研究目的
Design and synthesize a novel rhodamine-based probe for selective fluorescent detection of Au3+ and colorimetric detection of Cu2+ ions in aqueous acetonitrile.
研究成果
The rhodamine-based chemosensor RC effectively provides selective fluorescent detection of Au3+ and colorimetric detection of Cu2+ in aqueous-organic media, with high sensitivity and minimal interference from other ions. The approach of using complementary receptors enhances selectivity and multi-sensing capabilities, offering a viable tool for future probe design in environmental and analytical applications.
研究不足
The probe shows cross-sensitivity where Au3+ and Pt4+ can intensify the fluorescent response for Cu2+ detection, though this is manageable with standard addition methods. The response time is slower for Au3+ (11 minutes) compared to Cu2+ (3 minutes). The system is complex due to multiple binding sites, which may affect selectivity in mixed ion environments.
1：Experimental Design and Method Selection:
The probe RC was synthesized by introducing a 1-aza-4,13-dithia-15-crown-5 ring into rhodamine 6G hydrazide. Spectroscopic experiments were conducted in aqueous acetonitrile (1/1, v/v) at pH 7.0 using HEPES buffer. The sensing mechanism involves reversible spirolactam-amide conversion and photoinduced electron transfer (PET) effects.
2：0 using HEPES buffer. The sensing mechanism involves reversible spirolactam-amide conversion and photoinduced electron transfer (PET) effects. Sample Selection and Data Sources:
2. Sample Selection and Data Sources: Metal ions tested included Ag+, Ca2+, Mn2+, Co2+, Ni2+, Cu2+, Zn2+, Pd2+, Ba2+, Hg2+, Pb2+, Al3+, Cr3+, Fe3+, Eu3+, Tb3+, Au3+, and Pt4+ (as chloride complexes or nitrate salts). Solutions were prepared using deionized water and analytical grade reagents.
3：List of Experimental Equipment and Materials:
Equipment: Perkin Elmer Spectrum 100BX II FT-IR spectrometer, Bruker Avance 400 NMR spectrometer, Shimadzu LCMS-2010 mass spectrometer, Shimadzu UV-1800 spectrophotometer, Shimadzu RF-6000 spectrofluorophotometer, Sartorius Professional Meter PP-50 pH meter. Materials: Rhodamine 6G, DMF, N-phenyldiethanolamine, POCl3, hexane, chloroform, 1,2-bis(2-mercaptoethoxy)ethane, N2H4·H2O, Cs2CO3, silica gel, ethanol, chloroform/ethylacetate eluent, HEPES buffer.
4：Experimental Procedures and Operational Workflow:
Synthesis involved refluxing compounds in ethanol, purification by column chromatography. Spectroscopic experiments: RC stock solution (2×10-5 M in acetonitrile) diluted with HEPES buffer, metal ion solutions added, equilibrated for 60 min, then UV-VIS and fluorescence measurements taken.
5：Data Analysis Methods:
Detection limits calculated based on signal-to-noise ratio of three. Binding stoichiometry determined by Job's method. Stability constants calculated from experimental data using the law of mass action. Response kinetics monitored over time.
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Spectrometer
Spectrum 100BX II
Perkin Elmer
Record Fourier transform infrared radiation (FT-IR) spectra of compounds in the range 400-4000 cm-1 using KBr pellets.
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NMR Spectrometer
Avance 400
Bruker
Perform 1H and 13C NMR spectra with proton resonance frequency of 400 MHz using CDCl3 as solvent and tetramethylsilane as internal reference.
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Mass Spectrometer
LCMS-2010
Shimadzu
Perform mass spectrometry using LC-ESI/MS system.
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Spectrophotometer
UV-1800
Shimadzu
Perform UV-VIS measurements using 1 cm path length cuvettes at room temperature.
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Spectrofluorophotometer
RF-6000
Shimadzu
Perform fluorescence measurements using 1 cm path length cuvettes at room temperature.
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pH Meter
PP-50
Sartorius
Carry out pH measurements.
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