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1.
Environ Sci Pollut Res Int ; 29(1): 498-508, 2022 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-34333743

RESUMO

The present study aimed to investigate the persistence and existence of chemical warfare agents (CWAs) and related dissipation products in the environment of Sardasht area, Iran. Three types of environmental samples including water, soil, and native local plant materials were collected and analyzed. Gas chromatography-mass spectrometry in the electron impact ionization mode has been developed for the separation, screening, identification, and qualification of chemicals after the sample preparation methods. The initial results revealed that no trace of related compounds or CWAs was detected in the soil and water samples. However, trace amounts of some degradation products of blistering agents like mustard gas (HD) and lewisite were found in a tree wood from a house subjected to chemical attack as well as in barley samples (a mixture of leaves and root) collected from an agricultural field in the area indicating chronic low exposure to the environment and people. In order to validate the applied extraction procedures, ethylene glycol was spiked to some of the samples including groundwater, surface soil, grape, and alfalfa plants. All the recoveries were in the range of 83.6-107.4% with the relative standard deviations varying from 4.9% to 12.4% (n = 3) successfully.


Assuntos
Substâncias para a Guerra Química , Gás de Mostarda , Substâncias para a Guerra Química/análise , Cromatografia Gasosa-Espectrometria de Massas , Humanos , Irã (Geográfico) , Gás de Mostarda/análise , Solo
2.
Spectrochim Acta A Mol Biomol Spectrosc ; 204: 409-415, 2018 Nov 05.
Artigo em Inglês | MEDLINE | ID: mdl-29966893

RESUMO

Herein, the application of Graphene oxide-polyaniline (GO/PANI) in one of newly hollow fiber based microextraction techniques so called (HF-S/LPME) was investigated successfully. Graphene oxide-polyaniline (GO/PANI) nanocomposite was generated via an amidation reaction in the presence of N, N'-dicyclohexylcarbodiimide (DCC), N-hydroxysuccinimide (NHS) and GO as starting material. The solid sorbent dispersed in dihexyl ether was immersed and injected into the lumen of hollow fiber. The results indicated that GO/PANI had a higher adsorption efficiency for the Ivermectin in comparison with GO and GO-ethylen diamine (GO/EDA). A Taguchi experimental design with an OAD16 (45) matrix was employed to optimize the affecting parameters such as pH, stirring rate, extraction time, salt addition and the volume of donor phase. Under the optimized extraction conditions, the method showed a good linear dynamic range (0.1-5000.0 ppb) with a lower limit of detection (0.03 ppb) and excellent preconcentration factor (PF = 219.88) respectively.


Assuntos
Compostos de Anilina/química , Resíduos de Drogas/análise , Grafite/química , Ivermectina/isolamento & purificação , Nanocompostos/química , Poluentes Químicos da Água/isolamento & purificação , Adsorção , Animais , Cromatografia Líquida de Alta Pressão , Resíduos de Drogas/química , Resíduos de Drogas/isolamento & purificação , Ivermectina/análise , Ivermectina/química , Limite de Detecção , Modelos Lineares , Microextração em Fase Líquida , Leite/química , Óxidos/química , Reprodutibilidade dos Testes , Poluentes Químicos da Água/análise , Poluentes Químicos da Água/química
3.
J Chromatogr A ; 1420: 46-53, 2015 Nov 13.
Artigo em Inglês | MEDLINE | ID: mdl-26477522

RESUMO

In this paper, TiO2 nanowires and TiO2 nanoparticles have been successfully anchored on graphene oxide (GO) nanosheets by a facile one-step hydrothermal method. The synthesized TiO2 NWs/RGO and TiO2 NPs/RGO nanocomposites were characterized by Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM) and X-ray diffraction (XRD) analysis. After comparatively studying of the as-made nanocomposites, TiO2 NWs/RGO nanocomposite showed the best adsorbing performance and applied as an attractive efficient sorbent reinforced with microporous hollow fiber membrane through the sol-gel technology. In the following, the selected nanocomposite was utilized for simultaneous preconcentration and determination of clotrimazole and tylosin using high performance liquid chromatography (HPLC)-UV detection, respectively. In order to optimize the extraction conditions through affecting parameters (pH, stirring rate, salt addition, extraction time and volume of donor phase), response surface methodology (RSM) was employed as a powerful statistical technique. Under the optimal conditions, the limit of detection (S/N=3) of proposed HFSPME method, was 0.67 µg L(-1) for clotrimazole and 0.91 µg L(-1) for tylosin with good linear ranges of 1.7-8000.0 µg L(-1) and 4.0-6000.0 µg L(-1). The inter-day and intra-day relative standard deviations (RSD%) at 100 µg L(-1) concentration level were in the ranges of 2.10-3.58% for clotrimazole and 3.45-7.80% for tylosin (n=5), respectively. The proposed microextraction device was extended for determination of ultra trace amounts of target analytes in milk and urine samples with satisfactory results.


Assuntos
Clotrimazol/isolamento & purificação , Grafite/química , Leite/química , Nanocompostos/química , Nanofibras/química , Titânio/química , Tilosina/isolamento & purificação , Animais , Bovinos , Cromatografia Líquida de Alta Pressão/métodos , Clotrimazol/análise , Membranas Artificiais , Microscopia Eletrônica de Varredura , Tilosina/análise , Difração de Raios X
4.
J Sep Sci ; 37(15): 2025-31, 2014 Aug.
Artigo em Inglês | MEDLINE | ID: mdl-24890459

RESUMO

The aim of this study was to introduce a novel, simple, and highly sensitive preparation method for determination of tylosin in different milk samples. In the so-called functionalized TiO2 hollow fiber solid/liquid-phase microextraction method, the acceptor phase is functionalized TiO2 nanoparticles that are dispersed in the organic solvent and held in the pores and lumen of a porous polypropylene hollow fiber membrane. An effective functionalization of TiO2 nanoparticles has been done in the presence of aqueous H2 O2 and a mild acidic ambient under UV irradiation. This novel extraction method showed excellent extraction efficiency and a high enrichment factor (540.2) in comparison with conventional hollow fiber liquid-phase microextraction. All the experiments were monitored at λmax = 284 nm using a simple double beam UV-visible spectrophotometer. A Taguchi orthogonal array experimental design with an OA16 (4(5) ) matrix was employed to optimize the factors affecting the efficiency of hollow fiber solid/liquid-phase microextraction such as pH, stirring rate, salt addition, extraction time, and the volume of donor phase. This developed method was successfully applied for the separation and determination of tylosin in milk samples with a linear concentration range of 0.51-7000 µg/L (r(2) = 0.991) and 0.21 µg/L as the limit of detection.


Assuntos
Antibacterianos/isolamento & purificação , Contaminação de Alimentos/análise , Microextração em Fase Líquida/métodos , Leite/química , Tilosina/isolamento & purificação , Animais , Antibacterianos/análise , Bovinos , Microextração em Fase Líquida/instrumentação , Nanopartículas/química , Espectrofotometria Ultravioleta , Titânio/química , Tilosina/análise
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