Search results for "Sample preparation"
showing 10 items of 343 documents
Determination of benzomercaptans in environmental complex samples by combining zeolitic imidazolate framework-8-based solid-phase extraction and high…
2020
[EN] In this work, the synthesis of zeolitic imidazolate framework-8 (ZIF-8) crystals and their subsequent application as effective sorbents for extraction and preconcentration of several benzomercaptans from environmental complex samples is described. These materials were prepared by solvothermal approach varying the concentration of n-butylamine modulator to modify the surface of the metal-organic framework. The resulting materials were characterized by scanning and transmission electron microscopy, powder X-ray diffraction and Fourier transform infrared spectroscopy. The ZIF-8 material that gave the best features was selected as extractive phase and the influence of various parameters (s…
Application of solid-phase microextraction for determining phenylurea herbicides and their homologous anilines from vegetables.
2004
Abstract Residues of metobromuron, monolinuron and linuron herbicides and their aniline homologous were analyzed in carrots, onions and potatoes by solid-phase microextraction (SPME) performed with a polyacrylate fiber. A juice was obtained from food samples that were further diluted, and an aliquot was extracted after sodium chloride (14%) addition and pH control. At pH 4 only the phenylureas were extracted. A new extraction at pH 11 allowed the extraction of phenylureas plus homologous aniline metabolites. Determination was carried out by gas chromatography with nitrogen–phosporus detection (NPD) the identity of the determined compounds was studied by gas chromatography–mass spectrometry.…
A statistical design of experiments for optimizing the MALDI-TOF-MS sample preparation of polymers. An application in the assessment of the thermo-me…
2011
[EN] The sample preparation procedure for MALDI-TOF MS of polymers is addressed in this study by the application of a statistical Design of Experiments (DoE). Industrial poly (ethylene terephthalate) (PET) was chosen as model polymer. Different experimental settings (levels) for matrixes, analyte/matrix proportions and concentrations of cationization agent were considered. The quality parameters used for the analysis were signal-to-noise ratio and resolution. A closer inspection of the statistical results provided the study not only with the best combination of factors for the MALDI sample preparation, but also with a better understanding of the influence of the different factors, individua…
Assessing the MALDI-TOF MS sample preparation procedure to analyze the influence of thermo-oxidative ageing and thermo-mechanical degradation on poly…
2011
[EN] Multiple processing by means of successive injection cycles was used to simulate the thermo-mechanical degradation effects on the oligomeric distribution of PLA under mechanical recycling. Likewise, an accelerated thermal ageing over PLA glass transition was performed in order to simulate its service life. MALDI-TOF MS was used for the analysis and the sample preparation procedure was assessed by means of a statistical Design of Experiments (DoE). The quality effects in use for the analysis were signal-to-noise ratio and Resolution. Different matrixes, analyte/matrix proportions and the use of NaTFA as cationization agent were considered. A deep inspection of the statistical results pr…
On-line sample treatment and FT-IR determination of doxylamine succinate in pharmaceuticals
2005
Abstract A low solvent consumption method for Fourier transform infrared spectroscopy (FT-IR) determination of doxylamine succinate in pharmaceuticals has been developed. The analyte was continuous and selectively extracted with a 13% (v/v) ethanol:chloroform solvent mixture, recirculating the solvent through the sample and monitoring the process by FT-IR. Doxylamine succinate was determined by on-line standard addition measuring the peak area in the regions 1730–1710 and 1485–1462 cm −1 corrected with a two-point baseline established between 2000 and 1800 cm −1 . This new method implies low volumes of chloroformic solvent mixture, only 2.6 mL per sample, in front of classical batch FT-IR m…
Dispersive solid-phase extraction based on oleic acid-coated magnetic nanoparticles followed by gas chromatography-mass spectrometry for UV-filter de…
2011
Abstract A sensitive analytical method to concentrate and determine extensively used UV filters in cosmetic products at (ultra)trace levels in water samples is presented. The method is based on a sample treatment using dispersive solid-phase extraction (dSPE) with laboratory-made chemisorbed oleic acid-coated cobalt ferrite (CoFe 2 O 4 @oleic acid) magnetic nanoparticles (MNPs) as optimized sorbent for the target analytes. The variables involved in dSPE were studied and optimized in terms of sensitivity, and the optimum conditions were: mass of sorbent, 100 mg; donor phase volume, 75 mL; pH, 3; and sodium chloride concentration, 30% (w/v). After dSPE, the MNPs were eluted twice with 1.5 mL …
Application of matrix solid-phase dispersion to the determination of a new generation of fungicides in fruits and vegetables.
2002
A method based on matrix solid-phase dispersion (MSPD) and gas chromatography to determine eight fungicides in fruits and vegetables is described. Fungicide residues were identified and quantified using nitrogen-phosphorus detection and electron-capture detection connected in parallel and confirmed by mass spectrometric detection. The method required 0.5 g of sample, C18 bonded silica as dispersant sorbent, silica as clean-up sorbent and ethyl acetate as eluting solvent. Recoveries from spiked orange, apple, tomato, artichoke, carrot and courgette samples ranged from 62 to 102% and relative standard deviations were less than 15% in the concentration range 0.05-10 mg kg(-1). Detection and qu…
Sample preparation strategies for the determination of psychoactive substances in biological fluids
2020
This review focuses on the existing analytical procedures for the determination of new psychoactive substances (NPS) in biological fluids by chromatographic methods. Direct analysis of samples is scarcely employed and most proposed methodologies include a sample pre-treatment in order to remove matrix interferents and, in some cases, pre-concentrate extracts. Current extraction methods for NPS determination in plasma/serum, urine, and oral fluids have been widely discussed, such as liquid-liquid, solid-phase, and micro extraction approaches, highlighting the advantages and drawbacks of the proposed extraction methodologies. Regarding microextraction approaches, techniques like microextracti…
Dispersive micro-solid phase extraction
2019
Abstract Dispersive micro-solid phase extraction (D-μSPE) has gained special attention in the sample preparation process due to its simplicity, speed and efficiency. Different dispersion approaches have been used within this technique to allow a close contact between the sorbent and the donor sample solution during the entrapping step, but also between the sorbent and the solvent in the elution step. This dispersion favors the kinetics of both sorption and elution and therefore increases the efficiency of the overall extraction procedure. This technique boasts of high versatility owing to the great variety of solids available, covering a high range of chemical functionalities. This article …
Determination of dithiocarbamates and metabolites in plants by liquid chromatography–mass spectrometry
2004
Abstract A quantitative matrix solid-phase dispersion and liquid chromatography–atmospheric pressure chemical ionization mass spectrometry (LC–APCI–MS) method is outlined for the simultaneous analysis of dithiocarbamates (DTCs) and their degradation products in plants. Compounds analyzed are dazomet, disulfiram, thiram and the metabolites ethylenthiourea and propylenthiourea. The performance of two different sample preparation protocols, the proposed one and other based on solid-phase extraction, as well as, of both atmospheric pressure ionization sources, APCI and electrospray, were compared. The effect of several parameters on the extraction, separation and detection was studied. Dithioca…