Search results for "010401 analytical chemistry"
showing 10 items of 1284 documents
Determination of N-nitrosodiethanolamine in cosmetic products by reversed-phase dispersive liquid-liquid microextraction followed by liquid chromatog…
2016
A new analytical method for the determination of N-nitrosodiethanolamine (NDELA), a very harmful compound not allowed in cosmetic products, is presented. The method is based on a new approach of dispersive liquid-liquid microextraction (DLLME) useful for extraction of highly polar compounds, called reversed-phase DLLME (RP-DLLME), followed by liquid chromatography-ultraviolet/visible (LC-UV/Vis) determination. The variables involved in the RP-DLLME process were studied to provide the best enrichment factors. Under the optimized conditions, a mixture of 750µL of acetone (disperser solvent) and 125µL of water (extraction solvent) was rapidly injected into 5mL of toluene sample solution. The e…
Fast extraction methodologies for the determination of toxic arsenic in meat
2017
Summary A nonchromatographic analytical procedure has been developed for the determination of arsenic in meat samples including the major toxic arsenic species arsenite, arsenate, monomethylarsonic acid (MMA) and dimetylarsinic acid (DMA). The method is based on the extraction of arsenic species in mild conditions, selective trivalent hydride formation and final determination by hydride generation atomic fluorescence spectroscopy (HG-AFS). Different extractant agents and two different procedures, microwave-assisted extraction (MAE) and ultrasound assisted extraction at room temperature, were evaluated for As species extraction. The method provided a limit of detection of 0.013 ng mL−1 and a…
Development of a molecularly imprinted monolithic polymer disk for agitation-extraction of ecgonine methyl ester from environmental water
2019
Abstract In this study, a new extraction approach based on rotating molecularly imprinted polymer (MIP) disks was developed. The preparation procedure of MIP-disk is simple. Firstly, in order to immobilize MIP onto the surface of polytetrafluoroethylene (PTFE) disk, previous modification and vinylization steps of this fluoropolymer were conducted. Then, MIP synthesis was done by in situ polymerization. The resulting MIP was characterized by Fourier-transform infrared spectroscopy and scanning electron microscopy. Afterwards, two ring magnets were placed in the sides of the MIP-disk to integrate the stirring and preconcentration of sample in just one step. To demonstrate the feasibility of t…
Uptake and translocation monitoring of imidacloprid to chili and tomato plants by molecularly imprinting extraction - ion mobility spectrometry
2019
Abstract The degradation of imidacloprid in soil and its uptake and translocation to chili and tomato plants was evaluated, as a proof of concept, of the possibilities of the combination of molecularly imprinted polymers (MIPs) and ion mobility spectrometry (IMS) for a fast and sensitive bioprocesses monitoring tool. To do it, a method based on the selective extraction of imidacloprid from soil and plant materials was developed. In the selected conditions, the MIP-IMS procedure provided a recovery of imidacloprid in soil and plant samples from 102 to 114%, for spiked concentration levels from 0.2 to 2.0 μg g−1. Precision of the methodology, expressed as the relative standard deviation (RSD)…
Direct analysis in real-time high-resolution mass spectrometry as a valuable tool for polyphenols profiling in olive oil
2018
A fast and reliable method to characterize the polyphenolic compound profiles in extra virgin olive oil (EVOO) has been developed using direct analysis in real time (DART) and linear ion-trap Orbitrap mass spectrometry (LTQ-Orbitrap-MS). Hydroalcoholic extraction increased speed and reduced matrix effects, and DART-MS/MS ensured accurate analysis. Characterization of polyphenol fingerprinting in EVOO samples takes 2 min. This method exhibited proper linearity (R2 ≥ 0.99) in the range of 5–2500 μg g−1, limit of detection (LOD) of 1.5 μg g−1 (signal-to noise S/N = 3), and limits of quantitation (LOQs) of 5 μg g−1 (S/N = 10) for resveratrol (a polyphenol not detected in olive oil). Six spiked …
Introducing a new and rapid microextraction approach based on magnetic ionic liquids: Stir bar dispersive liquid microextraction
2017
With the aim of contributing to the development and improvement of microextraction techniques, a novel approach combining the principles and advantages of stir bar sorptive extraction (SBSE) and dispersive liquid-liquid microextraction (DLLME) is presented. This new approach, termed stir bar dispersive liquid microextraction (SBDLME), involves the addition of a magnetic ionic liquid (MIL) and a neodymium-core magnetic stir bar into the sample allowing the MIL coat the stir bar due to physical forces (i.e., magnetism). As long as the stirring rate is maintained at low speed, the MIL resists rotational (centrifugal) forces and remains on the stir bar surface in a manner closely resembling SBS…
Trace determination of volatile polycyclic aromatic hydrocarbons in natural waters by magnetic ionic liquid-based stir bar dispersive liquid microext…
2017
In this work, a novel hybrid approach called stir bar dispersive liquid microextraction (SBDLME) that combines the advantages of stir bar sorptive extraction (SBSE) and dispersive liquid-liquid microextraction (DLLME) has been employed for the accurate and sensitive determination of ten polycyclic aromatic hydrocarbons (PAHs) in natural water samples. The extraction is carried out using a neodymium stir bar magnetically coated with a magnetic ionic liquid (MIL) as extraction device, in such a way that the MIL is dispersed into the solution at high stirring rates. Once the stirring is ceased, the MIL is magnetically retrieved onto the stir bar, and subsequently subjected to thermal desorptio…
Calibration of LA-ICP-MS via standard addition using dried picoliter droplets
2020
A novel microanalytical calibration approach for quantitative spatially resolved analysis of thin layered materials with laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) is presented. This method relies on standard addition via the generation of dried pL-droplet residues. Therefore, a drop on demand dosing device based on a modified commercial ink cartridge and a dosing interface, both accessible via a self-constructed microcontroller, were developed. This dosing device enables the precise deposition of pL-droplets onto solid samples for the generation of residues with dimensions in the low μm-range. The LA-ICP-MS analysis of such residues allows calibration over at l…
Non-chromatographic speciation of mercury in mushrooms
2016
A fast, sensitive and cheap procedure has been developed for the determination of inorganic mercury (i-Hg) and organic mercury (o-Hg) in mushroom samples. The procedure is based on the use of cold vapour atomic fluorescence spectrometry (CV-AFS). The method involves the extraction of total mercury (t-Hg) with diluted HCl, followed by measurements of the corresponding Hg vapour under two different conditions: (i) directly to determine i-Hg, and (ii) after oxidation with a mixture KBr/KBrO3 to determine t-Hg. o-Hg was estimated from the difference between t-Hg and i-Hg. Previous studies were focused on the assessment of different reagents for mercury extraction and breakdown of organomercury …
Determination of N -nitrosamines in cosmetic products by vortex-assisted reversed-phase dispersive liquid-liquid microextraction and liquid chromatog…
2018
A new analytical method for the simultaneous determination of trace levels of seven prohibited N-nitrosamines (N-nitrosodimethylamine, N-nitrosoethylmethylamine, N-nitrosopyrrolidine, N-nitrosodiethylamine, N-nitrosopiperidine, N-nitrosomorpholine, and N-nitrosodiethanolamine) in cosmetic products has been developed. The method is based on vortex-assisted reversed-phase dispersive liquid-liquid microextraction, which allows the extraction of highly polar compounds, followed by liquid chromatography with mass spectrometry. The variables involved in the extraction process were studied to obtain the highest enrichment factor. Under the selected conditions, 75 μL of water as extraction solvent …