研究目的
To synthesize and characterize a novel imine-substituted cobalt phthalocyanine complex and apply it for the electrochemical detection and sensing of L-cysteine.
研究成果
The novel cobalt tetrabromo imine phthalocyanine complex was successfully synthesized and characterized, demonstrating good thermal stability and electrochemical activity. The modified electrode enabled sensitive and selective detection of L-cysteine at nanomolar levels with high sensitivity and low detection limits, showing potential for real-sample applications such as in commercial tablets and human urine.
研究不足
The synthesized complex has limited solubility in organic solvents, which may lead to aggregation over time. The electrode modification may result in slower electron transfer kinetics due to the resistive film. The study is focused on L-cysteine detection and may not be directly applicable to other biomolecules without further modification.
1:Experimental Design and Method Selection:
The study involved synthesizing a novel cobalt phthalocyanine complex with imine substituents, characterizing it using various spectroscopic and analytical techniques, and immobilizing it on a glassy carbon electrode for electrochemical sensing of L-cysteine. Methods included cyclic voltammetry, amperometry, and impedance spectroscopy.
2:Sample Selection and Data Sources:
The complex was synthesized from precursors like 4-nitrophthalonitrile and p-bromoaniline. L-cysteine solutions were prepared in phosphate buffer (pH 7.4) for electrochemical measurements.
3:4) for electrochemical measurements. List of Experimental Equipment and Materials:
3. List of Experimental Equipment and Materials: Equipment included Vario EL III CHNS elemental analyzer, Ocean optics spectrometer, FTIR Perkin Elmer Spectrum-Two spectrophotometer, Bruker D8 Advance X-ray diffractometer, STA6000 thermal analyzer, 500 MHz Varian NMR instrument, Agilent 6100 GC/MS, CHI620E electrochemical analyzer, and a three-electrode cell with glassy carbon, Ag/AgCl, and platinum electrodes. Materials included cobalt(II) chloride, 4-nitrophthalonitrile, DBU, p-bromoaniline, sodium hydroxide, salicylaldehyde, potassium carbonate, L-cysteine, potassium ferrocyanide, TBAP, n-pentanol, methanol, ethanol, acetone, n-hexane, DMF, DMSO, hydrochloric acid, sulphuric acid, and nafion binder.
4:Experimental Procedures and Operational Workflow:
Synthesis involved refluxing precursors, purification, and characterization. Electrode modification was done by drop-casting the complex ink on GCE. Electrochemical experiments were performed in N2 atmosphere with cyclic voltammetry, amperometry, and impedance measurements for L-cysteine detection.
5:Data Analysis Methods:
Data were analyzed using linear regression for calibration curves, equivalent circuit fitting for impedance, and standard formulas for capacitance and surface coverage calculations.
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Spectrometer
Ocean optics, serial number FLMSO4808
Ocean Optics
Recorded UV-Vis spectra in the 300–800 nm range.
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FTIR Spectrophotometer
Perkin Elmer Spectrum-Two
Perkin Elmer
Recorded FT-IR spectra using KBr pellet method.
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X-ray Diffractometer
Bruker D8 Advance
Bruker
Recorded powder X-ray diffraction patterns.
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GC/MS Instrument
6100 series
Agilent Technologies
Used for mass analysis of synthesized compounds.
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Electrochemical Analyzer
CHI620E
CH Instruments
Used for electrochemical studies including cyclic voltammetry and amperometry.
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Elemental Analyzer
Vario EL III
Not specified
Used for elemental analysis of the synthesized complex.
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Thermal Analyzer
STA6000
Not specified
Studied thermal stability via thermogravimetric analysis.
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NMR Instrument
500 MHz Varian
Varian
Used for NMR studies of precursors and ligands.
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Glassy Carbon Electrode
CHI104
CH Instruments Inc.
Used as working electrode for electrochemical detection.
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Reference Electrode
Saturated Ag/AgCl
Not specified
Used as reference electrode in electrochemical cell.
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Counter Electrode
Platinum wire
Not specified
Used as counter electrode in electrochemical cell.
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Polishing Cloth
Micro Cloth
Buehler
Used for polishing the glassy carbon electrode.
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