sulfate pentahydrate, L-ascorbic acid, and various solvents. Experimental Procedures and Operational Workflow:
4. Experimental Procedures and Operational Workflow: Fibers were swollen in solvents (water, DMSO, DMAc, NaOH, urea), then modified with azidosilane in aqueous NaOH. Alkynylated protoporphyrin was synthesized and attached via CuAAC in DMF with CuSO4 and ascorbic acid. Fibers were washed and characterized. Antimicrobial activity was tested by placing fibers on bacterial lawns under light and dark conditions.
5:Data Analysis Methods:
Characterization involved FTIR, NMR, UV/Vis spectroscopy, elemental analysis, SEM, and EDX. Antimicrobial activity was assessed by visual inspection of inhibition zones.
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FTIR spectrometer
PerkinElmer Frontier
PerkinElmer
Characterization of chemical bonds and functional groups in modified fibers.
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NMR spectrometer
Bruker Avance III HD 400
Bruker
Structural analysis of compounds and modified fibers.
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NMR spectrometer
Bruker Avance II 400
Bruker
Structural analysis of compounds.
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UV/Vis spectrophotometer
PerkinElmer Lambda 35
PerkinElmer
Measurement of absorption spectra for porphyrin compounds.
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SEM
FEI INSPECT S50
FEI
Imaging and analysis of fiber morphology and surface modifications.
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Lyocell fibers
TENCEL VR
Lenzing AG
Base cellulosic material for modification and antimicrobial testing.
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Elemental analyzer
EURO EA 3000 CHNS-O
HEKAtech
Determination of elemental composition (C, H, N, S, O) of modified fibers.
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LED panel
Optonica DL2352
Optonica
Light source for photobactericidal activity testing.
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