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1.
Anal Chim Acta ; 875: 83-91, 2015 May 22.
Article in English | MEDLINE | ID: mdl-25937109

ABSTRACT

A typical, reproducible, and rugged screen printed carbon electrode, modified with dual-ion imprinted beads, was fabricated employing the "surface grafting from" approach. For this, the acyl chloride functionalized magnetic nanoparticles were first immobilized and chemically attached with a typical functional monomer (but-2-enedioic acid bis-[(2-amino-ethyl)-amide]) on the electrode surface. This was subsequently subjected to the thermal polymerization in the presence of template ions (Ce(IV) and Gd(III)), cross-linker (ethylene glycol dimethacrylate), initiator (AIBN), and multiwalled carbon nanotubes. The modified sensor was used for the simultaneous analysis of both template ions in aqueous, blood serum, and waste-water samples, using differential pulse anodic stripping voltammetry which revealed two oxidation peaks for respective templates with resolution as much as 950 mV, without any cross reactivity, interferences and false-positives. The detection limits realized by the proposed sensor, under optimized conditions, were found to be as low as 0.07 ng mL(-1) for Ce(IV) and 0.19 ng mL(-1) for Gd(III) (S/N=3) that could eventually be helpful for lanthanide estimation at stringent levels.

2.
Biosens Bioelectron ; 59: 81-8, 2014 Sep 15.
Article in English | MEDLINE | ID: mdl-24704689

ABSTRACT

A rapid, selective, and sensitive double-template imprinted polymer nanofilm-modified pencil graphite electrode was fabricated for the simultaneous analysis of phosphorus-containing amino acid-type herbicides (glyphosate and glufosinate) in soil and human serum samples. Since both herbicides respond overlapped oxidation peaks and only glyphosate is prone to nitrosation, n-nitroso glyphosate and glufosinate were used as templates for obtaining the well-resolved quantitative differential pulse anodic stripping voltammetric peaks on the proposed sensor. Toward sensor fabrication, a nano-structured polymer film was first grown directly on the electrode via initial immobilization of gold nanoparticles at its surface. This was followed by linking of monomeric (N-methacryloyl-l-cysteine) molecules through S-Au bonds. Subsequently, these molecules were subjected to free radical polymerization, in the presence of templates, cross linker, initiator, and multiwalled carbon nanotubes as pre-polymer mixture. The modified sensor observed wide linear ranges (3.98-176.23 ng mL(-1) and 0.54-3.96 ng mL(-1)) of simultaneous analysis with detection limits as low as 0.35 and 0.19 ng mL(-1) (S/N=3) for glyphosate and glufosinate, respectively, in aqueous samples. The respective oxidation peak potentials of both analytes were found to be substantially apart by 265 mV. This enabled the simultaneous determination of one target in the presence of other, without any cross reactivity, interferences, and false-positives, in real samples.


Subject(s)
Aminobutyrates/analysis , Electrochemical Techniques/instrumentation , Glycine/analogs & derivatives , Herbicides/analysis , Molecular Imprinting , Polymers/chemistry , Aminobutyrates/blood , Equipment Design , Glycine/analysis , Glycine/blood , Herbicides/blood , Humans , Limit of Detection , Nanostructures/chemistry , Soil/chemistry , Water/analysis , Glyphosate
3.
Talanta ; 120: 398-407, 2014 Mar.
Article in English | MEDLINE | ID: mdl-24468388

ABSTRACT

In simultaneous determination of group of elements, there are inter-metallic interactions which result in a non-linear relationship between the peak current and ionic concentration for each of the element, at bare (unmodified) electrode. To resolve this problem, we have resorted, for the first time, to develop a modified pencil graphite electrode using a typical ion imprinted polymer network (dual-ion imprinted polymer embedded in sol-gel matrix (inorganic-organic hybrid nano-material)) for the simultaneous analysis of a binary mixture of Cd(II) and Cu(II) ions, without any complication of inter-metallic interactions and competitive bindings, in real samples. The adequate resolution of differential pulse anodic stripping voltammetry peaks by 725 mV (cf, 615 mV with unmodified electrode), without any cross-reactivity and the stringent detection limits as low as, 0.050 and 0.034 ng mL(-1) (S/N=3) for Cd(II) and Cu(II) ions, respectively by the proposed sensor can be considered useful for the primitive diagnosis of several chronic diseases in clinical settings.


Subject(s)
Cadmium/analysis , Copper/analysis , Molecular Imprinting/methods , Animals , Cadmium/blood , Cattle , Copper/blood , Electrochemical Techniques/methods , Humans , Lakes/analysis , Limit of Detection , Milk/chemistry , Phase Transition , Polymers/chemistry
4.
Biosens Bioelectron ; 50: 19-27, 2013 Dec 15.
Article in English | MEDLINE | ID: mdl-23831643

ABSTRACT

A dual-template imprinted polymer film containing dispersed multiwalled carbon nanotubes was exploited in the fabrication of a typical, reproducible, and rugged carbon ceramic electrode, adopting "surface grafting from" approach for the growth of a nanometer thin coating on its surface. For this, chloro groups were first introduced at the exterior surface of silica-carbon composite electrode through sol-gel modification using (3-chloropropyl)-trimethoxysilane, followed by an iniferter (sodium diethyl dithiocarbamate) initiated photopolymerization of functional monomer (2,4,6-trisacrylamido-1,3,5-triazine), mixed templates (ascorbic acid and dopamine), and cross-linker (ethylene glycol dimethacrylate), in the presence of multiwalled carbon nanotubes. The modified sensor was validated for the simultaneous analysis of ascorbic acid and dopamine in aqueous, blood serum, cerebrospinal fluid, and pharmaceutical samples, using differential pulse anodic stripping voltammetric technique. The oxidation peak potentials for both analytes were found to be well apart approximately by 300 mV, which was large enough to allow selective and sensitive analysis of one in the presence of other, without any cross reactivity, interferences and false-positives. The detection limits realized by the proposed sensor, under optimized conditions, were found to be as low as 2.24 ng mL(-1) for ascorbic acid and 0.21 ng mL(-1) for dopamine (S/N=3). Such stringent limits could be considered suitable for the primitive diagnosis of several chronic diseases, in clinical settings.


Subject(s)
Ascorbic Acid/blood , Ascorbic Acid/cerebrospinal fluid , Biosensing Techniques/methods , Dopamine/blood , Dopamine/cerebrospinal fluid , Molecular Imprinting , Ascorbic Acid/analysis , Carbon/chemistry , Ceramics/chemistry , Dopamine/analysis , Electrodes , Humans , Limit of Detection , Nanotubes, Carbon/chemistry , Pharmaceutical Preparations/chemistry , Polymers/chemistry , Silicon Dioxide/chemistry
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