Your browser doesn't support javascript.
loading
Mostrar: 20 | 50 | 100
Resultados 1 - 20 de 58
Filtrar
Más filtros










Base de datos
Intervalo de año de publicación
1.
Int J Biol Macromol ; 174: 216-228, 2021 Mar 31.
Artículo en Inglés | MEDLINE | ID: mdl-33516856

RESUMEN

The presence of heavy metal and radionuclides in water bodies has been a long-lasting environmental problem which results in many undesirable consequences. In this framework, the biosorption process, which uses inexpensive and naturally produced material such as alginate, is an alternative technology in the environmental remediation. This review provides relevant and recent literature regarding the application of alginate and its derivatives on removal of various heavy metal ions and radionuclides. The effects of process variables such as solution pH, adsorbent dosage, metal ion concentration, contact time, temperature and co-existing ions used in batch studies in addition to kinetic, isothermal models as well as thermodynamic that fit the adsorption experimental data are critically discussed. This review also includes mechanisms involved during adsorption process. Furthermore, future research needs for the removal of contaminants by alginate-based materials with the aims of improving their adsorption performance and their practical applications are commented.


Asunto(s)
Alginatos/química , Metales Pesados/análisis , Radioisótopos/análisis , Contaminantes del Agua/análisis , Adsorción , Concentración de Iones de Hidrógeno , Cinética , Temperatura , Termodinámica
2.
Int J Biol Macromol ; 153: 513-522, 2020 Jun 15.
Artículo en Inglés | MEDLINE | ID: mdl-32142849

RESUMEN

A new crosslinked chitosan grafted with methyl methacrylate (M-CTS) adsorbent was synthesized via free radical polymerization for effective removal of Cu(II) ions from aqueous solution. Crosslinked chitosan (1 g) was grafted with 29.96 × 10-1 M methyl methacrylate in the presence of 2.63 × 10-1 M ammonium persulfate as initiator at 60 °C for 2 h to give grafting and yield percentages of 201% and 67%, respectively. Batch adsorption experiment was performed as a function of solution pH, initial metal ion concentration and contact time. The isotherm data were adequately described by Langmuir model, while kinetic study revealed that the pseudo-second order rate model best fitted for the experimental data. The maximum adsorption capacity for M-CTS at pH 4 was 192.31 mg g-1. Furthermore, the reusability of over six adsorption-desorption cycles suggested that M-CTS is a durable adsorbent and good candidate for metal ions treatment.


Asunto(s)
Quitosano/química , Cobre/química , Purificación del Agua , Adsorción , Cationes Bivalentes/química
3.
J Chromatogr A ; 1612: 460638, 2020 Feb 08.
Artículo en Inglés | MEDLINE | ID: mdl-31676087

RESUMEN

Magnetic solid phase extraction (MSPE) employing oil-palm fiber activated carbon (OPAC) modified with magnetite (Fe3O4) and polypyrrole (OPAC-Fe3O4-PPy) was successfully used for the determination of two organochlorine pesticides (OCPs), namely endosulfan and dieldrin in environmental water samples. Analysis was performed using gas chromatography with micro-electron capture detection (GC-µECD). The effects of three preparation variables, namely Fe3O4:OPAC ratio, amount of pyrrole monomer, and amount of FeCl3 oxidant were optimized using Box-Behnken design (BBD) (R2 < 0.99, p-value < 0.001%). The optimum conditions were as follows: Fe3O4:OPAC ratio of 2:1 w/w, 1 g of FeCl3 and 100 µL of pyrrole monomer. The experimental results obtained agreed satisfactorily with the model prediction (> 90% agreement). Optimized OPAC-Fe3O4-PPy composite was characterized using field emission scanning electron microscope, vibrating sample magnetometer and Fourier transform infrared spectroscopy. Four numerical parameters of MSPE procedure was optimized using BBD. The significance of the MSPE parameters were salt addition > sample solution pH > extraction time and desorption time. Under the optimized conditions (extraction time: 90 s, desorption time: 10 min, salt: 0%, and pH: 5.8), the method demonstrated good linearity (25-1000 ng L-1) with coefficients of determination, R2 > 0.991, and low detection limits for both endosulfan (7.3 ng L-1) and dieldrin (8.6 ng L-1). The method showed high analyte recoveries in the range of 98.6-103.5% for environmental water samples. The proposed OPAC-Fe3O4-PPy MSPE method offered good features such as sustainability, simplicity, and rapid extraction.


Asunto(s)
Cromatografía de Gases , Hidrocarburos Clorados/análisis , Plaguicidas/análisis , Extracción en Fase Sólida/métodos , Contaminantes Químicos del Agua/análisis , Fibra de Carbono , Carbón Orgánico , Electrones , Óxido Ferrosoférrico/química , Límite de Detección , Fenómenos Magnéticos , Aceite de Palma , Polímeros , Pirroles/química
4.
J Environ Manage ; 253: 109658, 2020 Jan 01.
Artículo en Inglés | MEDLINE | ID: mdl-31666209

RESUMEN

A new effective adsorbent, 3-aminopropyltrimethoxysilane functionalized magnetic sporopollenin (MSp@SiO2NH2) based silica-coated graphene oxide (GO), (GO@SiO2-MSp@SiO2NH2) was successfully synthesized and applied for the first time in the removal of hazardous Pb(II) ions from aqueous solution. The properties of the composite were characterized using Fourier-transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), field emission scanning electron microscopy (FESEM), energy-dispersive X-ray spectroscopy (EDX) and vibrating-sample magnetometery (VSM). Evaluation of GO@SiO2-MSp@SiO2NH2 adsorption performance at optimum conditions revealed that the adsorbent has a maximum adsorption capacity of 323.5 mg/g for Pb(II) using 50-200 mg/L initial Pb(II) ions concentrations. Initial and final concentrations of Pb(II) ions in aqueous solution were analyzed using graphite furnace atomic absorption spectroscopy (GF-ASS). The adsorption behavior of Pb(II) ions onto GO@SiO2-MSp@SiO2NH2 was studied using Langmuir, Freundlich and Temkin isotherms models. The values of coefficient of determination showed that the adsorption best fitted the Langmuir model (R2 = 0.9994). Kinetic studies suggested that the adsorption of Pb(II) ion followed a pseudo-second-order rate model (R2 = 1.00) and thermodynamic studies revealed that the adsorption process is endothermic and spontaneous. The effect of co-existing ions on Pb(II) ion adsorption were also studied and found to have considerable effects only at higher matrix concentration. The adsorbent can be reused up to ten times and retain its good adsorption capacity. In addition, GO@SiO2-MSp@SiO2NH2 showed great potential for Pb(II)removal from industrial wastewater samples.


Asunto(s)
Grafito , Contaminantes Químicos del Agua , Adsorción , Biopolímeros , Carotenoides , Cinética , Plomo , Óxidos , Propilaminas , Silanos , Dióxido de Silicio
5.
Methods Mol Biol ; 1985: 407-416, 2019.
Artículo en Inglés | MEDLINE | ID: mdl-31069749

RESUMEN

Particular attention has been paid to capillary electrophoresis as versatile and environmentally friendly approach for enantioseparations of a wide spectrum of compounds. Cyclodextrin-modified micellar electrokinetic chromatography (CD-MEKC) is a method of choice to provide effective separation toward hydrophobic and uncharged stereoisomers. The chiral discrimination of the solutes relies upon the partitioning between a given CD in the aqueous phase and micelles formed from a surfactant. Synergistic combinations of chiral selectors, surfactant, and modifier contribute to successful enantioseparations of the enantiomers. In this chapter, an application of CD-MEKC for the enantioseparation of selected imidazole drugs employing a dual CDs system is described.


Asunto(s)
Cromatografía Capilar Electrocinética Micelar/métodos , Ciclodextrinas/química , Imidazoles/química , Preparaciones Farmacéuticas/química , Preparaciones Farmacéuticas/aislamiento & purificación , Estereoisomerismo
6.
Int J Biol Macromol ; 133: 1260-1267, 2019 Jul 15.
Artículo en Inglés | MEDLINE | ID: mdl-31047925

RESUMEN

Grafting of crosslinked chitosan with monomer, N-vinyl-2-pyrrolidone, has been carried out to investigate its adsorption capacity toward Orange G (OG) from aqueous solutions. The adsorption performance of modified chitosan (cts(x)-g-PNVP) was examined and compared with that of the unmodified chitosan. The effects of initial pH, contact time and initial dye concentration were investigated in a batch system. The experimental data were correlated with the Langmuir and Freundlich isotherm models. The maximum adsorption capacity of cts(x)-g-PNVP (63.7mgg-1) based on Langmuir equation was relatively higher than that of the unmodified chitosan (1.7mgg-1). The kinetic studies showed that the adsorption process was consistent with the pseudo-second order kinetic model. Interaction mechanisms between OG and cts(x)-g-PNVP were also proposed. The overall results suggested that the prepared cts(x)-g-PNVP stands a good candidate as adsorbent for removal of anionic dye from aqueous solutions.


Asunto(s)
Compuestos Azo/química , Compuestos Azo/aislamiento & purificación , Quitosano/química , Microesferas , Purificación del Agua/métodos , Agua/química , Adsorción , Concentración de Iones de Hidrógeno , Cinética , Soluciones , Contaminantes Químicos del Agua/química , Contaminantes Químicos del Agua/aislamiento & purificación
7.
Environ Sci Process Impacts ; 21(4): 714-726, 2019 Apr 17.
Artículo en Inglés | MEDLINE | ID: mdl-30869668

RESUMEN

A novel nanocomposite of MGO-NGC, composed of magnetic Fe3O4 nanoparticles (M), graphene oxide (GO), and N-methyl-d-glucamine functionalized calix[4]arene (NGC), was synthesized and applied as an effective adsorbent for the removal of two selected pesticides, namely hexaconazole and chlorpyrifos from water samples. The adsorbent was characterized by FTIR, SEM, EDX, TEM, and XRD. The main parameters affecting the adsorption process such as adsorbent dosage, pH of sample solution, salt effect, pesticide concentration, and adsorption time were investigated. The data from kinetic studies fitted well to the pseudo-second order kinetic model with R2 > 0.99. Among the isotherm models of Langmuir, Freundlich, Temkin, and Dubinin-Radushkevich, the Langmuir isotherm fitted well to the adsorption process and demonstrated the monolayer adsorption pattern of the pesticides. Moreover, high adsorption capacities of 78.74 and 93.46 mg g-1 were obtained for chlorpyrifos and hexaconazole, respectively. Thermodynamic and free energy data indicated the physisorption mechanism for the adsorption process. The new adsorbent can be employed as an efficient, environment friendly, and highly reusable alternative for the removal of chlorinated pesticides from aqueous media.


Asunto(s)
Calixarenos/química , Grafito/química , Plaguicidas/aislamiento & purificación , Fenoles/química , Termodinámica , Contaminantes Químicos del Agua/aislamiento & purificación , Adsorción , Cinética , Nanocompuestos , Purificación del Agua
8.
Environ Technol ; 40(19): 2482-2493, 2019 Aug.
Artículo en Inglés | MEDLINE | ID: mdl-29464995

RESUMEN

Magnetic nanocomposites adorned with calixarene were successfully prepared by immobilizing diethanolamine functionalized p-tert-butylcalix[4]arene (DEA-Calix) onto silica-coated magnetic nanoparticles (MNPs). The synthesis, surface morphology, purity, elemental composition and thermal stability of newly prepared nanocomposites were analyzed using FT-IR spectroscopy, scanning electron microscopy (SEM), energy dispersive spectroscopy (EDX), X-ray diffractometer (XRD), thermal gravimetric analysis (TGA) and vibrating sample magnetometer (VSM). Magnetic solid-phase adsorption (MSPA) was employed to explore the adsorption behavior of DEA-Calix-MNPs towards Pb(II) from water samples prior to its flame atomic absorption spectrometric analysis. The essential analytical factors governing the adsorption efficiency such as solution pH, mass of adsorbent, concentration and contact time have been investigated and optimized. The results depict that DEA-Calix-MNPs has excellent adsorption efficiency 97% (at pH 5.5) with high adsorption capacity of 51.81 mg g-1 for Pb(II) adsorption. Additionally, kinetic and equilibrium studies suggested that Pb(II) adsorption process follows a pseudo-second-order model and Langmuir isotherms, respectively. Real sample analysis also confirmed field applicability of the new DEA-Calix-MNPs adsorbent.


Asunto(s)
Calixarenos , Nanocompuestos , Contaminantes Químicos del Agua , Adsorción , Plomo , Espectroscopía Infrarroja por Transformada de Fourier
9.
J Sep Sci ; 41(19): 3751-3763, 2018 Oct.
Artículo en Inglés | MEDLINE | ID: mdl-30125466

RESUMEN

This study describes a dispersive liquid-liquid microextraction combined with dispersive solid-phase extraction method based on phenyl-functionalized magnetic sorbent for the preconcentration of polycyclic aromatic hydrocarbons from environmental water, sugarcane juice, and tea samples prior to gas chromatography with mass spectrometry analysis. Several important parameters affecting the extraction efficiency were investigated thoroughly, including the mass of sorbent, type and volume of extraction solvent, extraction time, type of desorption solvent, desorption time, type and amount of salt-induced demulsifier, and sample volume. Under the optimized extraction and gas chromatography-mass spectrometric conditions, the method revealed good linearity (10-100000 ng/L) with coefficient of determination (R2 ) of ≥0.9951, low limits of detection (3-16 ng/L), high enrichment factors (61-239), and satisfactory analyte recoveries (86.3-109.1%) with the relative standard deviations < 10% (n = 5). The entire sample preparation procedure was simple, rapid and can be accomplished within 10 min. This method was applied (after pretreatment) to 30 selected samples, and the presence of studied analytes was quantified in 17 samples.

10.
J Sep Sci ; 41(14): 2942-2951, 2018 Jul.
Artículo en Inglés | MEDLINE | ID: mdl-29877605

RESUMEN

We describe the preparation, characterization, and application of a composite film adsorbent based on blended agarose-chitosan-multiwalled carbon nanotubes for the preconcentration of selected nonsteroidal anti-inflammatory drugs in aqueous samples before determination by high performance liquid chromatography with ultraviolet detection. The composite film showed a high surface area (4.0258 m2 /g) and strong hydrogen bonding between the multiwalled carbon nanotubes and agarose/chitosan matrix, which prevent adsorbent deactivation and ensure long-term stability. Several parameters, such as sample pH, addition of salt, extraction time, desorption solvent, and concentration of multiwalled carbon nanotubes in the composite film were optimized using a one-factor-at-time approach. The optimum extraction conditions obtained were as follows: isopropanol as conditioning solvent, 10 mL of sample solution at pH 2, extraction time of 30 min, stirring speed of 600 rpm, 100 µL of isopropanol as desorption solvent, desorption time of 5 min under ultrasonication, and 0.4% w/v of composite film. Under the optimized conditions, the calibration curve showed good linearity in the range of 1-500 ng/mL (r2  = 0.997-0.999), and good limits of detection (0.89-8.05 ng/mL) were obtained with good relative standard deviations of < 4.59% (n = 3) for the determination of naproxen, diclofenac sodium salt, and mefenamic acid drugs.

11.
Int J Biol Macromol ; 116: 255-263, 2018 Sep.
Artículo en Inglés | MEDLINE | ID: mdl-29746971

RESUMEN

In this study, the Cu(II) and Cd(II) ions removal behavior of crosslinked chitosan beads grafted poly(methacrylamide) (abbreviated as crosslinked chitosan-g-PMAm) from single metal ion solutions was investigated. The modified chitosan beads presented a remarkable improvement in acid resistance. The batch experiments demonstrated that pH of solution played a significant role in adsorption. It was found that the adsorption of Cu(II) and Cd(II) were optimum at pH 4 and pH 5, respectively. The maximum adsorption capacities for Cu(II) and Cd(II) based on Langmuir equation were 140.9 mg g-1 and 178.6 mg g-1, respectively. Pseudo-second order gave a better fit for adsorption data with respect to linearity coefficients than pseudo-first order suggesting that chemisorption or electron transfer is the dominant mechanism of the metal ions onto crosslinked chitosan-g-PMAm. In addition, X-ray photoelectron spectroscopy (XPS) investigations revealed that adsorption of both metal ions took place on the surfaces of crosslinked chitosan-g-PMAm by chelation through CNH2, CO and CO groups. Overall, the modified chitosan has proved a promising adsorbent for removal of metal ions.


Asunto(s)
Cadmio/química , Quitosano/química , Cobre/química , Iones/química , Adsorción , Concentración de Iones de Hidrógeno , Cinética , Espectroscopía de Fotoelectrones/métodos , Contaminantes Químicos del Agua/química , Purificación del Agua/métodos
12.
Int J Biol Macromol ; 107(Pt A): 891-897, 2018 Feb.
Artículo en Inglés | MEDLINE | ID: mdl-28935540

RESUMEN

Crosslinked chitosan beads were grafted with N-vinyl-2-pyrrolidone (NVP) using ammonium persulfate (APS) as free radical initiator. Important variables on graft copolymerization such as temperature, reaction time, concentration of initiator and concentration of monomer were optimized. The results revealed optimum conditions for maximum grafting of NVP on 1g crosslinked chitosan as follows: reaction temperature, 60°C; reaction time, 2h and concentrations of APS and NVP of 2.63×10-1M and 26.99×10-1M, respectively. The modified chitosan beads were characterized by FTIR spectroscopy, 13C NMR, SEM and BET to provide evidence of successful crosslinking and grafting reactions. The resulting material (cts(x)-g-PNVP) was evaluated as adsorbent for the removal of Cu(II) ions from aqueous solutions in a batch experiment. The Langmuir and Freundlich adsorption models were also applied to describe the equilibrium isotherms. The results showed that the adsorption of the copper ions onto the beads agreed well with Langmuir model with the maximum capacity (qmax) of 122mgg-1.


Asunto(s)
Quitosano/química , Cobre/química , Contaminantes Químicos del Agua/química , Purificación del Agua , Cobre/toxicidad , Reactivos de Enlaces Cruzados/química , Iones/química , Iones/toxicidad , Cinética , Pirrolidinonas/química , Agua/química , Contaminantes Químicos del Agua/toxicidad
13.
J Sep Sci ; 41(1): 195-208, 2018 Jan.
Artículo en Inglés | MEDLINE | ID: mdl-28834218

RESUMEN

The efficiency of the extraction and removal of pollutants from food and the environment has been an important issue in analytical science. By incorporating inorganic species into an organic matrix, a new material known as an organic-inorganic hybrid material is formed. As it possesses high selectivity, permeability, and mechanical and chemical stabilities, organic-inorganic hybrid materials constitute an emerging research field and have become popular to serve as sorbents in various separaton science methods. Here, we review recent significant advances in analytical solid-phase extraction employing organic-inorganic composite/nanocomposite sorbents for the extraction of organic and inorganic pollutants from various types of food and environmental matrices. The physicochemical characteristics, extraction properties, and analytical performances of sorbents are discussed; including morphology and surface characteristics, types of functional groups, interaction mechanism, selectivity and sensitivity, accuracy, and regeneration abilities. Organic-inorganic hybrid sorbents combined with extraction techniques are highly promising for sample preparation of various food and environmental matrixes with analytes at trace levels.


Asunto(s)
Contaminantes Ambientales/análisis , Contaminación de Alimentos/análisis , Nanocompuestos/química , Extracción en Fase Sólida , Adsorción , Ambiente , Ensayo de Materiales , Nanopartículas del Metal , Compuestos Orgánicos , Permeabilidad , Polímeros/química , Dióxido de Silicio
14.
Food Chem ; 239: 208-216, 2018 Jan 15.
Artículo en Inglés | MEDLINE | ID: mdl-28873561

RESUMEN

Graphene (G) modified with magnetite (Fe3O4) and sol-gel hybrid tetraethoxysilane-methyltrimethoxysilane (TEOS-MTMOS) was used as a clean-up adsorbent in magnetic solid phase extraction (MSPE) for direct determination of acrylamide in various food samples prior to gas chromatography-mass spectrometry analysis. Good linearity (R2=0.9990) was achieved for all samples using matrix-matched calibration. The limit of detection (LOD=3×SD/m) obtained was 0.061-2.89µgkg-1 for the studied food samples. Native acrylamide was found to be highest in fried potato with bright-fleshed (900.81µgkg-1) and lowest in toasted bread (5.02µgkg-1). High acrylamide relative recovery (RR=82.7-105.2%) of acrylamide was obtained for spiked (5 and 50µgkg-1) food samples. The Fe3O4@G-TEOS-MTMOS is reusable up to 7 times as a clean-up adsorbent with good recovery (>85%). The presence of native acrylamide was confirmed by mass analysis at m/z=71 ([C3H5NO]+) and m/z=55 ([C3H3O]+).


Asunto(s)
Acrilamida/análisis , Análisis de los Alimentos , Cromatografía de Gases y Espectrometría de Masas , Grafito , Magnetismo , Extracción en Fase Sólida
15.
J Chromatogr Sci ; 56(2): 166-176, 2018 Feb 01.
Artículo en Inglés | MEDLINE | ID: mdl-29069322

RESUMEN

Two-phase micro-electrodriven membrane extraction (EME) procedure for the pre-concentration of selected non-steroidal anti-inflammatory drugs (NSAIDs) in aquatic matrices was investigated. Agarose film was used as interface between donor and acceptor phase in EME which allowed for selective extraction of the analytes prior to high performance liquid chromatography-ultraviolet detection. Charged analytes were transported from basic aqueous sample solution through agarose film into 1-octanol as an acceptor phase at 9 V potential. Response surface methodology in conjunction with the central composite design showed good correlations between extraction time and applied voltage (R2 > 0.9358). Under optimized extraction conditions, the method showed good linearity in the concentration range of 0.5-500 µg L-1 with coefficients of determination, r2≥ 0.9942 and good limits of detection (0.14-0.42 µg L-1) and limits of quantification (0.52-1.21 µg L-1). The results also showed high enrichment factors (62-86) and good relative recoveries (72-114%) with acceptable reproducibilities (RSDs ≤ 7.5% n = 3). The method was successfully applied to the determination of NSAIDs from tap water and river water samples. The proposed method proved to be rapid, simple and requires low voltage and minute amounts of organic solvent, thus environmentally friendly.


Asunto(s)
Antiinflamatorios no Esteroideos , Cromatografía Líquida de Alta Presión/métodos , Contaminantes Químicos del Agua , 1-Octanol , Antiinflamatorios no Esteroideos/análisis , Antiinflamatorios no Esteroideos/aislamiento & purificación , Técnicas Electroquímicas/instrumentación , Técnicas Electroquímicas/métodos , Diseño de Equipo , Límite de Detección , Modelos Lineales , Reproducibilidad de los Resultados , Contaminantes Químicos del Agua/análisis , Contaminantes Químicos del Agua/aislamiento & purificación
16.
J Chromatogr Sci ; 56(2): 177-186, 2018 Feb 01.
Artículo en Inglés | MEDLINE | ID: mdl-29186451

RESUMEN

In this study, caged calcium alginate-caged multiwalled carbon nanotubes dispersive microsolid phase extraction was described for the first time for the extraction of polycyclic aromatic hydrocarbons (PAHs) from water samples prior to gas chromatographic analysis. Fluorene, phenanthrene and fluoranthene were selected as model compounds. The caged calcium alginate-caged multiwalled carbon nanotubes was characterized by Fourier transform infrared spectroscopy, scanning electron microscopy and thermal gravimetry analyses. The effective parameters namely desorption solvent, solvent volume, extraction time, desorption time, the mass of adsorbent and sample volume were optimized. Under the optimum extraction conditions, the developed method showed good linearity in the range of 0.5-50 ng mL-1 (R2 ≥ 0.996), low limits of detection and quantification (0.42-0.22 ng mL-1) (0.73-1.38 ng mL-1) respectively, good relative recoveries (71.2-104.2%) and reproducibility (RSD 1.8-12.4%, n = 3) for the studied PAHs in water sample. With high enrichment factor (1,000), short extraction time (<30 min), low amounts of adsorbent (100 mg) and low amounts of solvent (0.1 mol) have proven that the microsolid phase extraction method based on calcium alginate-caged multiwalled carbon nanotubes are environmentally friendly and convenient extraction method to use as an alternative adsorbent in the simultaneous preconcentration of PAHs from environmental water samples.


Asunto(s)
Alginatos/química , Cromatografía de Gases/métodos , Nanotubos de Carbono/química , Hidrocarburos Policíclicos Aromáticos/análisis , Extracción en Fase Sólida/métodos , Contaminantes Químicos del Agua/análisis , Ácido Glucurónico/química , Ácidos Hexurónicos/química , Límite de Detección , Modelos Lineales , Hidrocarburos Policíclicos Aromáticos/química , Hidrocarburos Policíclicos Aromáticos/aislamiento & purificación , Reproducibilidad de los Resultados , Contaminantes Químicos del Agua/química , Contaminantes Químicos del Agua/aislamiento & purificación
17.
J Chromatogr A ; 1532: 50-57, 2018 Jan 12.
Artículo en Inglés | MEDLINE | ID: mdl-29241956

RESUMEN

A facile dispersive-micro-solid phase extraction (D-µ-SPE) method coupled with HPLC for the analysis of selected non-steroidal anti-inflammatory drugs (NSAIDs) in water samples was developed using a newly prepared magnetic sporopollenin-cyanopropyltriethoxysilane (MS-CNPrTEOS) sorbent. Sporopollenin homogenous microparticles of Lycopodium clavatum spores possessed accessible functional groups that facilitated surface modification. Simple modification was performed by functionalization with 3-cyanopropyltriethoxysilane (CNPrTEOS) and magnetite was introduced onto the biopolymer to simplify the extraction process. MS-CNPrTEOS was identified by infrared spectrometrywhile the morphology and the magnetic property were confirmed by scanning electron microscopy (SEM) and vibrating sample magnetometer (VSM), respectively. To maximize the extraction performance of ketoprofen, ibuprofen, diclofenac and mefenamic acid using the proposed MS-CNPrTEOS, important D-µ-SPE parameters were comprehensively optimized. The optimum extraction conditions were sorbent amount, 40 mg; extraction time, 5 min; desorption time; 5 min; sample volume, 15 mL; sample pH 2.0; and salt addition, 2.5% (w/v). The feasibility of the developed method was evaluated using spiked tap water, lake water, river water and waste water samples. Results showed that ketoprofen and ibuprofen were linear in the range of 1.0-1000 µg L-1 whilst diclofenac and mefenamic acid were linear in the range 0.8-500 µg L-1. The results also showed good detection limits for the studied NSAIDs in the range of 0.21-0.51 µg L-1 and good recoveries for spiked water samples in the range of 85.1-106.4%. The MS-CNPrTEOS proved a promising dispersive sorbent and applicable to facile and rapid assay of NSAIDs in water samples.


Asunto(s)
Antiinflamatorios no Esteroideos/análisis , Cromatografía Líquida de Alta Presión , Monitoreo del Ambiente/métodos , Agua Dulce/química , Microextracción en Fase Sólida , Biopolímeros/análisis , Biopolímeros/química , Carotenoides/química , Ibuprofeno/análisis , Cetoprofeno/análisis , Límite de Detección , Magnetismo , Aguas Residuales/química , Contaminantes Químicos del Agua/análisis
18.
J Sep Sci ; 40(21): 4222-4233, 2017 Nov.
Artículo en Inglés | MEDLINE | ID: mdl-28837263

RESUMEN

A new facile magnetic micro-solid-phase extraction coupled to gas chromatography and mass spectrometry detection was developed for the extraction and determination of selected antidepressant drugs in biological fluids using magnetite-MCM-41 as adsorbent. The synthesized sorbent was characterized by several spectroscopic techniques. The maximum extraction efficiency for extraction of 500 µg/L antidepressant drugs from aqueous solution was obtained with 15 mg of magnetite-MCM-41 at pH 12. The analyte was desorbed using 100 µL of acetonitrile prior to gas chromatography determination. This method was rapid in which the adsorption procedure was completed in 60 s. Under the optimized conditions using 15 mL of antidepressant drugs sample, the calibration curve showed good linearity in the range of 0.05-500 µg/L (r2  = 0.996-0.999). Good limits of detection (0.008-0.010 µg/L) were obtained for the analytes with good relative standard deviations of <8.0% (n = 5) for the determination of 0.1, 5.0, and 500.0 µg/L of antidepressant drugs. This method was successfully applied to the determination of amitriptyline and chlorpromazine in plasma and urine samples. The recoveries of spiked plasma and urine samples were in the range of 86.1-115.4%. Results indicate that magnetite micro-solid-phase extraction with gas chromatography and mass spectrometry is a convenient, fast, and economical method for the extraction and determination of amitriptyline and chlorpromazine in biological samples.


Asunto(s)
Antidepresivos/sangre , Antidepresivos/orina , Óxido Ferrosoférrico , Dióxido de Silicio , Amitriptilina/sangre , Amitriptilina/orina , Clorpromazina/sangre , Clorpromazina/orina , Cromatografía de Gases y Espectrometría de Masas , Humanos , Nanopartículas de Magnetita , Extracción en Fase Sólida
19.
J Sep Sci ; 40(21): 4256-4263, 2017 Nov.
Artículo en Inglés | MEDLINE | ID: mdl-28851082

RESUMEN

Polypyrrole-magnetite dispersive micro-solid-phase extraction method combined with ultraviolet-visible spectrophotometry was developed for the determination of selected cationic dyes in textile wastewater. Polypyrrole-magnetite was used as adsorbent due to its thermal stability, magnetic properties, and ability to adsorb Rhodamine 6G and crystal violet. Dispersive micro-solid-phase extraction parameters were optimized, including sample pH, adsorbent amount, extraction time, and desorption solvent. The optimum polypyrrole-magnetite dispersive micro-solid phase-extraction conditions were sample pH 8, 60 mg polypyrrole-magnetite adsorbent, 5 min of extraction time, and acetonitrile as the desorption solvent. Under the optimized conditions, the polypyrrole-magnetite dispersive micro-solid-phase extraction with ultraviolet-visible method showed good linearity in the range of 0.05-7 mg/L (R2  > 0.9980). The method also showed a good limit of detection for the dyes (0.05 mg/L) and good analyte recoveries (97.4-111.3%) with relative standard deviations < 10%. The method was successfully applied to the analysis of dyes in textile wastewater samples where the concentration found was 1.03 mg (RSD ±7.9%) and 1.13 mg/L (RSD ± 4.6%) for Rhodamine 6G and crystal violet, respectively. It can be concluded that this method can be adopted for the rapid extraction and determination of dyes at trace concentration levels.

20.
Crit Rev Anal Chem ; 47(4): 332-339, 2017 Jul 04.
Artículo en Inglés | MEDLINE | ID: mdl-28266865

RESUMEN

The ionic liquids (ILs) are salts with melting points below 100°C. These are called as ionic fluids, ionic melts, liquid electrolytes, fused salts, liquid salts, ionic glasses, designer solvents, green solvents and solvents of the future. These have a wide range of applications, including medical, pharmaceutical and chemical sciences. Nowadays, their use is increasing greatly in separation science, especially in chromatography and capillary electrophoresis due to their remarkable properties. The present article describes the importance of ILs in high-performance liquid chromatography and capillary electrophoresis. Efforts were also made to highlight the future expectations of ILs.


Asunto(s)
Cromatografía Líquida de Alta Presión/métodos , Electroforesis Capilar/métodos , Líquidos Iónicos/química , Animales , Humanos , Líquidos Iónicos/toxicidad
SELECCIÓN DE REFERENCIAS
DETALLE DE LA BÚSQUEDA
...