Search results for "SOLVENT"

Extraction and analysis of ochratoxin A in bread using pressurised liquid extraction and liquid chromatography.

2005

A pressurised liquid extraction (PLE) method for the analysis of ochratoxin A (OTA) in bread samples is given. Parameters such as solvent, temperature, pressure and time were investigated thoroughly. The optimized PLE conditions were: methanol as extraction solvent, 80 degrees C, 2000 psi and a 5-min cycle. OTA was determined by liquid chromatography coupled with fluorescence detection and confirmed by methyl ester derivatization. Under these conditions OTA recovery is 92.3% with a RSD of 5%. Limits of detection and quantification were 0.02 and 0.06 microg/kg, respectively. The proposed method was applied to 20 bread samples, finding two positive samples with OTA levels below the maximum pe…

Determinación de residuos de paraquat en lechuga y repollo cultivados en Lepaterique mediante HPLC-DAD

2018

La determinación de residuos del herbicida paraquat en lechuga (Lactuca sativa) y repollo (Brassica oleracea) producidos en la comunidad de La Brea, Lepaterique y comercializados en la ciudad de Tegucigalpa fue llevada a cabo en los meses de octubre y noviembre de 2017, mediante la aplicación de cromatografía líquida de elevada resolución con detector de arreglo de diodos (HPLC-DAD) en menos de 6 minutos, con un mecanismo de separación de fase reversa empleando una columna superficialmente porosa C18 y una mezcla de ácido orto fosfórico al 0.1 M (pH 3,0) con acetonitrilo en proporción de 3:1 como fase móvil. El método se basa en la extracción con baño ultrasónico utilizando agua como solven…

Selective solid-phase extraction of organophosphorus pesticides and their oxon-derivatives from water samples using molecularly imprinted polymer fol…

2020

Abstract A molecularly imprinted polymer was synthesized and characterized to be used as solid-phase extraction sorbent for simultaneous chlorpyrifos and diazinon and their oxon derivatives. Several imprinted polymers were prepared and evaluated in a retention study of these analytes compared with a non-printed polymer. Several parameters affecting the extraction of imprinted polymer such as washing solvent, composition and volume of the eluting solvent and sample volume, were also investigated. Under the optimum conditions, the developed method provided satisfactory limits of detection ranging between 0.07 µg L−1 to 0.12 µg L−1 and the material showed an excellent reusability (> 50 reuses)…

Determination of volatile organic compounds in contaminated air using semipermeable membrane devices

2009

Abstract Semipermeable membrane devices (SPMDs) were evaluated as passive samplers for the determination of 26 volatile organic compounds (VOCs) in contaminated air of occupational environments. A direct methodology based on the use of head-space-gas chromatography–mass spectrometry (HS-GC–MS) was developed for VOCs determinations in SPMDs, without any sample pre-treatment and avoiding the use of solvents. A desorption temperature of 150 °C for 10 min was sufficient for a sensitive VOCs determination providing limits of detection in the range of 15 ng SPMD−1 for 21 of 26 studied compounds. Linear and equilibrium uptake models were established for each VOC from compound isotherms. Highly vol…

Pulsed EPR determination of water accessibility to spin-labeled amino acid residues in LHCIIb.

2009

Membrane proteins reside in a structured environment in which some of their residues are accessible to water, some are in contact with alkyl chains of lipid molecules, and some are buried in the protein. Water accessibility of residues may change during folding or function-related structural dynamics. Several techniques based on the combination of pulsed electron paramagnetic resonance (EPR) with site-directed spin labeling can be used to quantify such water accessibility. Accessibility parameters for different residues in major plant light-harvesting complex IIb are determined by electron spin echo envelope modulation spectroscopy in the presence of deuterated water, deuterium contrast in …

Separation of plasma membrane proteins of cultured human fibroblasts by affinity chromatography on bonded microparticulate silicas.

1984

Abstract Adsorbents for high-performance affinity chromatography were prepared by bonding proteins and reactive Procion triazine dyes to 3-isothiocyanatopropyl- and 3-aminopropylsilicas. The materials prepared were used successfully in the separation of hydrophobic plasma membrane proteins of cultured human fibroblasts. The data obtained show that the reaction of 3-isothiocyanatopropyltriethoxysilane (ITCPS) with the surface hydroxyl groups of silica yields a new and convenient route to preparing an “activated carrier” that is capable of coupling with potential affinity ligands containing amino functional groups. The reaction and bonding procedures of 3-isothiocyanatopropyltriethoxysilane a…

Efficient Nucleophilic Degradation of an Organophosphorus Pesticide “Diazinon” Mediated by Green Solvents and Microwave Heating

2019

An efficient strategy for the degradation of organophosphate pesticide Diazinon was investigated. In this work, ionic liquids, bio-based solvents, and two conventional organic solvents were used as reaction media. Kinetics studies by means of half-life (t1/2,h) were followed by 31P NMR and the products analyzed by GC-MS, HPLC-MS and NMR techniques. These results have shown that t1/2 values in ionic liquids were the lowest and also they were able to activate two electrophilic centers in Diazinon, whilst degradation in bio-based solvents occurred slowly by only an aromatic pathway. In addition, a study to estimate the influence of green activation techniques was carried out by using Ultrasoun…

Simultaneous clean up of fish fat containing low levels of residues and separation of PCB from chlorinated pesticides by thin-layer chromatography

1974

Polar Diels–Alder reactions using electrophilic nitrobenzothiophenes. A combined experimental and DFT study

2015

Abstract The reactions between 2- and 3-nitrobenzothiophenes with three dienes of different nucleophilicity, 1-methoxy-3-trimethylsilyloxy-1,3-butadiene, 1-trimethylsilyloxy-1,3-butadiene and isoprene developed in anhydrous benzene and alternative under microwave irradiation with molecular solvents or in free solvent conditions, respectively, for produce dibenzothiophenes permit to conclude that both nitroheterocycles act as electrophile with the cited dienes. In the cases of the dienes 1-methoxy-3-trimethylsilyloxy-1,3-butadiene and 1-trimethylsilyloxy-1,3-butadiene which posses major nucleophilicity the observed product is the normal cycloaddition one. However when the diene is isoprene t…

Liquid Structure of Trihexyltetradecylphosphonium Chloride at Ambient Temperature: An X-ray Scattering and Simulation Study

2009

We report on an experimental and simulation study done on a representative room temperature ionic liquid, namely tetradecyltrihexylphosphonium chloride, at ambient conditions. The study was conducted using small and wide angle X-ray scattering and molecular dynamics simulations. Both approaches converge in indicating that this material is characterized by the existence of strong P-Cl interactions (with characteristic distances between 3.5 and 5.0 Å) and by the occurrence of nanoscale segregation, despite the symmetric nature of the cation and similarly to other room temperature ionic liquids. A good agreement is found between the structure factor and pair correlation functions obtained from…