0000000000134778
AUTHOR
R.a. González-fuenzalida
Miniaturized liquid chromatography coupled on-line to in-tube solid-phase microextraction for characterization of metallic nanoparticles using plasmonic measurements. A tutorial.
Abstract This tutorial aims at providing guidelines for analyzing metallic nanoparticles (NPs) and their dispersions by using methods based on miniaturized liquid chromatography with diode array detection (MinLC-DAD) and coupled on-line to in-tube solid-phase microextraction (IT-SPME). Some practical advice and considerations are given for obtaining reliable results. In addition, this work outlines the potential applications that set these methodologies apart from microscopy-related techniques, dynamic light scattering, single particle ICP-MS, capillary electrophoresis, field-flow fractionation and other chromatographic configurations, which are discussed and mainly seek to accomplish size …
In Situ Colorimetric Quantification of Silver Cations in the Presence of Silver Nanoparticles
Silver ions (Ag(+)) can be quantified in situ in the presence of AgNPs by using a colorimetric sensing probe (3,3',5,5'-tetramethylbenzidine). Interestingly, it also enables detection of the Ag(+) adsorbed on the AgNP surface. This is relevant to design new methods to make AgNPs while ensuring the total reduction of Ag(+).
Adsorbent phases with nanomaterials for in-tube solid-phase microextraction coupled on-line to liquid nanochromatography
Following the present trends in miniaturization, a methodology that combines on-line In-Tube Solid-Phase Microextraction (IT-SPME) with Liquid Nanochromatography (nano-LC) and UV-vis diode array detection (DAD) was developed. This coupling was achieved by using two interconnected valves (i.e. conventional and micro-automatic valves) in the system of injection. As for IT-SPME, different materials, containing in some cases nanostructures or nanoparticles and in other cases polymeric adsorbent phases immobilized on capillary columns, were tested in order to improve extraction efficiencies of organic compounds; diclofenac was selected as the target analyte. Additionally, the transfer time of th…
New Tools for Characterizing Metallic Nanoparticles: AgNPs, A Case Study.
Currently, transmission electron microscopy (TEM) is the main technique for estimating the sizes of spherical nanoparticles (NPs) and through them, their concentrations. This paper demonstrates for the first time that C18 reversed-phase capillary liquid chromatography (Cap-LC) coupled to diode array detection (DAD) has the potential to estimate mean concentrations of silver nanoparticles (AgNPs) and thereby determine their average size. Direct injection of the sample without previous extraction or separation steps is carried out. Only a unique standard with a known AgNP size is needed for the calibration. In a first approach, the new method has been tested over silver nanoparticles, produce…
Cleaning sorbents used in matrix solid-phase dispersion with sonication: Application to the estimation of polycyclic aromatic hydrocarbons at ng/g levels in marine sediments
This study shows that ultrasonic assisted extraction is a good practise for removing impurities from sorbents used for matrix-solid phase dispersion (MSPD). A previous washing of the sorbent with an organic solvent or mixture of solvents eliminates part of the interferences, but this treatment is not enough for the quantification of PAHs at ng/g levels. It is demonstrated that the determination of traces of polycyclic aromatic hydrocarbons (PAHs) in solid samples processed by matrix-solid phase dispersion (MSPD) may be severely affected by the presence of sorbent impurities. Different extraction solvents and sonication conditions have been tested, and on the basis of the results obtained a …
Quantitative study of the capture of silver nanoparticles by several kinds of soils
The capacity of different soils to capture silver nanoparticles (AgNPs) by measuring changes of an AgNP intrinsic property such as the plasmon for the first time, was studied. In-tube solid-phase microextraction (IT-SPME) coupled on-line to capillary liquid chromatography (CapLC) with diode array detection (DAD) was employed for measuring the interactions between soil and in-contact AgNP dispersions. Its achieved LOD 9 pM assures quantitative retention measurements and selectivity for soil lixiviation was suitable. Electronic microscopy was employed for corroborating the entrapped Ag into the soils. Capture % of AgNPs was calculated in compost (>99%), mountain (>99%), orchard (15±1%) and ur…
Establishing the occurrence and profile of polycyclic aromatic hydrocarbons in marine sediments: The eastern Mediterranean coast of Spain as a case study.
Sampling, cost-effective analysis, diagnosis of sources of pollution and assessment of potential toxicological effects were included in the case study. Marine sediments collected from 24 points along the eastern Mediterranean coast of Spain (Comunitat Valenciana region) in 2010, 2011, 2012 and 2015 have been analysed for polycyclic aromatic hydrocarbons. Fluoranthene, pyrene, chrysene, benzo[b]fluoranthene and benzo[a]pyrene were the most found. An analysis of the relative abundance of selected PAHs revealed that petrogenic and mixed petrogenic/pyrogenic sources are predominant in the area. The total concentrations of the target compounds ranged from 14.7 to 615.3 ng/g dry weight. The effec…
Microextraction with phases containing nanoparticles.
In this article, the state of the art of microextraction techniques that involve nanoparticles or nanomaterials (NPs) is reviewed, with special emphasis on the applications described in the biomedical field. The uses and advantages of the different types of NPs such as carbon nanotubes (either single- and multi-walled) and other carbon-based materials, metallic NPs, including gold, silver and magnetic NPs, and silica NPs are summarized. The main strategies used to modify the selectivity, extractive capacity and/or the stability of NPs through a chemical reaction are also reviewed. The potential advantages of NPs in different forms of off-line and on-line microextraction are discussed, and …
Evaluation of Superparamagnetic Silica Nanoparticles for Extraction of Triazines in Magnetic in-Tube Solid Phase Microextraction Coupled to Capillary Liquid Chromatography
The use of magnetic nanomaterials for analytical applications has increased in the recent years. In particular, magnetic nanomaterials have shown great potential as adsorbent phase in several extraction procedures due to the significant advantages over the conventional methods. In the present work, the influence of magnetic forces over the extraction efficiency of triazines using superparamagnetic silica nanoparticles (NPs) in magnetic in tube solid phase microextraction (Magnetic-IT-SPME) coupled to CapLC has been evaluated. Atrazine, terbutylazine and simazine has been selected as target analytes. The superparamagnetic silica nanomaterial (SiO2-Fe3O4) deposited onto the surface of a capil…
In Situ Analysis Devices for Estimating the Environmental Footprint in Beverages Industry
Abstract The need to calculate the environmental footprint could mean the integration of sustainability in differentiation strategies for beverages industries. The parameters for estimating the footprint are outlined and discussed. The main negative impacts are related to water pollution, atmospheric pollution, and solid waste. Agro-industrial effluents may contain pesticides, complex oils, alkaline or acidic compounds, and other organic substances. As for atmospheric emissions, particulate material, SO2, NOx, hydrocarbons, and other organic compounds, can be mentioned. The state of art of in situ analysis devices for this purpose is described. The devices are compared through the tool CALI…