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1.
Sci Rep ; 14(1): 14478, 2024 Jun 24.
Artigo em Inglês | MEDLINE | ID: mdl-38914725

RESUMO

Nowadays, the use of natural wastes and adsorbents along with their modification by simple and new methods based on metal oxides to remove dye pollutants has been the focus of many researchers. In this study, for the first time, simple and low-cost modification of eggshell (EGS) with tungsten oxide (WO3) based on the photochemical modification method as a green, ultra-fast, cost-effective, and biodegradable adsorbent is reported to remove of methylene blue (MB) dye pollutant. The EGS modified by WO3 was investigated by EDX, EDX mapping, XRD, FE-SEM, and UV-Vis Diffuse Reflectance (DRS) analyses. The obtained results show that the modified EGS by WO3 has more than ten times (78.5%) the ability to remove MB dye pollutant within 3 min compared to bare EGS (11%). Various parameters including dye pollutant pH, dye concentration, adsorbent dosage, and reusability of the WO3/EGS adsorbent for removal of MB dye pollutant were investigated and the result show that the adsorbent capacity of WO3/EGS is 1.64 mg g-1. EGS adsorbent The synthesis of WO3/EGS adsorbent with a novel photochemical method as a fast and very cheap adsorbent with excellent efficiency can be a promising alternative adsorbent for various purposes in removing dye pollutants from water environments.

2.
Anal Methods ; 16(26): 4247-4254, 2024 Jul 04.
Artigo em Inglês | MEDLINE | ID: mdl-38904334

RESUMO

The analytical determination of opiates in biological samples is a critical mission and remains a challenge for almost all judicial and clinical drug testing panels due to their high abuse potential. Based on the high sensitivity of the longitudinal surface plasmon resonance (LSPR) peak of gold nanorods (AuNRs), we successfully developed a novel and simple refractive index sensing platform for detection of morphine (MOR) and codeine (COD) by means of 2-amino-5-mercapto-1,3,4-thiadiazole functionalized gold nanorods (AMTD-AuNRs) in aqueous solution, which is, to the best of our knowledge, the first report on the assay of MOR and COD using AuNRs. AMTD molecules strongly anchor onto the tips of AuNRs via the mercapto group and subsequent hydrogen-bonding interactions between AMTD and the analytes induced end-to-end chain assembly of AuNRs and a consequent decrease of the LSPR absorption band at 850 nm along with a bathochromic shift and emergence of a new hybridized plasmon mode at 1050 nm which was characterized using a Vis-NIR spectrophotometer. After systematic optimization, the absorbance ratio (A1050/A850) was proportional to the concentration of MOR in the ranges of 0.08-5 µM and 0.2-8 µM for COD without any significant effect from possible interferents. Furthermore, detection limits of 40 and 62 nM were achieved for MOR and COD, respectively, which are much lower than the cut-off level of 2000 ng mL-1 for opiates in urine samples set by the Substance and Abuse Mental Health Services Administration (SAMHSA). Eventually, as proof-of-applicability, human urine and blood serum samples spiked with MOR and COD were analyzed and excellent recoveries ranging from 94.4 to 108.9% were obtained, demonstrating the successful applicability of the designed refractive index probe in real biological specimens.


Assuntos
Codeína , Ouro , Morfina , Nanotubos , Ressonância de Plasmônio de Superfície , Codeína/urina , Codeína/sangue , Codeína/análise , Ouro/química , Nanotubos/química , Morfina/urina , Morfina/sangue , Humanos , Ressonância de Plasmônio de Superfície/métodos , Técnicas Biossensoriais/métodos , Limite de Detecção , Espectroscopia de Luz Próxima ao Infravermelho/métodos
3.
Spectrochim Acta A Mol Biomol Spectrosc ; 313: 124104, 2024 May 15.
Artigo em Inglês | MEDLINE | ID: mdl-38493511

RESUMO

So far, many adsorbents and nanocomposites have been synthesized by different methods and used to remove or degradation of dye pollutants. Nowadays, the use of natural adsorbents and their modification with simple methods based on metal oxides are of interest to many researchers. In this study, for the first time, we report the simple and low-cost modification of tea pomace waste (TPW) with tungsten oxide (WO3) based on the photochemical method as a green, cost-effective, and biodegradable photocatalyst for the degradation of Rh B dye pollutant. The results obtained from FE-SEM, EDAX, XRD, XPS, PL, BET and UV-Vis Diffusive Reflectance (DRS) analyses confirmed the successful modification of the TPW surface with WO3 (WO3/TPW). The parameters affecting the photocatalytic behavior of WO3/TPW, including the time of photochemical modification and the type of radiation on its photocatalytic activity, were carefully optimized. WO3/TPW showed excellent photocatalytic activity compared to TPW for the degradation of Rh B dye pollutant under UV light for 30 min (94 %). Finally, the effective parameters on the value of Rh B dye degradation by WO3/TPW photocatalyst including pH, adsorbent dosage, the concentration of dye pollutant, and the kinetics of the degradation process were studied. It is expected that this type of photochemical modification method and natural WO3/TPW photocatalyst will be a promising path for the synthesis, modification, and increase of the photocatalytic performance of natural adsorbents.

4.
Sci Rep ; 13(1): 13569, 2023 Aug 21.
Artigo em Inglês | MEDLINE | ID: mdl-37604865

RESUMO

In this study, a polymeric adsorbent based on carboxymethyl tragacanth (CMT) grafted by poly acrylic acid-co-acrylamide (AAc-co-AAm) synthesized by radical polymerization for the first time was used to remove the fungicide penconazole (PEN) or Topas 20% from surface water. The parameters of solution pH, adsorption isotherm, and adsorption kinetics of PEN were studied by the synthetic adsorbent. The surface morphology and functional groups of CMT-g-poly (AAc-co-AAm) were confirmed by XRD, SEM and FT-IR techniques. Adsorption of PEN on CMT-g-poly (AAc-co-AAm) follows the Freundlich and pseudo-second-order models. The significant maximum adsorption capacity of the synthesized polymer was found to be 196.08 mg/g. The synthetic adsorbent had good reproducibility in PEN removal for up to 5 cycles. CMT-g-poly (AAc-co-AAm) is a cost-effective and non-toxic adsorbent for the decontamination of surface water from pesticides.

5.
Vet Res Forum ; 14(3): 169-176, 2023.
Artigo em Inglês | MEDLINE | ID: mdl-37033781

RESUMO

Volatile compounds of anal sac secretions are odorant chemicals used across the carnivores for social communication such as identifying individuals and group membership. Odor profiles taken from expressed anal sac secretions of some species of carnivores have been detected in previous studies. In this study, the volatile compounds of anal sac secretions between five male and five female domestic dogs (Canis lupus familiaris) were compared. Volatile chemicals were extracted, separated, and analyzed by gas chromatography-mass spectrometry with solid-phase micro-extraction and identified from their electron ionization mass spectra and Kovats retention indices. The results showed the presence of various types of compounds including organic fatty acids, ketones, aldehydes, esters, and alcohols in the anal sac secretions of dogs. Greater amounts of diversity and esters, and lower amounts of alcohols were detected in the anal sac secretions of females compared to males. This was accompanied by finding citrate and acetic acid ester only in the females. Furthermore, presence of some sex-specific organic compounds like dimethylcyclopentyl ethanone indicates that the volatile profiles of anal sac secretions in 10 domestic dogs are differentiated by host sex.

6.
Biosens Bioelectron ; 178: 112999, 2021 Apr 15.
Artigo em Inglês | MEDLINE | ID: mdl-33493897

RESUMO

The formation of G-quadruplex (G4) structures in Human telomeric DNA (H-Telo) has been demonstrated to inhibit the activity of telomerase enzyme that is associated with the proliferation of many cancer cells. Accordingly, G-quadruplex structures have become one of the well-established targets in anticancer therapeutic strategies. And, the development of simple and selective detection platforms for G4 structures has become a significant focus of research in recent years. In this study, a simple "off-on" fluorometric method was developed for the selective detection of picomolar quantities of H-Telo G4 DNA based on a fluorescent cerium-based metal organic framework (Ce-MOF) conjugated with hemin to form the sensing probe, Hemin@Ce-MOF. The solvothermal synthesis of the Ce-MOF took advantage of 5-aminoisophtlalic acid (5AIPA) as the organic bridging ligand, (Ce2(5AIPA)3(DMF)2). Characterization of Ce-MOF and Hemin@Ce-MOF was performed by XRD, XPS, TEM, SEM, BET and FTIR techniques. The detection and quantification of the H-Telo was carried out through the adsorption/incorporation of hemin molecules on the pores and surface of Ce-MOF resulting in the fluorescent quenching of the system followed by the restoration of the fluorescence upon addition of H-Telo probably due to a competition between H-Telo and Ce-MOF to bind to hemin. The impact of the key variables including MOF quantity, hemin concentration and detection time was investigated and optimized. Under the optimized conditions, the developed probe provides a limit of detection (LOD) of 665 pM, linear dynamic range (LDR) of 1.6-39.7 nM and excellent selectivity towards H-Telo. Taken together, these results present a simple, novel and superior platform for the selective detection of H-Telo G4 DNA.


Assuntos
Técnicas Biossensoriais , DNA Catalítico , Quadruplex G , Estruturas Metalorgânicas , DNA/genética , Hemina , Humanos
7.
Turk J Chem ; 44(4): 987-1001, 2020.
Artigo em Inglês | MEDLINE | ID: mdl-33488207

RESUMO

This study aimed to propose a mathematical method to investigate and optimize the simultaneous elimination process of multiple organic pollutants using the Fenton process. Hence, the treatment of rhodamine B (RB) and acid red 14 (AR14) dyes in their binary solution was studied. Multivariate curve resolution alternating least square (MCR-ALS), a novel chemometric method, was applied along with correlation constraints to resolute the UV-Vis spectrophotometric data, enabling quantification of investigated dyes despite a high spectral overlapping. Response surface methodology was adopted to assess the model and optimize individual and interactive effects of three independent factors (Fe2+, H2O2 and initial pH) on the simultaneous elimination of RB and AR14. The values of the regression coefficient for RB and AR14 were determined as 98.48 and 98.67 percent, respectively, revealing the reliability of the obtained polynomial models to predict decolorization efficiencies. Desirability function was employed to optimize the independent variables to attain the highest possible degradation performance for both dyes in their binary solution. At the optimum point of operation ([Fe2+] = 143.88 mg/L, [H2O2] = 126.89 mg/L and pH = 3.71), degradation efficiencies of RB and AR14 were found as 81.58% and 80.22%, respectively, which were nearly identical to the experimental results.

8.
Talanta ; 194: 859-869, 2019 Mar 01.
Artigo em Inglês | MEDLINE | ID: mdl-30609616

RESUMO

Reuse of polyethylene terephthalate (PET) bottles for storage of water and liquid food is so common in some countries of the world. However, it can result in the migration of plastic components or additives into the stored liquids and threatening of human health. In this respect, the present study developed a method for determination of endocrine disrupting chemicals (EDCs) that might be released from reused disposable plastic containers. The proposed method relied on the extraction of the phthalic acid esters (PAEs) and plastic additives by a self-magnetic nanocomposite monolithic (SMNM) kit and their determination by gas chromatography/mass spectroscopy (GC/MS). Extraction of the target analytes by the self-magnetic nanocomposite monolithic stir bar sorptive extraction (SMNMSBSE) method was optimized systematically by evaluating the effect of extraction time, ionic strength, stirring rate, desorption time and desorption solvent on the process. Analysis of different water and liquid food samples with various pH value and matrices unraveled that the acidic liquids and the samples stored at higher temperature have a greater chance of contamination by the released EDCs. Also, low-quality plastic bottles were found to release more plastic additives into the stored liquids. At the optimal conditions, the method demonstrated a linear response from 0.01 to 1000 µg L-1 and provided the limits of detection (LODs) of 0.008-1.000 µg L-1. Furthermore, the relative standard deviation (RSD) of the method did not exceed 10.05% and 8.12% for interday and intraday precision, respectively. In general, the results of this study indicated that the synthesized SMNM kit can effectively enrich the migrated plastic additives and the developed SMNMSBSE-GC/MS methodology is efficient for analysis of the target EDCs.


Assuntos
Disruptores Endócrinos/análise , Disruptores Endócrinos/isolamento & purificação , Plásticos/química , Reciclagem , Microextração em Fase Sólida/métodos , Poluentes Químicos da Água/análise , Poluentes Químicos da Água/isolamento & purificação , Disruptores Endócrinos/química , Limite de Detecção , Nanopartículas de Magnetita/química , Concentração Osmolar , Polietilenotereftalatos/química , Solventes/química , Fatores de Tempo , Poluentes Químicos da Água/química
9.
Spectrochim Acta A Mol Biomol Spectrosc ; 193: 451-457, 2018 Mar 15.
Artigo em Inglês | MEDLINE | ID: mdl-29289743

RESUMO

Herein, a rapid, sensitive and selective approach for the colorimetric detection of dopamine (DA) was developed utilizing unmodified gold nanoparticles (AuNPs). This assay relied upon the size-dependent aggregation behavior of DA and three other structurally similar catecholamines (CAs), offering highly specific and accurate detection of DA. By means of this study, we attempted to overcome the tedious procedures of surface premodifications and achieve selectivity through tuning the particle size of AuNPs. DA could induce the aggregation of the AuNPs via hydrogen-bonding interactions, resulting in a color change from pink to blue which can be monitored by spectrophotometry or even the naked-eye. The proposed colorimetric probe works over the 0.1 to 4µM DA concentration range, with a lower detection limit (LOD) of 22nM, which is much lower than the therapeutic lowest abnormal concentrations of DA in urine (0.57µM) and blood (16µM) samples. Furthermore, the selectivity and potential applicability of the developed method in spiked actual biological (human plasma and urine) specimens were investigated, suggesting that the present assay could satisfy the requirements for clinical diagnostics and biosensors.


Assuntos
Técnicas Biossensoriais , Dopamina/sangue , Dopamina/urina , Ouro/química , Nanopartículas Metálicas/química , Humanos , Limite de Detecção , Tamanho da Partícula
10.
Spectrochim Acta A Mol Biomol Spectrosc ; 189: 522-527, 2018 Jan 15.
Artigo em Inglês | MEDLINE | ID: mdl-28863401

RESUMO

In this paper, we describe a rapid, low-cost and highly sensitive colorimetric method for the detection of isoprenaline, based on 2-amino-5-mercapto-1,3,4-thiadiazol (AMTD) functionalized gold nanoparticles (AMTD-AuNPs) as a sensing element. Hydrogen bonding interaction between isoprenaline and AMTD resulted in the aggregation of AuNPs and a consequent color change of AuNPs from red to blue. The concentration of isoprenaline could be detected with the naked eye or a UV-visible spectrometer. Results showed that the absorbance ratio (A650/A524) was linear with isoprenaline concentrations in the range of 0.2 to 2.6µM (R=0.997). The detection limit of this method was 0.08µM. The proposed method is simple, without using complicated instruments and adding salts for enhancing sensitivity. This probe could be successfully applied to the determination of isoprenaline in human serum samples and urine samples after deproteinization.


Assuntos
Colorimetria/métodos , Ouro/química , Isoproterenol/análise , Nanopartículas Metálicas/química , Tiadiazóis/química , Adulto , Humanos , Ligação de Hidrogênio , Concentração de Íons de Hidrogênio , Isoproterenol/sangue , Isoproterenol/urina , Nanopartículas Metálicas/ultraestrutura , Espectrofotometria Infravermelho , Espectrofotometria Ultravioleta , Fatores de Tempo
11.
J Pharm Anal ; 7(6): 411-416, 2017 Dec.
Artigo em Inglês | MEDLINE | ID: mdl-29404068

RESUMO

In this work a new method is presented for simultaneous colorimetric determination of morphine(MOR) and ibuprofen(IBU) based on the aggregation of citrate-capped gold nanoparticles (AuNPs). Citrate-capped gold nanoparticles were aggregated in the presence of morphine and ibuprofen. The difference in kinetics of AuNPs aggregation in the presence of morphine / ibuprofen was used for simultaneous analysis of morphine and ibuprofen. The formation and size of synthesized Au NPs and the aggregated forms were monitored by infra-Red (IR) spectroscopy and transmission electron microscopy (TEM) respectively.. By adding morphine or ibuprofen the absorbance was decreased at 520 nm and increased at 620 nm. The difference in kinetic profiles of aggregation was applied for simultaneous analysis of MOR and IBU using partial least square regression as an efficient multivariate calibration method. The number of PLS latent variables was optimized by leave-one-out cross-validation method using predicted residual error sum of square. The proposed model exhibited a high capability in simultaneous prediction of MOR and IBU concentrations in real samples. Our results showed linear ranges of 1.33-33.29 µg/mL (R2=0.9904) and 0.28-6.9 µg/mL (R2=0.9902) for MOR and IBU respectively with low detection limits of 0.15 and 0.03 µg/mL(S/N=5).

12.
Artigo em Chinês | WPRIM (Pacífico Ocidental) | ID: wpr-664836

RESUMO

In this work a new method is presented for simultaneous colorimetric determination of morphine(MOR)and ibuprofen(IBU)based on the aggregation of citrate-capped gold nanoparticles(AuNPs).Citrate-capped AuNPs were aggregated in the presence of MOR and IBU. The difference in kinetics of AuNPs aggregation in the presence of MOR/IBU was used for simultaneous analysis of MOR and IBU. The formation and size of synthesized AuNPs and the aggregated forms were monitored by infra-red(IR)spectroscopy and transmission electron microscopy(TEM),respectively.By adding MOR or IBU the absorbance was decreased at 520 nm and increased at 620 nm.The difference in kinetic profiles of aggregation was applied for simultaneous analysis of MOR and IBU using partial least square(PLS)regression as an efficient multivariate calibration method.The number of PLS latent variables was optimized by leave-one-out cross-validation method using predicted residual error sum of square. The proposed model exhibited a high capability in simultaneous prediction of MOR and IBU concentrations in real samples. The results showed linear ranges of 1.33–33.29μg/mL (R2=0.9904) and 0.28–6.9μg/mL (R2=0.9902) for MOR and IBU respectively with low detection limits of 0.15 and 0.03μg/mL(S/N=5).

13.
Spectrochim Acta A Mol Biomol Spectrosc ; 122: 721-30, 2014 Mar 25.
Artigo em Inglês | MEDLINE | ID: mdl-24370937

RESUMO

In order to achieve the second-order advantage, second-order data per sample is usually required, e.g., kinetic-spectrophotometric data. In this study, instead of monitoring the time evolution of spectra (and collecting the kinetic-spectrophotometric data) replicate spectra are used to build a virtual second order data. This data matrix (replicate mode×λ) is rank deficient. Augmentation of these data with standard addition data [or standard sample(s)] will break the rank deficiency, making the quantification of the analyte of interest possible. The MCR-ALS algorithm was applied for the resolution and quantitation of the analyte in both simulated and experimental data sets. In order to evaluate the rotational ambiguity in the retrieved solutions, the MCR-BANDS algorithm was employed. It has been shown that the reliability of the quantitative results significantly depends on the amount of spectral overlap in the spectral region of occurrence of the compound of interest and the remaining constituent(s).


Assuntos
Espectrofotometria/métodos , Algoritmos , Calibragem , Análise dos Mínimos Quadrados , Análise Multivariada
14.
Talanta ; 85(2): 891-6, 2011 Aug 15.
Artigo em Inglês | MEDLINE | ID: mdl-21726715

RESUMO

A novel and sensitive cloud point extraction procedure using pH-sensitive hydrogel was developed for preconcentration and spectrophotometric determination of trace amounts of malachite green (MG). In this extraction method, appropriate amounts of poly(styrene-alt-maleic acid), as a pH-sensitive hydrogel, and HCl were added respectively into the aqueous sample so a cloudy solution was formed. The cloudy phase consists of hydrogel particles distributed entirely into the aqueous phase. Organic or inorganic compounds having the potential to interact with polymer particles (chemical interaction or physical adsorption) could be extracted to cloudy phase. After centrifuging, these particles of hydrogel were sedimented in the bottom of sample tube. The sedimented hydrogel-rich phase was diluted with acetonitrile and its absorbance was measured at 617 nm (λ(max) of malachite green in hydrogel). Central composite design and response surface method were applied to design the experiments and optimize the experimental parameters such as, concentration of hydrogel and HCl, extraction time and salting out effect. Under the optimum conditions, the linear range was 1 × 10(-8)-5 × 10(-7)mol L(-1) malachite green with a correlation coefficient of 0.992. The limit of detection (S/N=3) was 4.1 × 10(-9) mol L(-1). Relative standard deviation (RSD) for 7 replicate determinations of 10(-7) mol L(-1) malachite green was 3.03%. In this work, the concentration factor of 20 was reached. Also the improvement factor of the proposed method was 23. The advantages of this method are simplicity of operation, rapidity and low cost.

15.
Anal Chim Acta ; 639(1-2): 19-28, 2009 Apr 20.
Artigo em Inglês | MEDLINE | ID: mdl-19345754

RESUMO

In this work rank annihilation factor analysis (RAFA) using mean centering of ratio spectra was used to analyze the kinetic-spectrophotometric data. Annihilation of the contribution of one chemical component from the original data matrix is a general method in RAFA. However, sometimes, RAFA is not suitable for studying rank-deficient data such as kinetic-spectrophotometric measurements which involves closure rank deficiency. On the other hand, in order to apply RAFA for the determination of an analyte in an unknown sample, a standard two-way matrix of the analyte of interest with rank-one should generally be available. This is not usually attainable for kinetic-spectrophotometric monitoring of complexation reactions when both reactant and product are absorbing species. In these systems, the exact contribution of absorbing reagent should be eliminated from both unknown sample and standard calibration data matrix of analyte otherwise ordinary RAFA fails to give correct concentration of analyte of interest. Mean centering of ratio spectra using the spectrum of absorbing reagent as divisor can be used to eliminate the correct contribution of reagent for both sample data and standard calibration data of analyte. The obtained mean centering of ratio spectra matrix of sample and that of analyte of interested are full-rank and rank-one, respectively. Therefore the system can be analyzed by RAFA. The proposed method was investigated with simulated data at the first stage. The method was then applied in the analysis of experimental kinetic-spectrophotometric data of complexation reactions of Co(II), and Ni(II) with PAN in order to do multi-component determination of these ions in various real samples.

16.
J Hazard Mater ; 161(2-3): 1535-43, 2009 Jan 30.
Artigo em Inglês | MEDLINE | ID: mdl-18586388

RESUMO

In this study a homogeneous liquid-liquid extraction based on the Ph-dependent phase-separation process was investigated using a ternary solvent system (water-acetic acid-chloroform) for the preconcentration of Cu(2+) ions. 8-Hydroxy quinoline was used as the chelating agent prior to its extraction. Flame atomic absorption spectrophotometry using acetylene-air flame was used for the quantitation of analyte after preconcentration. The effect of various experimental parameters in extraction step was investigated using two optimization methods, one variable at a time and central composite design. The experimental design was done at five levels of operating parameters. Nearly the same optimized results were obtained using both methods: sample size, 5 mL; volume of NaOH 10 M, 2 mL; chloroform volume, 300 microL; 8-hydroxy quinoline concentration more than 0.01 M and salt amount did not affect the extraction significantly. Under the optimum conditions the calibration graph was linear over the range 10-2000 microg L(-1). The relative standard deviation was 7.6% for six repeated determinations (C = 500 microg L(-1)). Furthermore, the limit of detection (S/N=3) and limit of quantification (S/N=10) of the method were obtained as 1.74 and 6 microg L(-1), respectively.


Assuntos
Cobre/química , Ácido Acético/química , Calibragem , Quelantes/farmacologia , Clorofórmio/química , Íons , Ligantes , Modelos Estatísticos , Oxiquinolina/química , Hidróxido de Sódio/química , Solventes/química , Espectrofotometria Atômica/métodos , Propriedades de Superfície , Água/química , Poluentes Químicos da Água
17.
J Sep Sci ; 32(23-24): 4200-12, 2009 Dec.
Artigo em Inglês | MEDLINE | ID: mdl-20066682

RESUMO

In this study, dispersive liquid-liquid microextraction method was used for the preconcentration and simultaneous determination of Co(II) and Fe(III) in water samples as their oxinate chelates. In dispersive liquid-liquid microextraction process, methanol and chloroform were used as disperser and extracting solvents, respectively, and the ligand 8-hydroxy quinoline was used as a chelating agent for the extraction of Co(II) and Fe(III). HPLC was applied for the quantitation of the analytes after preconcentration. An experimental design, central composite design, coupled with response surface methodology was used for the optimization of the involved experimental parameters. In addition, the effect of various experimental parameters in the extraction was investigated using one variable at a time method. The calibration graphs were linear in the range of 20-4000 microg/L with the LODs of 3 microg/L for both analytes. The RSDs for six replicate measurements of 500 microg/L of Co(2+) and Fe(3+) were 3.3 and 4.1%, respectively.

18.
Talanta ; 75(3): 832-40, 2008 May 15.
Artigo em Inglês | MEDLINE | ID: mdl-18585154

RESUMO

In this study a dispersive liquid-liquid microextraction (DLLME) method based on the dispersion of an extraction solvent into aqueous phase in the presence of a dispersive solvent was investigated for the preconcentration of Cu(2+) ions. 8-Hydroxy quinoline was used as a chelating agent prior to extraction. Flame atomic absorption spectrometry using an acetylene-air flame was used for quantitation of the analyte after preconcentration. The effect of various experimental parameters on the extraction was investigated using two optimization methods, one variable at a time and central composite design. The experimental design was performed at five levels of the operating parameters. Nearly the same results for optimization were obtained using both methods: sample size 5 mL; volume of dispersive solvent 1.5 mL; dispersive solvent methanol; extracting solvent chloroform; extracting solvent volume 250 microL; 8-hydroxy quinoline concentration and salt amount do not affect significantly the extraction. Under the optimum conditions the calibration graph was linear over the range 50-2000 muicro L(-1). The relative standard deviation was 5.1% for six repeated determinations at a concentration of 500 microg L(-1). The limit of detection (S/N=3) was 3 microg L(-1).


Assuntos
Cobre/análise , Microquímica/métodos , Compostos Organometálicos/análise , Oxiquinolina/análogos & derivados , Abastecimento de Água/análise , Irã (Geográfico) , Compostos Organometálicos/química , Oxiquinolina/análise , Oxiquinolina/química , Espectrofotometria Atômica , Poluentes Químicos da Água/análise
19.
Talanta ; 76(2): 320-6, 2008 Jul 15.
Artigo em Inglês | MEDLINE | ID: mdl-18585284

RESUMO

Central composite design (CCD) and response surface methodology (RSM) were developed as experimental strategies for modeling and optimization of the influence of some variables on the performance of a new PVC membrane triiodide ion-selective electrode. This triiodide sensor is based on triiodide-clozapine ion-pair complexation. PVC, plasticizers, ion-pair amounts and pH were investigated as four variables to build a model to achieve the best Nernstian slope (59.9 mV) as response. The electrode is prepared by incorporating the ion-exchanger in PVC matrix plasticized with 2-nitrophenyl octal ether, which is directly coated on the surface of a graphite electrode. The influence of foreign ions on the electrode performance was also investigated. The optimized membranes demonstrate Nernstian response for triiodide ions over a wide linear range from 5.0 x 10(-6) to 1.0 x 10(-2)mol L(-1) with a limit of detection 2.0 x 10(-6) mol L(-1) at 25 degrees C. The electrodes could be used over a wide pH range 4-8, and have the advantages of easy to prepare, good selectivity and fast response time, long lifetime (over 3 months) and small interferences from hydrogen ion. The proposed electrode was successfully used as indicator electrode in potentiometric titration of triiodide ions and ascorbic acid.


Assuntos
Clozapina , Iodetos/análise , Eletrodos Seletivos de Íons/normas , Ácido Ascórbico/análise , Grafite , Concentração de Íons de Hidrogênio , Métodos , Cloreto de Polivinila , Sensibilidade e Especificidade
20.
Anal Chim Acta ; 613(2): 144-51, 2008 Apr 21.
Artigo em Inglês | MEDLINE | ID: mdl-18395053

RESUMO

This work presents a new and simple strategy for solving matrix effects using combination of H-point curve isolation method (HPCIM) and H-point standard addition method (HPSAM). The method uses spectrophotometric multivariate calibration data constructed by successive standard addition of an analyte into an unknown matrix. By successive standard addition of the analyte, the concentrations of remaining components (interferents) remain constant and therefore give constant cumulative spectrum for interferents in the unknown mixture. The proposed method firstly extracts such spectrum using H-point curve isolation method and then applies the obtained cumulative interferents spectrum for determination of analyte by H-point standard addition method. In order to evaluate the applicability of the method a simulated as well as several experimental data sets were tested. The method was then applied to the determination of paracetamol in pharmaceutical tablets and copper in urine samples and in a copper alloy.


Assuntos
Calibragem , Cobre/análise , Cobre/urina , Análise Multivariada , Preparações Farmacêuticas/química , Padrões de Referência , Comprimidos
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