Search results for "SOLID-PHASE"

Solid-phase microextraction-liquid chromatography-mass spectrometry applied to the analysis of insecticides in honey

2007

An approach based on solid-phase microextraction-liquid chromatography-mass spectrometry (SPME-LC-MS) has been developed for determining 12 insecticides (bromophos ethyl, chlorpyrifos methyl, chlorpyrifos ethyl, diazinon, fenoxycarb, fonofos, phenthoate, phosalone, pirimiphos methyl, profenofos, pyrazophos, and temephos) in honey. The influence of several parameters on the efficiency of the SPME was systematically investigated. Under optimal conditions, the procedure provided excellent linearity (>0.990), detection and quantification limits (between 0.001 and 0.1 microg g(-1) and between 0.005 and 0.5 microg g(-1), respectively), and precision (<19% at the quantification limits and from 6 t…

Highly selective recovery of Ni(II) in neutral and acidic media using a novel Ni(II)-ion imprinted polymer

2022

In this work, an original ion-imprinted polymer (IIP) was synthetized for the highly selective removal of Ni(II) ions in neutral and acidic media. First a novel functional monomer (AMP-MMA) was synthetized through the amidation of 2-(aminomethyl)pyridine (AMP) with methacryloylchloride. Following Ni(II)/AMP-MMA complex formation study, the Ni(II)-IIP was produced via inverse suspension polymerization (DMSO in mineral oil) and characterized with solid state 13C CPMAS NMR, FT-IR, SEM and nitrogen adsorption/desorption experiments. The Ni(II)-IIP was then used in solid-phase extraction of Ni(II) exploring a wide range of pH (from neutral to strongly acidic solution), several initial concentrat…

Induction of Cell Differentiation in Transformed Keratinocytes by Synthetic (Glyco)peptides from the Homophilic Recognition Domain of E-Cadherin

2002

Aroma Profiling of Leaf, Flower, Peel and In Vitro Embryo Tissues of “Ciaculli Late” Mandarin

2003

Abstract Volatile compounds released from leaf, flower and peel as well as from somatic (nucellar) embryo tissues of “Tardivo di Ciaculli” or “Ciaculli late” mandarin have been collected/ concentrated by headspace solid phase microextraction, HS-SPME, and analyzed by GC-MS. The tehnique allowed the rapid comparison of the volatiles from the various sources; in particular, 19 compounds were identified for the embryos, 16 for leaf and flower and 13 for peel. Limonene was the most abundant volatile component of the embryo and peel while γ-terpinene was the major compound among volatiles from leaf and flower. Relatively high amounts of methyl N-methyl anthranilate and β-caryophyllene were also …

The application of molecular imprinting technology to solid phase extraction

2001

In parallel to a long lasting search for universal multi-purpose sorbents, the area of solid phase extraction (SPE) is recently experiencing a rapid development of new types of tailor-made class specific or compound-specific sorbents which are designed to respond to the increasing demand for selectivity and efficiency in sample clean-up prior to quantification. An important issue here is the enrichment and clean-up of complex samples, such as environmental waters, sediments, biofluids and foodstuffs prior to detection. This because the analyte is often present in low concentration in a complex mixture of similar compounds and therefore needs to be isolated and enriched in order to be detect…

Polymeric monolithic microcartridges with gold nanoparticles for the analysis of protein biomarkers by on-line solid-phase extraction capillary elect…

2020

In this study, polymeric monoliths with gold nanoparticles (AuNP@monolith) were investigated as microcartridges for the analysis of protein biomarkers by on-line solid-phase extraction capillary electrophoresis-mass spectrometry (SPE-CE-MS). “Plug-and-play” microcartridges (7 mm) were prepared from a glycidyl methacrylate (GMA)-based monolithic capillary column (5 cm x 250 µm i.d.), which was modified with ammonia and subsequently functionalized with gold nanoparticles (AuNPs). The performance of these novel microcartridges was evaluated with human transthyretin (TTR), which is a protein related to different types of familial amyloidotic polyneuropathies (FAP). Protein retention depended on…

Synthesis of a polymer-bound galactosylamine and its application as an immobilized chiral auxiliary in stereoselective syntheses of piperidine and am…

2004

A 2,3,4-tri-O-pivaloylated beta-D-galactopyranosyl azide bearing a hydroxy-functionalized spacer unit at the C-6 position of the galactose was synthesized and immobilized on the solid phase by using a polymer-bound chlorosilane. The azide was reduced to the corresponding galactopyranosylamine, which served as a versatile chiral auxiliary in highly diastereoselective Ugi four-component condensation reactions at ambient temperature. Fluoride-induced cleavage from the polymeric support furnished N-glycosylated N-acylated alpha-amino acid amides. The reaction of the immobilized galactosylamine with aldehydes gave rise to the corresponding aldimines, which underwent a domino Mannich-Michael cond…

Investigation of cuticular hydrocarbons from Bagrada hilaris genders by SPME/GC-MS

2007

The cuticular hydrocarbons of male and female Bagrada hilaris Burmeister (Heteroptera: Pentatomidae) were investigated, by headspace solid-phase microextraction followed by gas chromatography-mass spectrometry. Measurements were done with fiber coatings of different polarity after optimization of headspace volumes and extraction temperatures. This resulted in the use of polyacrylate fiber, 22-ml vial as the sample holder, and an extraction temperature of 150 degrees C. The analytical procedures allowed identification of 13 peaks, corresponding to a homologous series of n-alkanes (nC(17)-nC(29)). The hydrocarbon profiles of male and female B. hilaris were qualitatively equal, but marked sex-…

Innovations in Extractive Phases for In-Tube Solid-Phase Microextraction Coupled to Miniaturized Liquid Chromatography: A Critical Review

2020

Over the past years, a great effort has been devoted to the development of new sorbents that can be used to pack or to coat extractive capillaries for in-tube solid-phase microextraction (IT-SPME). Many of those efforts have been focused on the preparation of capillaries for miniaturized liquid chromatography (LC) due to the reduced availability of capillary columns with appropriate dimensions for this kind of system. Moreover, many of the extractive capillaries that have been used for IT-SPME so far are segments of open columns from the gas chromatography (GC) field, but the phase nature and dimensions are very limited. In particular, polar compounds barely interact with stationary GC phas…

Improving the On-Line Extraction of Polar Compounds by IT-SPME with Silica Nanoparticles Modified Phases

2018

In the present work the extraction efficiency of in-tube solid-phase microextraction (IT-SPME) for polar herbicides has been evaluated using extractive capillaries coated with different polymeric sorbents. For this purpose, aqueous solutions of herbicides with a wide range of polarities, including some highly polar compounds (log Kow &lt; 1), have been directly processed by IT-SPME coupled on-line to capillary liquid chromatography with UV-diode array detection. For extraction, commercially available capillary columns coated with polydimethylsiloxane (PDMS) and polyetilenglicol (PEG)-based phases have been used, and the results have been compared with those obtained with a synthesized tetra…