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1.
J Sep Sci ; 46(21): e2300323, 2023 Nov.
Artigo em Inglês | MEDLINE | ID: mdl-37691072

RESUMO

This study introduces a reliable and inexpensive magnetic dispersive solid phase extraction to extract imipramine and its primary metabolite (desipramine) from urine samples. To accomplish this aim, Fe3 O4 magnetic nanoparticles were synthesized by sonication, subsequently, polycarbonate was precipitated gradually onto the surface of them to form the adsorbent. Extraction recoveries of 85% and 76%, enrichment factors of 57 and 51, limits of detection of 2.5 and 2.8 µg/L, and limits of quantification of 8.3 and 9.3 µg/L were obtained for imipramine and desipramine under the optimal conditions, respectively. In addition, relative standard deviations for intra- (n = 6) and inter-day (n = 5) precisions at two concentrations (50 and 100 µg/L of each analyte) were less than or equal to 4%. Short extraction time, good repeatability, high enrichment factors, and simplicity are the main advantages of the proposed method.


Assuntos
Imipramina , Nanopartículas de Magnetita , Desipramina , Extração em Fase Sólida , Cromatografia Líquida de Alta Pressão , Fenômenos Magnéticos
2.
Anal Methods ; 12(25): 3268-3276, 2020 07 02.
Artigo em Inglês | MEDLINE | ID: mdl-32930190

RESUMO

Herein, a solid-phase microextraction pencil lead fiber coated with a layer-by-layer graphenized graphite/graphene oxide/polyaniline nanocomposite (GG/GO/PANI) was fabricated by an in situ electrochemical technique for the trace analysis of organophosphorus pesticide residues in packed grape and apple juice and also fresh tomato samples. The effects of various parameters, including the type of desorption solvent, adsorption time, desorption time, pH, salt addition, and stirring rate, on the extraction efficiency of the studied pesticides were investigated and accordingly, these parameters were optimized. The proposed fiber demonstrated desirable linear ranges (0.01-300 µg L-1) with good correlation coefficients (R2 ≥ 0.996) as well as low limits of detection (0.003-0.03 µg L-1) for the studied pesticides. The relative standard deviations (n = 5) for the extraction of 50 µg L-1 of each analyte were less than 7 and 11.5% for inter and intra-day precisions, respectively. This fast, facile, and repeatable electrochemical fabrication method produced a porous and homogeneous coating. The proposed fiber demonstrated good extraction efficiency, high stability, and long life-time despite being low cost. The successful application of the proposed fiber for the trace determination of pesticides in complex food matrices was proven by the satisfactory relative recoveries of 80.7-116.5%.


Assuntos
Grafite , Nanocompostos , Resíduos de Praguicidas , Compostos de Anilina , Sucos de Frutas e Vegetais , Resíduos de Praguicidas/análise , Verduras
3.
J Sep Sci ; 42(7): 1364-1373, 2019 Apr.
Artigo em Inglês | MEDLINE | ID: mdl-30681294

RESUMO

A layer by layer graphenized graphite/polyaniline coating was fabricated on commercial pencil lead substrate by an in situ facile, fast and efficient electrochemical procedure. The electrodeposited polyaniline film on surface-confined graphene structure can integrate the advantages of the both layers and was used for solid-phase microextraction. Effective experimental parameters in electrochemical production of graphene nanosheets and electropolymerization of aniline were optimized. The prepared fiber was used for extraction and determination of four polycyclic aromatic hydrocarbons: phenanthrene, anthracene, fluoranthene and pyrene in aqueous samples by high performance liquid chromatography. The fiber coating was characterized by Fourier transform infrared spectroscopy, X-ray diffraction and scanning electron microscopy. Under the optimized conditions, the coating provided good linear ranges (0.10-25 µg/L for phenanthrene, 0.05-12.5 µg/L for anthracene, 0.825-99 µg/L for fluoranthene and 0.625-75 µg/L for pyrene (R2  = 0.999)) and limits of detection, 0.016 to 0.275 µg/L. The produced coating has several attractive features such as high stability, low cost and long operation time.

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