Your browser doesn't support javascript.
loading
Mostrar: 20 | 50 | 100
Resultados 1 - 20 de 22
Filtrar
Mais filtros










Base de dados
Intervalo de ano de publicação
1.
Anal Chim Acta ; 1312: 342721, 2024 Jul 11.
Artigo em Inglês | MEDLINE | ID: mdl-38834258

RESUMO

This study reports a fast and visual detection method of antidepressant sertraline (SRT) drug by the core-shell AuNPs@CDs as the nanoprobes. The CDs has been eco-friendly synthesized from sweet lemon wastes to directly reduce Au+ to AuNPs without any external photoirradiation process or additional reductants. Optimizing key variables that impact the sensing process has been done using the central composite design (CCD) approach to simulate the assay condition before the analysis. Adding SRT with different concentrations to the nanoprobes under mildly acidic conditions presents an absorbance peak at 560 nm with purple color tonalities that differ from the behavior of alone nanoprobes (530 nm, pink color). The obtained absorption change is linearly proportional to the increase of SRT concentration from 1 µM to 35 µM with a limit of detection (LOD) value of 100 nM. The color changes with a vivid tonality from pink and purple to violet as the colorful fingerprint patterns are readily traceable by the naked eye, allowing the visual assay of SRT. The greenness of the developed approach is well evaluated by some international indexes including the complimentary green analytical procedure (ComplexGAPI) and also, the analytical greenness (AGREE) indexes. The proposed waste-derived nanoprobes based on the eco-friendly procedure not only conduct quantitative and qualitative non-invasive analysis of SRT by the naked eye but also, may widen for other applications in various fields.


Assuntos
Compostos de Cádmio , Ouro , Nanopartículas Metálicas , Sertralina , Sulfetos , Ouro/química , Nanopartículas Metálicas/química , Sertralina/análise , Sertralina/química , Sulfetos/química , Compostos de Cádmio/química , Citrus/química , Colorimetria/métodos , Limite de Detecção , Antidepressivos/análise
2.
Mikrochim Acta ; 191(3): 168, 2024 02 29.
Artigo em Inglês | MEDLINE | ID: mdl-38418635

RESUMO

The interaction of Cu-tannic acid nanosheets (Cu-TA NShs) as nanozyme in a surfactant solution of CTAB under relatively acidic conditions is shown to exhibit a catalytic effect on quercetin (Qur). This catalytic property of Cu-TA NShs, which mimics laccase enzyme with many advantages, has been applied to developing a selective colorimetric sensor for the determination of trace amounts of Qur in vegetable samples. This strategy presents a desirable linear relationship between the absorbance signal intensity and the concentrations of Qur from 0.350 to 32.09 µM with a detection limit (LOD) of 0.064 µM (S/N = 3). The feasibility of the proposed portable colorimetric sensor for in situ analysis of the real samples has been validated with the high-performance liquid chromatography (HPLC) method as reference method, and two-tailed test (t test) statistical analysis certifies good agreement between the results. This enzyme-free and sensitive naked-eye sensor with the smartphone-based color map is promising to provide technical support for the rapid and visual detection of Qur in vegetables.


Assuntos
Colorimetria , Polifenóis , Quercetina , Lacase , Smartphone , Verduras
3.
Anal Bioanal Chem ; 415(14): 2665-2676, 2023 Jun.
Artigo em Inglês | MEDLINE | ID: mdl-37010560

RESUMO

For the hyphenating of dispersive liquid-liquid microextraction (DLLME) with nano mesoporous solid-phase evaporation (SPEV) as a novel method, MCM-41@SiO2 was synthesized and used as a nano mesoporous adsorbent for coating on the solid-phase fiber, preconcentration of fluoxetine antidepressant drug (as a model compound), and total evaporation of the extraction solvents obtained by the DLLME method. To detect the analyte molecules, a corona discharge ionization-ion mobility spectrometer (CD-IMS) was applied. In order to increase the extraction efficiency and the IMS signal of the fluoxetine drug, some variables including extraction solvent and its volume, disperser solvents and its volume, sample solution pH, desorption temperature, and evaporation time of the solvent from the solid-phase fiber were chosen and optimized. Some analytical parameters including limit of detection (LOD), limit of quantification (LOQ), linear dynamic range (LDR) with determination coefficient, and relative standard deviations (RSDs) were calculated under the optimized conditions. LOD (S/N = 3), 3 ng mL-1; LOQ (S/N = 10), 10 ng mL-1; LDR, 10-200 ng mL-1; and intra- and inter-day RSDs (n = 3), 2.5% and 9.6% for 10 ng mL-1, and 1.8% and 7.7% for 150 ng mL-1, respectively. To investigate the ability of the hyphenated method to determine fluoxetine in real samples, fluoxetine tablets, and some biological samples such as human urine and blood plasma were selected and the relative recovery values were calculated to be 85-110%. The accuracy of the proposed method was compared with that of the HPLC standard method.


Assuntos
Fluoxetina , Microextração em Fase Líquida , Humanos , Dióxido de Silício , Espectrometria de Mobilidade Iônica , Microextração em Fase Líquida/métodos , Solventes/química , Limite de Detecção
4.
Spectrochim Acta A Mol Biomol Spectrosc ; 296: 122665, 2023 Aug 05.
Artigo em Inglês | MEDLINE | ID: mdl-37011439

RESUMO

In the present study, bimetallic nanoparticles (NPs) consisting of gold (AuNPs) as the core and silver (AgNPs) as the shell have been synthesized and applied as the nanoprobe for detection of fluvoxamine (FXM) as the anti-depression drug. The physicochemical properties of the prepared citrate-capped Au@Ag core-shell NPs have been characterized by UV-Vis, Fourier-transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM) and scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDX) techniques. The design of the smartphone-based colorimetric FXM sensor relies on the fast hydrolysis of FXM under alkaline conditions by producing of 2-(Aminooxy)ethanamine without any significant peak at 400-700 nm. The interaction of the resulted molecule with the nanoprobe induced a red shift in the longitudinal localized surface plasmon resonance (LSPR) peak of the nanoprobe, which was accompanied by sharp and vivid color variations in the solution. A linear relationship between the absorption signal increasing by FXM concentration increasing from 1 µM to 10 µM presented a simple, low cost and minimally instrumented format for FXM quantification with a limit of detection (LOD) of 100 nM. The collected visual data with the elegant colorimetric response of the nanoprobe in the presence of FXM from Indian red to light red violet and bluish-purple color offered simple detection of FXM with the naked eye. The satisfactory results of the proposed cost-effective sensor in the rapid assay of FXM in human serum, urine, saliva and pharmaceutical samples guarantee the potential of the nanoprobe for on-site and visual determination of FXM in actual samples. The proposed sensor as the first non-invasive FXM sensor for saliva sample analysis may hold great promise to provide the technical support for the rapid and valid detection of FXM for forensic medicine and clinical organizations.


Assuntos
Nanopartículas Metálicas , Humanos , Nanopartículas Metálicas/química , Colorimetria/métodos , Fluvoxamina , Ouro/química , Smartphone
5.
Biosensors (Basel) ; 13(3)2023 Mar 12.
Artigo em Inglês | MEDLINE | ID: mdl-36979586

RESUMO

Inspired by laccase activity, herein, Cu-guanosine nanorods (Cu-Guo NRs) have been synthesized for the first time through a simple procedure. The activity of the Cu-Guo NR as the laccase mimicking nanozyme has been examined in the colorimetric sensing of rutin (Rtn) by a novel and simple spectrophotometric method. The distinct changes in the absorbance signal intensity of Rtn and a distinguished red shift under the optimum condition based on pH and ionic strength values confirmed the formation of the oxidized form of Rtn (o-quinone) via laccase-like nanozyme activity of Cu-Guo NRs. A vivid and concentration-dependent color variation from green to dark yellow led to the visual detection of Rtn in a broad concentration range from 770 nM to 54.46 µM with a limit of detection (LOD) of 114 nM. The proposed methodology was successfully applied for the fast tracing of Rtn in the presence of certain common interfering species and various complex samples such as propolis dry extract, human biofluids, and dietary supplement tablets, with satisfactory precision. The sensitivity and selectivity of the developed sensor, which are bonuses in addition to rapid, on-site, cost-effective, and naked-eye determination of Rtn, hold great promise to provide technical support for routine analysis in the real world.


Assuntos
Cobre , Nanotubos , Humanos , Cobre/análise , Colorimetria/métodos , Lacase , Guanosina , Rutina
6.
Talanta ; 254: 124168, 2023 Mar 01.
Artigo em Inglês | MEDLINE | ID: mdl-36549133

RESUMO

In this study, a new microfluidic-chip coupled with micro solid phase extraction (µ-SPE) and a RGB detection system was designed. The method was used for extraction and simultaneous determination of trace amounts of dyes with different acidic-basic properties. Erythrosine (Ery) and Crystal Violet (CV) were selected as acidic and basic model analytes, respectively. The first step of this method is based on the on-chip electromembrane extraction (CEME) of analytes from aqueous solution. The utilized microfluidic system is a single compartment that composed of three polymethyl metacrylate plates (with sandwiched structures) patterned with palm shaped helix channels. The device consisted one pair of platinum electrodes that were embedded in the acceptor phase channels in each side. The middle part was cut and used as the path of the sample. The extracted analytes by CEME were passed through the micro-packed column containing strong cation and anion exchanger sorbents respectively. Two adsorbents were separated by a polypropylene frit and sealed on each side by two polypropylene frites. Following dye adsorption on the sorbents, the colors that emerged were promptly evaluated using RGB colorimetry on a smartphone. Central composite design was used to analyze and optimize the effective parameters on extraction efficiency. The relative standard deviations (RSDs%) based on five replicate measurements were less than 7.8% for RGB and 8.6% for the spectrophotometry technique under ideal conditions. Image analysis using a smartphone yielded LOD values of 15.0 and 10.5 µg L-1 for Ery and CV, respectively. The CEME- µ-SPE -RGB approach produced findings that were equivalent to those obtained by spectrophotometry. Finally, the approach was used to accurately determine Ery and CV in water samples, yielding good relative recoveries (recovery ≥94.0).


Assuntos
Corantes , Microfluídica , Smartphone , Polipropilenos , Extração em Fase Sólida , Cromatografia Líquida de Alta Pressão/métodos
7.
Artigo em Inglês | MEDLINE | ID: mdl-35489127

RESUMO

In the present work, methyl red molecularly imprinted polymeric (MR-MIP) nanostructure was synthesized using the precipitation polymerizations for the separation of MR dye from aqueous media. The as-prepared MIP was characterized using colorimetry, infrared (IR) spectroscopy, and scanning electron microscopy (SEM). In addition, vortex-assisted dispersive micro-solid phase extraction (VAD-µSPE) based on MIP nanostructure was accomplished as a simple and efficient method for selective preconcentration of low amounts of MR from aqueous solutions. The effects of important parameters such as pH, adsorbent dose, eluent volume, and vortex adsorption-desorption time on the extraction efficiency were investigated. Two techniques including UV-Vis absorption spectroscopy and solution scanometry were applied for the analysis of MR content, comparatively. In spectrophotometric determination, the highest recovery was observed at pH 3.5 after 5 and 3 min of vortex time in the adsorption and desorption steps. The preconcentration factor of 75 and a wide linear concentration range (0.010 and 2.0 mg.L-1; R2 = 0.996) and low detection limit (LOD = 5.0 µg.L-1) with an acceptable precision (RSD = 3.4 %) was observed, too. Under optimum conditions in scanometric determination, a high preconcentration factor (i.e. 500) and similar linearity (0.010-2.0 mg.L-1; R2 = 0.989) and a low LOD of 3.1 µg.L-1, with the relative standard deviation of 1.4% was observed. Both techniques were used for MR recovery from various aqueous samples, successfully.


Assuntos
Impressão Molecular , Nanoestruturas , Adsorção , Impressão Molecular/métodos , Polímeros/química , Extração em Fase Sólida/métodos , Água
8.
Food Chem ; 325: 126902, 2020 Apr 23.
Artigo em Inglês | MEDLINE | ID: mdl-32387937

RESUMO

Magnetic dual-template molecularly imprinted polymer (Fe3O4@SiO2-MDMIP) was prepared to enrich and determine both p-Coumaric acid (p-CA) and ferulic acid (FA) based on syringe-to-syringe magnetic solid-phase microextraction (SS-MSPME). The obtained MDMIP was characterized and recognized, and then its adsorbing performance was studied. Based on the results, the Fe3O4@SiO2-MDMIP indicated selective recognition towards p-CA and FA with large adsorption capacity. The optimization of MDMIP-SS-MSPME conditions (pH, Fe3O4@SiO2-MDMIP mass, NaCl concentration, number of cycle, and elution volume) were conducted using the central composite design (CCD). Under the optimum conditions, an effectual and a convenient method was established to determine p-CA and FA in pomegranate, grapes, and orange samples based on SS-MSPME coupling with high-performance liquid chromatography-ultraviolet (HPLC-UV). Our developed method showed the limit of detection (LOD) of 0.08 ng mL-1 for p-CA and 0.07 ng mL-1 for FA. The method also indicated good linearity with R2 > 0.99 and good recoveries of 85.12-94.96% with RSDs ≤ 5.58% spiked at three various concentration levels in pomegranate, grapes, and orange samples.

9.
J AOAC Int ; 100(6): 1861-1868, 2017 Nov 01.
Artigo em Inglês | MEDLINE | ID: mdl-28807089

RESUMO

In the present work, a simple, efficient, and environmentally friendly method was proposed for the simultaneous preconcentration and determination of minute quantities of copper and cobalt in water samples and serum by a supramolecular-based ultrasonic-assisted dispersion solidification liquid-liquid microextraction (DSLLME) procedure coupled with flame atomic absorption spectrometry. The procedure is based on the DSLLME of copper and cobalt with decanoic acid-tetrahydrofuran supramolecular solvent (SUPRAS) in the presence of sodium diethyldithiocarbamate, as the complexing agent. SUPRAS is a nanostructured liquid generated from amphiphiles through a sequential self-assembly process occurring on two scales, molecular and nano. Several variables that affect the extraction efficiency-including pH, concentration of complexing agent, volume of the extraction and dispersive solvents (volume of SUPRAS), sonication time, and ionic strength-were investigated and optimized. The method provided enrichment factors of 23.31 and 22.38 for copper and cobalt, respectively. The preconcentration factor for the two analytes was 20.00. Calibration plots were linear in the range of 5.00-700.00 ng/mL for copper and 5.00-500.00 ng/mL for cobalt, with correlations of determination of 0.9973 and 0.9981. The precision of the method were expressed as RSDs for six replicate measurements and LODs and found to be ±4.10 and ±2.30% for copper and 2.90 and 3.50 ng/mL for cobalt. The proposed method was successfully applied to the simultaneous determination of trace copper and cobalt in real water samples and serum with satisfactory results.


Assuntos
Cobalto/isolamento & purificação , Cobre/isolamento & purificação , Microextração em Fase Líquida/métodos , Espectrofotometria Atômica/métodos , Centrifugação , Cobalto/análise , Cobalto/sangue , Cobre/análise , Cobre/sangue , Ditiocarb/química , Água Potável/análise , Humanos , Concentração de Íons de Hidrogênio , Solventes/química , Fatores de Tempo , Ultrassom , Poluentes Químicos da Água/análise , Poluentes Químicos da Água/isolamento & purificação
10.
Nat Prod Res ; 30(17): 1927-33, 2016 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-26506268

RESUMO

Based on a literature survey on cytotoxic medicinal plants, Juniper species were identified as interesting source of antitumor compounds. Using bioassay-guided fractionation against Caov-4 cancer cells on acetone extract of leaves and branchlets of Juniperus foetidissima led to the isolation of a new 3H-benzofuaran-2-one: 4-methyl-3-methoxy-3H-benzofuaran-2-one (1), a new sesquiterpene: 4,9(α)-dihydroxy-nardosin-6-en (2) and an already known labdane-type diterpene: 15-hydroxy-8(17),13(E)-labdadiene-19-carboxilic acid (3). Compounds 1-3 exhibited cytotoxic effects, with moderate cytotoxicity against the EJ-138 bladder and CAOV-4 ovary cancer cell lines.


Assuntos
Antineoplásicos Fitogênicos/isolamento & purificação , Juniperus/química , Antineoplásicos Fitogênicos/farmacologia , Linhagem Celular Tumoral , Humanos , Extratos Vegetais/análise , Folhas de Planta/química
11.
Environ Monit Assess ; 186(2): 1113-21, 2014 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-24065134

RESUMO

In this study, cloud point extraction was used for the preconcentration of Al(3+) ion after the complex formation with 1,4-dihydroxy-9,10-anthraquinone (Quinizarin [QUIN]), and subsequent analysis by spectrophotometeric method, using Triton X-114 as surfactant. The optimal extraction and reaction conditions were studied (i.e., pH = 5.5, 0.1 mM QUIN, Triton X-114 = 0.1% (w/v)), and the analytical characteristics of the method (e.g., limit of detection, linear range, preconcentration, and enrichment factors) were obtained. Linearity was obeyed in the range of 3.33-166.67 ng ml(-1) of Al(3+) ion. The detection limit of the method was 2.09 ng ml(-1) for Al(3+) ion. The interference effect of some anions and cations was also tested. The method was applied to determine Al(3+) ion in water samples.


Assuntos
Alumínio/análise , Antraquinonas/química , Fracionamento Químico/métodos , Monitoramento Ambiental/métodos , Poluentes Químicos da Água/análise , Alumínio/química , Cátions , Poluentes Químicos da Água/química
12.
J AOAC Int ; 92(4): 1208-18, 2009.
Artigo em Inglês | MEDLINE | ID: mdl-19714992

RESUMO

New iodide ion-selective electrodes based on bis(2-methyl-3-phenyl-propenylidene)1,2-propanediamine)mercury(II) bromide [Hg(BMPPMB)Br2], bis (5-bromo salicylaldehyde) ethylenediimine vanadyl(IV) [VO(5-Br Salen)], and bis(5-bromo salicylaldehyde) ethylenediimine uranyl(VI) [UO2(5-Br Salen)] carriers are described. The electrodes exhibited Nernstian slopes of -58.3 +/- 1.0, -58.5 +/- 1.4, and -59.0 +/- 1.2 mV/decade for Hg(BMPPMB)Br2, VO(5-Br Salen), and UO2(5-Br Salen) iodide ion concentration in the range of 1.0 x 10(-6)-0.1 M, with detection limits of about 0.6, 0.5, and 0.3 microM, respectively. The potentiometric responses of the electrodes were independent of pH over the range 1.7-10.6, 2.2-11.3, and 2.1-11.1, with satisfactory reproducibility. The electrodes had response times of < or =5 s and could be used for at least 84, 80, and 100 days for Hg(BMPPMB)Br2, VO(5-Br Salen), and UO2(5-Br Salen), respectively, without any considerable divergence in their potential responses.


Assuntos
Iodetos/análise , Ionóforos/análise , Eletrodos , Grafite , Concentração de Íons de Hidrogênio , Indicadores e Reagentes , Membranas Artificiais , Preparações Farmacêuticas/análise , Cloreto de Polivinila , Potenciometria , Espectrofotometria Ultravioleta
13.
J AOAC Int ; 92(3): 907-13, 2009.
Artigo em Inglês | MEDLINE | ID: mdl-19610384

RESUMO

A cloud point extraction (CPE) procedure was presented for the preconcentration of silver, zinc, and lead ions in various samples. The complexes of these metal ions with 2-(((1H-benzo[d]imidazol-2-yl)methoxy)methyl)-1H-benzo[d]imidazole (BIMMBI) are quantitatively extracted into the Triton X-114-rich phase after centrifugation. A solution of 1.0 M HNO3 in methanol was added to the surfactant-rich phase as the effective eluant before analysis by flame atomic absorption spectrometry. The influence of effective parameters such as the concentrations of BIMMBI, Triton X-114, and HNO3, pH, bath temperature, centrifuge rate, and time on method sensitivity and efficiency was optimized. Detection limits of 2.8, 1.7, and 1.1 ng/mL for Pb2+, Ag+, and Zn2+, respectively, along with a preconcentration factor of 30 and enrichment factors of 33, 48, and 53 for Pb2+, Ag+, and Zn2+, respectively, were obtained. The present CPE method is suitable for accurate and precise determination of trace amounts of analyte ions in complex matrixes. The proposed CPE procedure was applied to the determination of these ions in biological, natural water, wastewater, soil, and blood samples.


Assuntos
Chumbo/análise , Prata/análise , Espectrofotometria Atômica/métodos , Zinco/análise , Concentração de Íons de Hidrogênio , Octoxinol , Polietilenoglicóis/química , Cloreto de Sódio/química , Temperatura , Viscosidade
14.
J Hazard Mater ; 168(2-3): 1022-7, 2009 Sep 15.
Artigo em Inglês | MEDLINE | ID: mdl-19380196

RESUMO

The phase-separation phenomenon of non-ionic surfactants occurring in aqueous solution was used for the extraction of cadmium(II), lead(II), palladium(II) and silver(I). The analytical procedure involved the formation of understudy metals complex with bis((1H-benzo [d] imidazol-2yl)ethyl) sulfane (BIES), and quantitatively extracted to the phase rich in octylphenoxypolyethoxyethanol (Triton X-114) after centrifugation. Methanol acidified with 1molL(-1) HNO(3) was added to the surfactant-rich phase prior to its analysis by flame atomic absorption spectrometry (FAAS). The concentration of BIES, pH and amount of surfactant (Triton X-114) was optimized. At optimum conditions, the detection limits of (3 sdb/m) of 1.4, 2.8, 1.6 and 1.4 ng mL(-1) for Cd(2+), Pb(2+), Pd(2+) and Ag(+) along with preconcentration factors of 30 and enrichment factors of 48, 39, 32 and 42 for Cd(2+), Pb(2+), Pd(2+) and Ag(+), respectively, were obtained. The proposed cloud point extraction has been successfully applied for the determination of metal ions in real samples with complicated matrix such as radiology waste, vegetable, blood and urine samples.


Assuntos
Cádmio/análise , Poluentes Ambientais/análise , Chumbo/análise , Paládio/análise , Prata/análise , Espectrofotometria Atômica/métodos , Cádmio/isolamento & purificação , Concentração de Íons de Hidrogênio , Chumbo/isolamento & purificação , Octoxinol , Paládio/isolamento & purificação , Polietilenoglicóis , Reprodutibilidade dos Testes , Prata/isolamento & purificação , Cloreto de Sódio , Temperatura
15.
Chemosphere ; 74(4): 583-9, 2009 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-19027140

RESUMO

A simple and relatively fast approach for developing a solid phase extraction has been described and used for determination of trace quantities of some heavy and transition metal ions with sodium dodecyl sulfate (SDS)-coated poly vinyl chloride (PVC) modified with bis(2-hydroxyacetophenone)-1,4-butanediimine (BHABDI) ligand. The adsorbed ions were stripped from the solid phase by 10 mL of 3M nitric acid as eluent. The eluting solution was analyzed for metals content (cadmium, chromium, cobalt, copper, lead and zinc) by flame atomic absorption spectrometry (FAAS). The main factors such as pH, amount of ligand and PVC, amount and type of surfactant, and condition of eluting solutions on the sorption recovery of metal ions have been investigated in detail. The relative standard deviation was found in the range of 1.0-3.2% for 0.2 microg mL(-1)of metals ions. After optimization of the extraction condition and the instrumental parameters, a detection limit was found to be in the range of 1.2-3.1 microg L(-1), with enrichment factor of 50 was achieved. The method was successfully applied for the determination of these metals contents in real samples with satisfactory results.


Assuntos
Metais Pesados/isolamento & purificação , Cloreto de Polivinila/química , Dodecilsulfato de Sódio/química , Adsorção , Concentração de Íons de Hidrogênio , Metais Pesados/análise , Metais Pesados/química , Reprodutibilidade dos Testes , Extração em Fase Sólida , Espectrofotometria Atômica , Elementos de Transição/análise , Elementos de Transição/química , Elementos de Transição/isolamento & purificação
16.
J Hazard Mater ; 160(2-3): 435-40, 2008 Dec 30.
Artigo em Inglês | MEDLINE | ID: mdl-18433996

RESUMO

A cloud point extraction procedure was presented for the preconcentration of copper(II) ion in various samples. After complexation by 4-(phenyl diazenyl) benzene-1,3-diamine (PDBDM) (chrysoidine), copper(II) ions were quantitatively recovered in Triton X-114 after centrifugation. 0.5ml of methanol acidified with 1.0molL(-1) HNO3 was added to the surfactant-rich phase prior to its analysis by flame atomic absorption spectrometry (FAAS). The influence of analytical parameters including ligand, Triton X-114 and HNO3 concentrations, bath temperature, heating time, centrifuge rate and time were optimized. The effect of the matrix ions on the recovery of copper(II) ions was investigated. The detection limit (3S.D.b/m, n=10) of 0.6ngmL(-1) along with preconcentration factor of 30 and enrichment factor of 41.1 with R.S.D. of 1.0% for Cu was achieved. The proposed procedure was applied to the analysis of various environmental and biological samples.


Assuntos
Cobre/análise , Poluentes Ambientais/análise , Animais , Análise Química do Sangue , Calibragem , Centrifugação , Corantes , Cobre/isolamento & purificação , Análise de Alimentos , Humanos , Concentração de Íons de Hidrogênio , Indicadores e Reagentes , Micelas , Octoxinol , Polietilenoglicóis , Cloreto de Sódio , Espectrofotometria Atômica , Temperatura , Abastecimento de Água/análise , p-Aminoazobenzeno/análogos & derivados , p-Aminoazobenzeno/química
17.
J Hazard Mater ; 158(1): 131-6, 2008 Oct 01.
Artigo em Inglês | MEDLINE | ID: mdl-18314265

RESUMO

A new and efficient solid phase extraction method is described for the preconcentration of trace heavy metal ions. The method is based on the adsorption of Fe(3+), Cu(2+) and Zn(2+) on 2-phenyl-1H-benzo[d] imidazole (PHBI) loaded on Triton X-100-coated polyvinyl chloride (PVC). The influences of the analytical parameters including pH and sample volume were investigated. Common coexisting ions did not interfere on the separation and determination of analytes under study. The adsorbed analytes were desorbed by using 5 mL of 4 mol L(-1) nitric acid. The preconcentration factor is 90. The detection limits (3 sigma) were in the range of 0.95-1 microg L(-1). The sorbent exhibited excellent stability and its sorption capacity under optimum conditions has been found to be more than 2.7 mg of ions per gram of sorbent. The recoveries of analytes were generally higher than 95%. The relative standard deviations (R.S.D.s) were generally lower than 4%. The method has been successfully applied to some real samples.


Assuntos
Benzimidazóis/química , Metais Pesados/química , Octoxinol/química , Cloreto de Polivinila/química , Extração em Fase Sólida/métodos , Reutilização de Equipamento , Concentração de Íons de Hidrogênio , Íons/química , Reprodutibilidade dos Testes , Tensoativos/química
18.
Spectrochim Acta A Mol Biomol Spectrosc ; 71(2): 655-62, 2008 Nov 15.
Artigo em Inglês | MEDLINE | ID: mdl-18329953

RESUMO

The complexation reaction between some oximes including methyl-2-pyridylketone oxime (MPKO), phenyl-2-pyridylketone oxime (PPKO) and diacetyl monooxime (DMO) with some transition and heavy metal ions Co2+, Ni2+, Zn2+, Pb2+, Fe2+, Fe3+, Cr3+ and La3+ has been studied potentiometrically in aqueous solution at 25+/-0.1 degrees C and ionic strength (mu) of 0.1M supported by KCl. The overall stability constants logbeta's of respective species were obtained by computer refinement of pH-volume data using BEST program. The best model among the several proposed models was selected according to the lowest sigma(fit) value. The main species in binary systems are ML, ML2, MLH, MLH2, ML2H, ML2H2, MOHL, M(OH)2L, M(OH)L2 and M(OH)2L2 (L = MPKO or PPKO or DMO).


Assuntos
Diacetil/análogos & derivados , Metais Pesados/química , Oximas/química , Piridinas/química , Elementos de Transição/química , Diacetil/química , Concentração de Íons de Hidrogênio , Íons/química , Estrutura Molecular , Potenciometria , Soluções , Titulometria
19.
J Hazard Mater ; 155(1-2): 121-7, 2008 Jun 30.
Artigo em Inglês | MEDLINE | ID: mdl-18155354

RESUMO

A sensitive and selective solid phase extraction procedure for the determination of traces of Cu(II), Zn(II), Pb(II) and Fe(III) has been developed. An alumina-sodium dodecyl sulfate (SDS) coated on with meso-phenyl bis(indolyl) methane (MPBIM) was used for preconcentration and determination of Cu(II), Zn(II), Pb(II) and Fe(III) ions by flame atomic absorption spectrometry. The analyte ions were adsorbed quantitatively on adsorbent due to their complexation with MPBIM. Adsorbed metals were quantitatively eluted using 6 mL of 4 mol L(-1) nitric acid. The effects of parameters such as pH, amount of alumina, amount of MBITP, flow rate, type and concentration of eluting agent were examined. The effects of interfering ions on the separation-preconcentration of analytes were also investigated. The relative standard deviation of the method was found to be less than 3.0%. The presented procedure was successfully applied for determination of analytes in real samples.


Assuntos
Óxido de Alumínio/química , Metais Pesados/análise , Dodecilsulfato de Sódio/química , Poluentes do Solo/análise , Tensoativos/química , Poluentes Químicos da Água/análise , Indóis/química , Metais Pesados/sangue , Extração em Fase Sólida , Espectrofotometria Atômica , Spinacia oleracea/química
20.
Ann Chim ; 97(9): 823-36, 2007 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-17970298

RESUMO

A simple, selective and sensitized spectrophotometric method for determination of trace amounts of Fe3+ ion in tap and waste water solutions has been described. The spectrophotometric determination of Fe3+ ion using Ferron in the presence of N,N-Dodecytrimethylammonium bromide (DTAB) has been carried out. The Beer's law is obeyed over the concentration range of 0.05-2.6 microg mL(-1) of Fe3+ ion with the relative standard deviation (RSD %) <0.2% and the molar absorptivity of complexes in pH 3.5 is 3.8 x 10(3) L mol(-1) cm(-1). Potentiometric pH titration has been used for prediction of protonation constants of ferron, and evaluating its stoichiometry and respective stability constant with Fe3+ ion. As it is obvious the most likely species of ferron alone and its complexes are LH (log = 7.64), LH2 (logK = 10.52), LH3 (logK = 11.74) and ML2 (logbeta = 23.68), ML3 (logbeta = 23.68), ML3H (logbeta = 23.68), ML3H2 (logbta = 23.68) and ML(OH)2 (logbeta = 23.68) respectively.


Assuntos
Compostos Férricos/análise , Potenciometria/métodos , Concentração de Íons de Hidrogênio , Reprodutibilidade dos Testes , Sensibilidade e Especificidade , Espectrofotometria Ultravioleta
SELEÇÃO DE REFERÊNCIAS
DETALHE DA PESQUISA
...