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1.
Front Chem ; 10: 1045552, 2022.
Artículo en Inglés | MEDLINE | ID: mdl-36688049

RESUMEN

In this project, we have synthesized and used a molecular imprinted polymer (MIP) for adsorption of oxycodone residue from the biological samples. Indeed, this study aims to develop a suitable method for determination of oxycodone drug residue in the human plasma using the common analysis methods. Therefore, the MIP was used for the solid phase extraction (MIP-SPE) approach in order to collect the oxycodone opioid and to concentrate it in the blood plasma samples. The extraction parameters such as adsorption time, pH, and the amount of sorbent in blood plasma were optimized and the capacity of loading amount (LA) for adsorbing it was determined. Moreover, a high performance liquid chromatography (HPLC)-UV detector method was validated and used for analyzing of the mentioned opioid extracted from plasma. The results showed that the limit of detection (LOD), and the limit of quantization (LOQ) for the developed MIP-SPE method were 1.24 ppb, and 3.76 ppb, respectively. Moreover, both of the MIP-, and non-imprinted polymers (NIP)-drug complexes were designed and were then optimized by the density functional theory (DFT) method. The results showed that the theoretical calculations supported the experimental data, confirming the favorability of adsorption of the drug by MIP compared to NIP.

2.
Mikrochim Acta ; 188(3): 92, 2021 02 19.
Artículo en Inglés | MEDLINE | ID: mdl-33608774

RESUMEN

A screen-printed electrode (SPE) is described modified with sulfur-tin oxide nanoparticles (S@SnO2NP) for the determination of entacapone (ENT) in the presence of other medicines against Parkinson's disease (PD). The S@SnO2NP was synthesized through the hydrothermal method and used in the modification of the SPE. The smart utilization of the S@SnO2NP and the SPE provided excellent properties such as high surface area and current density amplification by embedding an efficient sensing interface for highly selective electrochemical measurement. Under optimized experimental conditions, the anodic peak current related to the ENT oxidation onto the sensor surface at 0.46 V presented a linear response towards different ENT concentration sin the range 100 nM to 75 µM. The limit of detection (LOD) and electrochemical sensitivity were estimated to be 0.010 µM and 2.27 µA·µM-1·cm-2, respectively. The applicability of the sensor was evaluated during ENT determination in the presence of other conventional medicines againts, including levodopa (LD), carbidopa (CD), and pramipexole (PPX). The results of the analysis of human urine and pharmaceutical formulation as real samples using the developed sensor were in good agreement withre sults of high-performance liquid chromatography (HPLC) as a standard method. These findings demonstrated that the strategy based on the SPE is a cost-effective platform creating a promising candidate for practical determination of ENT in routine clinical testing.Graphical abstract.


Asunto(s)
Antiparkinsonianos/orina , Catecoles/orina , Técnicas Electroquímicas/métodos , Nanopartículas del Metal/química , Nitrilos/orina , Antiparkinsonianos/química , Catecoles/química , Técnicas Electroquímicas/instrumentación , Electrodos , Humanos , Límite de Detección , Nitrilos/química , Oxidación-Reducción , Azufre/química , Comprimidos/análisis , Compuestos de Estaño/química
3.
Anal Chim Acta ; 683(2): 206-11, 2011 Jan 10.
Artículo en Inglés | MEDLINE | ID: mdl-21167972

RESUMEN

This work is a first study on extraction efficiency and thermal stability of nano-structured self-doped polyaniline (SPAN) as a coating of solid-phase microextraction (SPME) fibers. SPAN-based fibers were prepared using electrochemical deposition on platinum wires. The particle sizes of prepared nano-structure were in the range of 50-100 nm. Extraction properties of the fiber to 1,4-dioxane were examined using headspace solid-phase microextraction (HS-SPME) coupled to gas chromatography-flame ionization detection (GC-FID). The results have proved higher thermal stability of the proposed fiber compared to common PANI fiber. The SPAN coating was proved to be very stable at relatively high temperatures (up to 350 °C) with high extraction capacity and long lifespan (more than 50 times). Therefore, it can be a good substitute of polyaniline (PANI) as a SPME coating. The extraction procedure was optimized by selecting the appropriate extraction parameters including extraction time, extraction temperature, salt concentration, stirring rate and headspace volume. Calibration graph was linear in the concentration range of 1-100 ng mL(-1) (R(2)>0.993) with detection limit of 0.1 ng mL(-1). Single fiber and fiber-to-fiber repeatability were lower than 6.0% and 10.4%, respectively. Different water samples were analyzed as real samples and good recoveries (98-120%) were obtained.

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