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1.
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
2.
Food Chem ; 403: 134273, 2023 Mar 01.
Artigo em Inglês | MEDLINE | ID: mdl-36174345

RESUMO

Herein, an ultrasound-assisted dispersive solid phase microextraction (UA-DSPME) approach has been described for trace level analysis of triazole fungicides in real samples. For this purpose, a new nanosorbent was prepared through modification of carboxymethylcellulose biopolymer with zinc-based metal-organic framework and graphene oxide, and fully characterized. Then, the effect of extraction parameters on extraction efficiency was optimized for the microextraction process. Finally, desorbed triazole fungicides with ethanol were determined using gas chromatography equipped with flame ionization detector. This technique provided good linearity (R2 > 0.99), low detection limits (0.3-1.5 ng mL-1), high preconcentration factors (419-426), good relative recoveries (91.6-102 %), and high repeatability (RSD < 4.1 %) at optimized conditions (amount of sorbent: 15 mg; pH of solution: 7.0; and extraction time; 4 min). Ultimately, this approach was applied to determine triazole fungicides in different water and food samples.


Assuntos
Fungicidas Industriais , Microextração em Fase Líquida , Nanocompostos , Microextração em Fase Sólida/métodos , Fungicidas Industriais/análise , Verduras/química , Triazóis/análise , Frutas/química , Água/análise , Celulose/análise , Ultrassom , Nanocompostos/análise , Microextração em Fase Líquida/métodos , Extração em Fase Sólida , Limite de Detecção
3.
Anal Methods ; 13(30): 3394-3401, 2021 08 14.
Artigo em Inglês | MEDLINE | ID: mdl-34236068

RESUMO

In this paper, a novel solid phase microextraction fiber based on Co3O4 quantum dot incorporated polyacrylamide-co-ethylene glycol dimethacrylate followed by corona discharge ion mobility spectrometry is presented for the trace determination of organophosphorus pesticides in environmental water samples. Ion mobility spectrometry is a comparatively inexpensive, well-known, robust, and easy to operate analytical instrument. This combination would provide a low-cost, fast, selective, and sensitive quantitative system for detection of organophosphorus pesticides. In order to obtain the best extraction efficiency, the optimization of parameters affecting this method was carried out. After optimization, a solution pH of 7.0, extraction temperature of 60 °C, adsorption temperature of 260 °C, extraction time of 30 min, stirring speed of 750 rpm, and ionic strength of 10% w/w were obtained. Consequently, the presented method showed low limits of detection (0.3-0.6 ng mL-1), excellent enrichment factors (PF = 221-263), good linearity (R2 > 0.995), and repeatabilities (intra-day: 3.4 to 4.8%) and (inter-day: 4.7 to 6.1%). The reproducibility (RSD% of fiber to fiber) was also investigated by analyzing three as-prepared fibers under the same conditions and was found to be less than 7.6%. Finally, the developed fiber was used for determination of organophosphorus pesticides in the field samples.


Assuntos
Praguicidas , Pontos Quânticos , Resinas Acrílicas , Metacrilatos , Compostos Organofosforados , Praguicidas/análise , Reprodutibilidade dos Testes , Microextração em Fase Sólida , Água
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