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1.
J Sep Sci ; 41(2): 475-482, 2018 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-28988449

RESUMO

Surfactant-assisted electromembrane extraction coupled with cyclodextrin-modified capillary electrophoresis was developed for the separation and determination of Tranylcypromine enantiomers in biological samples. This combination would provide a new strategy for selective and sensitive determination of target analytes. The addition of surfactant in the donor solution improved the analyte transport into the lumen of hollow fiber that resulted in an enhancement in the analytes migration into acceptor solution. Optimization of the variables, affecting proposed method, was carried out and best results were achieved with a 175 V potential as driving force of the electromembrane extraction, 2-nitrophenyloctylether as the supported liquid membrane, donor solution containing 0.2 mM Triton X-100 with pH 3 and 0.1 M HCl for acceptor solution. Then, the extract was analyzed using cyclodextrin-modified capillary electrophoresis method for separation of Tranylcypromine enantiomers. The best results were obtained with a phosphate running buffer (100 mM, pH 2.0) containing 7% w/v hydroxypropyl-α-cyclodextrin. Under the optimum conditions, a low limit of detection (3.03 ng/mL), good linearity (R2  > 0.9953), and relative standard deviations below 4.0% (n = 5) were obtained. Finally, this procedure was applied to determine the concentration of Tranylcypromine enantiomers in urine samples with satisfactory results.


Assuntos
Ciclodextrinas/química , Tensoativos/química , Tranilcipromina/química , Tranilcipromina/urina , Urinálise/métodos , Eletroforese Capilar , Humanos , Concentração de Íons de Hidrogênio , Íons , Octoxinol/química , Fosfatos/química , Estereoisomerismo , Temperatura , alfa-Ciclodextrinas/química
2.
J Sep Sci ; 40(15): 3114-3119, 2017 Aug.
Artigo em Inglês | MEDLINE | ID: mdl-28581637

RESUMO

A simple, fast, sensitive, and low-cost method was developed for the quantification of nitroaromatic compounds in water samples based on CO2 -assisted liquid-phase microextraction using a switchable-hydrophilicity solvent followed by gas chromatography detection. Dipropylamine was used as extraction solvent with switchable hydrophilicity that can be miscible or immiscible upon the addition or removal of CO2 as a reagent. Experimental parameters affecting the extraction efficiency such as the volume of acceptor phase, the volume of donor phase, pH of donor phase, ionic strength, and extraction time were investigated. Under the optimal conditions, detection limits and preconcentration factors were obtained in the ranges of 0.9-1.8 µg/L and 132-138, respectively. Also, the extraction recoveries of water samples were above 88%. Finally, the developed method was successfully applied to the determination of nitroaromatic compounds in real water samples.

3.
Electrophoresis ; 36(24): 3034-41, 2015 Dec.
Artigo em Inglês | MEDLINE | ID: mdl-26383092

RESUMO

In this paper, for the first time, surfactant-assisted electromembrane extraction coupled with capillary electrophoresis with UV detector was introduced for the extraction of acidic drugs from biological fluids. In this technique, in the presence of the nonionic surfactant in the donor phase, tendency of analyte ions into the supported liquid membrane (SLM) was increased. Naproxen and diclofenac were selected as model acidic drugs. In order to obtain the best extraction efficiency, several factors influencing the extraction efficiency were investigated. Optimal extractions were accomplished with 1-octanol as the SLM, 15 Volt dc potential as the driving force, pH 12 in acceptor solution, and 0.2 mmol/L Triton X-100 with pH 7.4 in donor solution. Equilibrium extraction conditions were obtained after 15 min of operation where the whole assembly agitated at 1000 rpm. Under the optimized conditions, preconcentration factors in the range of 176-184 and recoveries in the range of 88-92% were obtained. The applied method offers acceptable linearity with correlation coefficients higher than 0.9992. Limits of detection of 1.51 ng/mL and 2.42 ng/mL were obtained for naproxen and diclofenac, respectively. Finally, the developed method was successfully applied for the determination of naproxen and diclofenac in different matrices including plasma and urine samples.


Assuntos
Fracionamento Químico/métodos , Eletroforese Capilar/métodos , Tensoativos/química , Humanos , Limite de Detecção , Modelos Lineares , Membranas Artificiais , Preparações Farmacêuticas/sangue , Preparações Farmacêuticas/química , Preparações Farmacêuticas/urina , Reprodutibilidade dos Testes
4.
J Chromatogr A ; 1378: 1-7, 2015 Jan 23.
Artigo em Inglês | MEDLINE | ID: mdl-25560453

RESUMO

This paper proposes for the first time the use of a nonionic surfactant for the enhancement of electromembrane extraction performance. The presence of nonionic surfactant in donor phase promotes ionic analytes efficient migration through the organic liquid membrane. Surfactant assisted electromembrane extraction coupled with capillary electrophoresis was used for the extraction of basic drugs (methamphetamine, ephedrine and methadone) from biological samples. Parameters that affect the extraction efficiency were investigated and optimized for the proposed method. Optimal extractions were accomplished with 2-nitrophenyl octyl ether as the supported liquid membrane, with 125V as the driving force and 0.2mM Triton X-100 with pH 5.0 in donor and pH 1 in acceptor solutions. Equilibrium extraction conditions were obtained after 20min of operation where the whole assembly agitated at 1000rpm. Under the optimum experimental conditions, good limits of detection (0.90-2.42ngmL(-1)), linearities (R(2)>0.9995), and repeatability of extraction (RSDs below 4.4%, n=5) were obtained. Finally, the developed method was applied to drug level monitoring in the biological samples including hair and urine samples and satisfactory results were obtained.


Assuntos
Técnicas de Química Analítica/métodos , Éteres/química , Preparações Farmacêuticas/análise , Tensoativos/química , Eletroforese Capilar , Membranas Artificiais , Octoxinol/química
5.
J Sep Sci ; 37(1-2): 85-91, 2014 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-24243888

RESUMO

In this work, carbon-nanotube-assisted electromembrane extraction in the two-phase mode combined with GC was developed for the preconcentration and determination of basic drugs in body fluids. The multiwalled carbon nanotubes dispersed in organic solvent are held in the pores of the porous fiber wall by capillary forces and sonification. The membrane with immobilized carbon nanotubes acts as a sorbent and provides an additional pathway for analyte transport. This study demonstrates that the immobilization of carbon nanotubes in the supported liquid membrane is an excellent approach to enhance the performance of the extraction. Optimization of the variables affecting this method was carried out in order to achieve the best extraction efficiency. Optimal extractions were accomplished with octanol as the extraction solvent, 50 V as the driving force and pH 7.4 in the sample solution with the whole assembly agitated at 1000 rpm for 20 min. Under the optimized extraction conditions, the proposed technique provided good linearity (R(2) > 0.9990), repeatability (3.5-3.8%), low LODs (1.5 ng/mL), good preconcentration factors (292-316) and high recoveries (80-87%). Finally, this method was successfully used for the determination of tramadol and methadone in different body fluids including plasma and urine samples.


Assuntos
Cromatografia Gasosa/métodos , Técnicas Eletroquímicas/métodos , Nanotubos de Carbono/química , Preparações Farmacêuticas/análise , Preparações Farmacêuticas/isolamento & purificação , Extração em Fase Sólida/métodos , Adsorção , Técnicas Eletroquímicas/instrumentação , Membranas Artificiais , Extração em Fase Sólida/instrumentação
6.
J Chromatogr A ; 1285: 1-6, 2013 Apr 12.
Artigo em Inglês | MEDLINE | ID: mdl-23473518

RESUMO

A new design of low voltage electromembrane extraction (EME) using carbon nanotube reinforced hollow fiber was developed for the determination of acidic drugs in biological and wastewater samples. The supported liquid membrane (SLM) with carbon nanotubes as the sorbent interface was used in this research. CNTs have large surface area and high adsorption capacity for a wide range of organic and inorganic species. Therefore, the presence of CNTs in SLM increased the overall analyte partition coefficient in the membrane and lead to enhancement in analyte transport. Optimization of the variables affecting this method was carried out in order to achieve the best extraction efficiency. Ibuprofen and naproxen, nonsteroid anti-inflammatory drugs (NSAIDs), were selected as model acidic drugs. Optimal extractions were accomplished with 1-octanol with 3.0 mg mL(-1) CNTs as the SLM, with 5V as the driving force, and with pH 7.4 in donor and pH 12 in acceptor solutions. Equilibrium extraction conditions were obtained after 10 min of operation with the whole assembly agitated at 500 rpm. Under the optimized extraction conditions, the proposed EME technique provided good linearity (>0.998), repeatability (RSD=2.7-3.2), low limits of detection (1-3 ng mL(-1)), excellent preconcentration (PF=180-188) and high recoveries (90-94%). In comparison with the conventional EME method, this method showed better results (lower voltage, higher preconcentration factors and higher recoveries). Finally, the developed method was successfully used for the determination of ibuprofen and naproxen in different spiked matrices including plasma, urine, breast milk and wastewater samples.


Assuntos
Técnicas Eletroquímicas/métodos , Membranas Artificiais , Leite Humano/química , Nanotubos de Carbono/química , Preparações Farmacêuticas/análise , Águas Residuárias/química , Técnicas Eletroquímicas/instrumentação , Eletroforese Capilar , Feminino , Humanos , Concentração de Íons de Hidrogênio , Ibuprofeno/análise , Irã (Geográfico) , Limite de Detecção , Modelos Químicos , Naproxeno/análise , Preparações Farmacêuticas/sangue , Reprodutibilidade dos Testes , Poluentes Químicos da Água/análise
7.
Anal Chim Acta ; 767: 75-80, 2013 Mar 12.
Artigo em Inglês | MEDLINE | ID: mdl-23452789

RESUMO

In this work carbon nanotubes assisted electromembrane extraction (CNTs/EME) coupled with capillary electrophoresis (CE) and ultraviolet (UV) detection was developed for the determination of buprenorphine as a model of basic drugs from urine samples. Carbon nanotubes reinforced hollow fiber was used in this research. Here the CNTs serve as a sorbent and provide an additional pathway for solute transport. The presence of CNTs in the hollow fiber wall increased the effective surface area and the overall partition coefficient on the membrane; and lead to an enhancement in the analyte transport. For investigating the influence of the presence of CNTs in the SLM on the extraction efficiency, a comparative study was carried out between EME and CNTs/EME methods. Optimization of the variables affecting these methods was carried out in order to achieve the best extraction efficiency. Optimal extractions were accomplished with NPOE as the SLM, with 200V as the driving force, and with pH 2.0 in the donor and pH 1.0 in the acceptor solutions with the whole assembly agitated at 750rpm after 25min and 15min for EME and CNTs/EME, respectively. Under the optimized conditions, in comparison with the conventional EME method, CNTs/EME provided higher extraction efficiencies in shorter time. This method provided lower limit of detection (1ngmL(-1)), higher preconcentration factor (185) and higher recovery (92). Finally, the applicability of this method was evaluated by the extraction and determination of buprenorphine in patients' urine samples.


Assuntos
Buprenorfina/urina , Técnicas Eletroquímicas , Membranas Artificiais , Nanotubos de Carbono/química , Buprenorfina/química , Eletrodos , Eletroforese Capilar , Humanos , Conformação Molecular , Valores de Referência , Raios Ultravioleta
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