研究目的
Detection of copper and mercury ions in environmental and biological systems using a synthesized rhodanine-based fluorescent sensor.
研究成果
The synthesized 2-OxI-Rh probe is a non-toxic, selective turn-on sensor for Hg2+ and Cu2+ ions, with 1:1 binding ratios, binding constants of 2.15×104 M?1 for Hg2+ and 1.21×104 M?1 for Cu2+, and LOD values of 3.36 μM and 2.31 μM, respectively. It is effective in different solvent systems and has potential applications in environmental monitoring and biological sensing.
研究不足
The sensor may have limitations in detecting mercury ions in forms other than chlorides (e.g., acetates, nitrates, iodides showed some variations). The probe's performance could be affected by solvent composition and pH, and it may not be suitable for all environmental matrices without optimization.
1:Experimental Design and Method Selection:
The study involved synthesizing a rhodanine-based probe (2-OxI-Rh) via a green approach and evaluating its sensing properties for metal ions using colorimetric and fluorometric techniques. Theoretical models include Job's plot for binding ratio and Benesi-Hildebrand equation for binding constants.
2:Sample Selection and Data Sources:
Samples included the synthesized probe 2-OxI-Rh and various metal ions (e.g., Hg2+, Cu2+) as chloride salts. Data were acquired from UV-Vis and fluorescence spectroscopy measurements.
3:List of Experimental Equipment and Materials:
Equipment included a Buchi 539 capillary melting apparatus for melting points, Mattson 1000 FT-IR spectrophotometer for IR spectra, Varian and Bruker spectrometers for NMR, LECO CHNS-932 for elemental analysis, silica gel for chromatography, TLC plates, JEOL JES-FA300 ESR spectrometer for ESR, Shimadzu UV-3101PL UV-Vis-NIR spectrometer for UV-Vis, and Perkin-Elmer LS 55 Fluorescence Spectrophotometer for fluorescence. Materials included chemicals from Sigma-Aldrich or Merck, ethanol, HEPES buffer, HClO4, NaOH, and various metal salts.
4:Experimental Procedures and Operational Workflow:
Synthesis of 2-OxI-Rh involved heating 3-amino-rhodanine and isatin in ethanol. Sensing studies involved preparing solutions of probe and ions, recording UV-Vis and fluorescence spectra after adding ions, performing titrations, Job's plot measurements, and competitive experiments. pH studies were conducted using HClO4 or NaOH to modulate pH.
5:Data Analysis Methods:
Data were analyzed using Job's plot for binding stoichiometry, Benesi-Hildebrand equation for binding constants, and standard formulas for LOD and LOQ. Statistical techniques included linear regression (R2 values).
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elemental analyzer
LECO CHNS-932
LECO
Performing elemental analysis.
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ESR spectrometer
JEOL JES-FA300
JEOL
Recording ESR spectra to study radical formation.
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UV-Vis spectrometer
Shimadzu UV-3101PL UV-Vis-NIR
Shimadzu
Recording UV-Vis absorption spectra.
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fluorescence spectrophotometer
Perkin-Elmer LS 55
Perkin-Elmer
Recording fluorescence spectra.
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capillary melting apparatus
Buchi 539
Buchi
Determining melting points of synthesized compounds.
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FT-IR spectrophotometer
Mattson 1000
Mattson
Recording infrared spectra of compounds.
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NMR spectrometer
400 MHz Varian, 100 MHz Bruker
Varian, Bruker
Recording 1H and 13C NMR spectra.
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silica gel
60 (230–400 mesh ASTM)
Used in column chromatography for purification.
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TLC plates
Merck Fertigplatten Kieselgel (60 F254)
Merck
Monitoring reaction progress by thin-layer chromatography.
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