Silsesquioxane organofunctionalized with 4-amino-3-hydrazino-5-mercapto-1,2,4-triazole: Preparation and subsequent reaction with silver and potassium hexacyanoferrate(III) for detection of l-cysteine

The octakis(3-chloropropyl)octasilsesquioxane (SS) was organofunctionalized with 4-amino-3-hydrazino-5-mercapto-1,2,4-triazole (Purpald). The functionalized silsesquioxane with Purpald (SP) was characterized by Fourier transform infrared spectroscopy (FT-IR), and nuclear magnetic resonance (NMR). Af...

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Bibliographic Details
Published in:Materials Science & Engineering C 2015-12, Vol.57, p.24-30
Main Authors: do Carmo, Devaney R., Silvestrini, Daniela R., da Silveira, Tayla F.S., Cumba, Loanda R., Dias Filho, Newton L., Soares, Layciane A.
Format: Article
Language:English
Subjects:
Chemical synthesis
Conductometry - instrumentation
Cysteine - analysis
Electrochemical properties
Electrodes
Equipment Design
Equipment Failure Analysis
Ferricyanides - chemistry
Fourier transforms
Infrared spectroscopy
Mathematical analysis
Nanocomposites - chemistry
Nanocomposites - ultrastructure
Nuclear magnetic resonance
Nuclear magnetic resonance (NMR)
Organosilicon Compounds - chemistry
Pastes
Potassium
Reproducibility of Results
Scanning electron microscopy
Sensitivity and Specificity
Silver - chemistry
Structural materials
Sulfhydryl Compounds
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Summary:The octakis(3-chloropropyl)octasilsesquioxane (SS) was organofunctionalized with 4-amino-3-hydrazino-5-mercapto-1,2,4-triazole (Purpald). The functionalized silsesquioxane with Purpald (SP) was characterized by Fourier transform infrared spectroscopy (FT-IR), and nuclear magnetic resonance (NMR). After functionalized, silsesquioxane can interact with silver nitrate and subsequently with potassium hexacyanoferrate (III) (AgHSP). The novel hybrid composite formed (AgHSP) was characterized by Fourier transform infrared spectra, scanning electron microscopy (SEM), and energy dispersive X-ray spectroscopy (EDX). AgHSP was electrochemically characterized by cyclic voltammetry (CV) using graphite paste electrode. The AgHSP incorporated into a graphite paste electrode (20% w/w) was tested for detection of l-cysteine. The modified electrode showed a linear response from 9.0×10−5 to 5.0×10−3molL−1 with the corresponding equation Y(A)=0.01315+1.865 [l-cysteine], and a correlation coefficient of r2=0.9995. The method showed a detection limit of 1.76×10−4molL−1 with a relative standard deviation of ±2% (n=3) and amperometric sensitivity of 1.865A/molL−1. [Display omitted] •Functionalization of silsesquioxane with Purpald compound•Characterization of silsesquioxane was done with FT-IR, NMR, SEM, EDX and VC.•The modified silsesquioxane was interacted with AgNO3 and K3[Fe(CN)6].•The composite was tested by cyclic voltammetry for detection of l-cysteine.
ISSN:0928-4931
1873-0191
DOI:10.1016/j.msec.2015.07.023