Search results for "phase microextraction"
showing 10 items of 134 documents
The summertime Boreal forest field measurement intensive (HUMPPA-COPEC-2010): an overview of meteorological and chemical influences
2011
This paper describes the background, instrumentation, goals, and the regional influences on the HUMPPACOPEC intensive field measurement campaign, conducted at the Boreal forest research station SMEAR II (Station for Measuring Ecosystem-Atmosphere Relation) in Hyyti¨al¨a, Finland from 12 July–12 August 2010. The prevailing meteorological conditions during the campaign are examined and contrasted with those of the past six years. Back trajectory analyses show that meteorological conditions at the site in 2010 were characterized by a higher proportion of southerly flow than in the other years studied. As a result the summer of 2010 was anomalously warm and high in ozone making the campaign rel…
Determination of ketosteroid hormones in meat by liquid chromatography tandem mass spectrometry and derivatization chemistry.
2015
A method for the determination and quantification of ketosteroid hormones in meat by mass spectrometry, based on the derivatization of the carbonyl moiety of steroids by O-methylhydroxylamine, is presented. The quantitative assay is performed by means of multiple-reaction-monitoring (MRM) scan mode and using the corresponding labelled species, obtained by reaction with d 3-methoxylamine, as internal standard. The accuracy of the method was established by evaluating artificially spiked samples, obtaining values in the range 90-110%. Recovery tests were performed on blank matrix samples spiked with non-natural steroids including trenbolone and melengestrol acetate. The latter experiment revea…
Multivariate approach to reveal relationships between sensory perception of cheeses and aroma profile obtained with different extraction methods
2014
A new and original statistical approach was used to compare the effectiveness of 4 different methods to analyse aroma compounds of seven different commercial semi-hard cheeses with regard to their orthonasal sensory perception. Four extraction methods were evaluated: Purge and Trap, Artificial Mouth, Solid-Phase Microextraction (SPME) and Solvent-Assisted Flavour Evaporation (SAFE). Among the headspace methods, Artificial Mouth gave the closest representation of the studied product space to the sensory perception one. The SAFE method was complementary to the dynamic headspace methods, as it was very efficient in extracting the heavy molecules but less efficient for extracting the most volat…
Combining poly(dimethyldiphenylsiloxane) and nitrile phases for improving the separation and quantitation of benzalkonium chloride homologues: In-tub…
2013
The retention and separation of four homologues of benzalkonium chloride (alkyl (C12, C14, C16, C18) dimethylbenzylammonium chloride) have been studied in poly(dimethyldiphenylsiloxane) (TRB) and nitrile capillary phases, respectively. Under the optimized conditions (50% acetonitrile in processed samples, 35% of diphenyl content of the TRB, capillary length 43 cm and water:methanol 60:40 as replacing solvent), the extraction efficiency was similar for all the homologues with satisfactory reproducibility and independently of the amount and proportion of homologues. Industrial samples with high viscosity or with complex composition and washes waters have been analyzed without previous treatme…
Footprint of carbonyl compounds in hand scent by in-tube solid-phase microextraction coupled to nano-liquid chromatography/diode array detection
2019
Abstract In the present work, the footprint of carbonyl compounds in hand scent was achieved by a miniaturized method consisting of sampling with cotton gauze, extraction and derivatization using 2,4-dinitrophenylhydrazine (DNPH) and preconcentration, separation and detection by in-tube solid-phase microextraction (IT-SPME) coupled to nano-liquid chromatography/Uv–vis diode array detection. The coupling IT-SPME-nanoLC-DAD was solved by using a two-valve system: the first valve for loading the sample and the second one to perform IT-SPME. To this aim, a nanoparticle-based capillary column was employed. Firstly, the transfer time from the load loop to the NP-based capillary column in the IT-S…
Occurrence of Mycotoxins in Botanical Dietary Supplement Infusion Beverages.
2019
The aim of the present work was to study the occurrence of mycotoxins [aflatoxins (1-4), 3-acetyldeoxyniavlenol (5), 15-acetyldeoxynivalenol (6), nivalenol (7), HT-2 (8), T-2 (9), ochratoxin A (10), zearalenone (11), enniatin A (12), enniatin A1 (13), enniatin B (14), enniatin B1 (15), and beauvericin (16)] present in potable products derived from herbal teas. Analysis was carried out by liquid chromatography coupled to ion-trap tandem mass spectrometry (LC-MS/MS-IT) after a dispersive liquid-liquid microextraction procedure (DLLME) was conducted. The DLLME method was applied to 52 commercial samples of chamomile, chamomile with anise, chamomile with honey, linden, pennyroyal mint, thyme, v…
Multimycotoxin analysis in water and fish plasma by liquid chromatography-tandem mass spectrometry
2015
High performance liquid chromatography-mass spectrometry was used for the determination of 15 mycotoxins in water and fish plasma samples, including aflatoxins, fumonisins, ochratoxin A, sterigmatocistin, fusarenon-X and emerging Fusarium mycotoxins. In this work, dispersive liquid-liquid microextraction (DLLME) was assessed as a sample treatment for the simultaneous extraction of mycotoxins. Results showed differences in recovery assays when different extraction solvents were employed. Ethyl acetate showed better recoveries for the major part of mycotoxins analyzed, except for aflatoxins B2, G1 and G2, which showed better recoveries when employing chloroform as extractant solvent. Fumonisi…
Direct Analysis of Psilocin and Muscimol in Urine Samples Using Single Drop Microextraction Technique In-Line with Capillary Electrophoresis
2020
The fully automated system of single drop microextraction coupled with capillary electrophoresis (SDME-CE) was developed for in-line preconcentration and determination of muscimol (MUS) and psilocin (PSC) from urine samples. Those two analytes are characteristic active metabolites of Amanita and Psilocybe mushrooms, evoking visual and auditory hallucinations. Study analytes were selectively extracted from the donor phase (urine samples, pH 4) into the organic phase (a drop of octanol layer), and re-extracted to the acidic acceptor (background electrolyte, BGE), consisting of 25 mM phosphate buffer (pH 3). The optimized conditions for the extraction procedure of a 200 µ
Bimodal copper oxide nanoparticles doped phase for the extraction of highly polar compounds by in-tube solid-phase microextraction coupled on-line to…
2020
Abstract Polymers obtained from tetraethyl orthosilicate (TEOS) and triethoxymethylsilane (MTEOS) have been functionalized with different metal and metal oxide nanoparticles (NPs), and used as coatings of extractive capillaries for the extraction of polar compounds by in-tube solid-phase microextraction (IT-SPME) coupled on-line to nano-liquid chromatography (nano-LC). The extraction capabilities of the new phases have been studied using several triazinic herbicides with log of octanol/water partition coefficients (Kow) ranging from -0.7 to 3.21 under reversed phase chromatographic conditions. Best extraction efficiencies for the most polar compounds (log Kow ≤ 2.3) were typically obtained …
Comparison of stir bar sorptive extraction in the liquid and vapour phases, solvent-assisted flavour evaporation and headspace solid-phase microextra…
2017
The volatile fraction plays an important role on the organoleptic properties and overall acceptability of fruit juices. This work reports for first time a non-targeted approach for the analysis of the volatile fraction of fruit juice by stir bar sorptive extraction (SBSE[1]) in liquid and vapour phase (HSSE[2]) at three extraction times (30, 60, and 120 min), two temperatures (room temperature and 40 °C), and two sample volumes (5 and 10 mL). The resultant volatile profiles were compared with solvent-assisted flavour evaporation (SAFE[3]) and headspace solid-phase microextraction (HS-SPME[4]). SBSE and HSSE enabled the detection and identification of more compounds than HS-SPME and less tha…