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1.
Anal Chim Acta ; 1034: 46-55, 2018 Nov 30.
Article in English | MEDLINE | ID: mdl-30193639

ABSTRACT

In this study, for the first time a rapid, selective and highly sensitive method was developed for simultaneous determination of warfarin and mycophenolic acid using carbon paste electrode modified by ß-cyclodextrin/multi-walled carbon nanotubes/cobalt oxide nanoparticles (ß-CD/MWCNTs/Co3O4NPs/CPE). The oxidation peaks of desired drugs was separated enough using the constructed electrode. Cyclic voltammetry (CV) and differential pulse voltammetry (DPV) were utilized for study the electrochemical response of the fabricated electrode and its surface modification was investigated by electrochemical impedance spectroscopy (EIS). Under optimal conditions, the adsorptive stripping voltammetric responses were linear in the concentration ranges 0.05-150 µM and 0.5-200 µM for WAR and MPA, respectively. The correlation coefficients were greater than 0.99. The limits of detection for WAR and MPA were 0.02 and 0.03 µM. The fabricated electrode was applied for the simultaneous determination of WAR and MPA in urine and human serum samples with satisfactory results.


Subject(s)
Electrochemical Techniques , Hydroxybenzoates , Warfarin , Adult , Carbon/chemistry , Electrodes , Humans , Hydroxybenzoates/blood , Hydroxybenzoates/urine , Male , Warfarin/blood , Warfarin/urine
2.
Anal Biochem ; 520: 1-8, 2017 03 01.
Article in English | MEDLINE | ID: mdl-28027887

ABSTRACT

A simple and sensitive method based on adsorptive anodic stripping differential pulse voltammetry (AASDPV) for the determination of cellcept, using a magnetic Fe3O4 nanoparticles and functionalized (carboxylated) multi-walled carbon nanotubes modified glassy carbon electrode (f-MWCNs/Fe3O4/GCE) was developed. In phosphate buffer solution (pH = 5), the voltammogram of cellcept exhibited tow anodic peaks and the well-defined peak at about 0.611 V vs SCE was used for its monitoring. The modified electrode was characterized by different methods such as electrochemical impedance spectroscopy (EIS), scanning electron microscopy (SEM) and cyclic voltammetry (CV). The experimental parameters, such as pH, deposition potential and time, as well as scan rate were optimized. Under the optimized conditions, Ip (µA) was proportional to the cellcept concentration in the range of 0.05-200 µM (R2 = 0.9989) with a detection limit of 9.0 nM and limit of quantification of 30.2 nM. The recovery was >98%. The practical analytical utilities of the modified electrode were demonstrated by the determination of cellcept in human urine and blood serum samples. Modified electrode showed an adequate sensitivity and stability for evaluated samples.


Subject(s)
Electrochemical Techniques , Ferrosoferric Oxide/chemistry , Magnetite Nanoparticles/chemistry , Mycophenolic Acid/analysis , Nanotubes, Carbon/chemistry , Adsorption , Carbon/chemistry , Dielectric Spectroscopy , Electrodes , Humans , Hydrogen-Ion Concentration , Limit of Detection , Microscopy, Electron, Scanning , Mycophenolic Acid/blood , Mycophenolic Acid/urine , Oxidation-Reduction , Reproducibility of Results , Sonication
3.
J Hazard Mater ; 160(2-3): 468-72, 2008 Dec 30.
Article in English | MEDLINE | ID: mdl-18420343

ABSTRACT

A method was proposed for the preconcentration of some transition elements at trace levels using a column packed with silica gel modified by a synthetic ligand. Metal ions were adsorbed on 2,4,6-trimorpholino-1,3,5-triazin modified silica gel, then analytes retained on the adsorbent were eluted by 1molL(-1) hydrochloric acid and determined by flame atomic absorption spectrometry (FAAS). The influences of some experimental parameters including pH of the sample solution, weight of adsorbent, type, concentration and volume of eluent, flow rates of the sample solution and eluent, and sample volume on the preconcentration efficiency have been investigated. The influences of some matrix elements were also examined. The method also was used for simultaneous preconcentration of these elements and the method was successfully applied to the preconcentration and determination of them. The detection limits of the method for Ni2+, Co2+, Cd2+ and Zn2+were 0.29, 0.20, 0.23 and, 0.30ngmL(-1), respectively. The application of this modified silica gel to preconcentration of investigated cation from tap water, lake water, urine and apple leaves gave high accuracy and precision (relative standard deviation (R.S.D.) <3%).


Subject(s)
Environmental Pollutants/analysis , Morpholines/analysis , Trace Elements/analysis , Triazines/analysis , Cobalt/urine , Humans , Hydrogen-Ion Concentration , Indicators and Reagents , Malus/chemistry , Nickel/analysis , Plant Leaves/chemistry , Silica Gel , Silicon Dioxide , Solid Phase Extraction , Spectrophotometry, Atomic
4.
J Hazard Mater ; 128(1): 67-72, 2006 Jan 16.
Article in English | MEDLINE | ID: mdl-16125306

ABSTRACT

A new modified silica gel using 2,4,6-trimorpholino-1,3,5-triazin was used for separation, preconcentration and determination of silver ion in natural water by atomic absorption spectrometry (AAS). This new bonded silica gel was used as an effective sorbent for the solid-phase extraction (SPE) of silver ion from aqueous solutions. Experimental conditions for effective adsorption of trace levels of silver ion were optimized with respect to different experimental parameters in column process. Common coexisting ions did not interfere with the separation and determination of silver at pH 3.5 so that silver ion completely adsorbed on the column. The preconcentration factor is 130 (1 mL elution volume for a 130 mL sample volume). The relative standard deviation (R.S.D.) under optimum conditions is 3.03% (n=5). The accuracy of the method was estimated by using spring and tap water samples that were spiked with different amounts of silver ion. The adsorption isotherm of silver ion was obtained. The capacity of the sorbent at optimum conditions has been found to be 384 microg of silver per gram of sorbent.


Subject(s)
Silicon Dioxide/chemistry , Silver/isolation & purification , Triazines/chemistry , Water Pollutants, Chemical/isolation & purification , Adsorption , Hydrogen-Ion Concentration , Silica Gel , Silver/chemistry , Thiosulfates/chemistry
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