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1.
Forensic Sci Med Pathol ; 11(4): 497-503, 2015 Dec.
Artigo em Inglês | MEDLINE | ID: mdl-26318597

RESUMO

In this paper we report a novel, sensitive, and rapid method of magnetic solid phase extraction based on surface modified magnetic nanoparticles as a novel nano sorbent for HPLC determination of morphine with diode array detection in human hair samples. Factors affecting the extraction efficiency of the proposed method, including the sample pH, quantity of magnetic nanoparticles, sample volume, desorption solvent type and its volume, and extraction time were investigated and optimized. Under the optimized experimental conditions, a good linearity was observed in the range of 1-800 µgL(-1) for the morphine, with a correlation coefficient (R (2)) of 0.990. The pre-concentration factor of 208.69 was achieved in this method. The detection limit of the method was 0.1 µgL(-1) based on S/N = 3 and good reproducibility with a relative standard deviations lower than (n = 5) 2.59 %. The proposed method has been successfully applied to the analysis of trace amounts of morphine in human hair samples with satisfactory results. This method can be applied in medical toxicology research and forensic medical centers.


Assuntos
Cabelo/química , Nanopartículas de Magnetita/química , Morfina/análise , Entorpecentes/análise , Silanos/química , Adsorção , Cromatografia Líquida de Alta Pressão/métodos , Toxicologia Forense , Humanos , Concentração de Íons de Hidrogênio , Limite de Detecção , Masculino , Microscopia Eletrônica de Transmissão , Reprodutibilidade dos Testes , Extração em Fase Sólida
2.
Arch Environ Contam Toxicol ; 68(2): 412-20, 2015 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-25367213

RESUMO

In the present study, a novel adsorbent, Fe3O4 magnetic nanoparticles (MNPs) functionalized by silane-coupling agent KH-570, was successfully synthesized. The prepared MNPs were characterized by Fourier-transform infrared spectroscopy and transmission electron microscopy. It was applied as functionalized magnetic nano-adsorbent for magnetic solid-phase extraction of trace levels of venlafaxine using gas chromatography with flame ionization detector. This method was developed and optimized for use in analysis of venlafaxine in human hair and aqueous environmental samples. The main factors influencing the extraction efficiency including pH of sample, amount of the MNPs, adsorption time, volume of sample, and desorption conditions such as volume of solvent and desorption time were studied and optimized. Under the optimized experimental conditions, good linearity was observed in the range of 1-1,000 µg L(-1) for aqueous environmental samples with correlation coefficients (R (2)) 0.996. The limits of detection and quantification were 0.1 and 0.5 µg L(-1), respectively. Good reproducibility with the relative standard deviations (n = 5) 3.21 % was obtained. The developed method was successfully applied to the extraction of venlafaxine from spiked human hair, river water, and surface water samples and the relative recoveries of 89.36, 93.43, and 94.99 % were obtained, respectively. The results indicated that Fe3O4/KH-570 MNPs have a satisfying extraction efficiency and can be served as a sensitive, inexpensive, and reliable method for analysis of antidepressant drugs such as venlafaxine in biological and aqueous environmental samples.


Assuntos
Antidepressivos de Segunda Geração/análise , Cicloexanóis/análise , Cabelo/química , Metacrilatos/química , Silanos/química , Poluentes Químicos da Água/análise , Cromatografia Gasosa , Ionização de Chama , Humanos , Reprodutibilidade dos Testes , Extração em Fase Sólida , Cloridrato de Venlafaxina
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