Search results for "HPLC"
showing 10 items of 201 documents
Preparation of organic monolithic columns in polytetrafluoroethylene tubes for reversed-phase liquid chromatography
2017
[EN] In this work, a method for the preparation and anchoring of polymeric monoliths in a polytetrafluoroethylene (PTFE) tubing as a column housing for microbore HPLC is described. In order to assure a covalent attachment of the monolith to the inner wall of the PTFE tube, a two-step procedure was developed. Two surface etching reagents, a commercial sodium naphthalene solution (Fluoroetch®), or mixtures of H2O2 and H2SO4, were tried and compared. Then, the obtained hydroxyl groups on the PTFE surface were modified by methacryloylation. Attenuated total reflectance Fourier-transform infrared (ATR-FTIR) spectroscopy and scanning electron microscopy (SEM) confirmed the successful modification…
Phosphatidylcholine covalently linked to a methacrylate-based monolith as a biomimetic stationary phase for capillary liquid chromatography
2015
Abstract In this study a strategy to immobilize phospholipids onto a polymer-based stationary phase is described. Methacrylate-based monoliths in capillary format (150 × 0.1 mm) were modified by soybean phosphatidylcholine through 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide coupling to obtain stationary phases suitable to mimic cell surface membranes. The covalent coupling reaction involves the phosphate group in phospholipids; therefore, the described methodology is suitable for all types of phospholipids. Immobilization of soy bean phosphatidylcholine on the monolith was confirmed by attenuated total reflectance Fourier transform infrared spectroscopy and gas chromatography-mass spectro…
3D printed fluidic platform with in-situ covalently immobilized polymer monolithic column for automatic solid-phase extraction
2020
Abstract In this work, 3D stereolithographic printing is proposed for the first time for the fabrication of fluidic devices aimed at in-situ covalent immobilization of polymer monolithic columns. Integration in advanced flow injection systems capitalized upon programmable flow was realized for fully automatic solid-phase extraction (SPE) and clean-up procedures as a ‘front-end’ to on-line liquid chromatography. The as-fabricated 3D-printed extraction column devices were designed to tolerate the pressure drop of forward-flow fluidic systems when handling large sample volumes as demonstrated by the determination of anti-microbial agents, plastic additives and monomers as models of emerging co…
Preparation of monolithic polymer-magnetite nanoparticle composites into poly(ethylene-co-tetrafluoroethylene) tubes for uses in micro-bore HPLC sepa…
2021
[EN] This paper describes the fabrication of a novel microbore monolithic column modified with magnetite nanoparticles (MNPs) prepared in a poly(ethylene-co-tetrafluoroethylene) (EFTE) tubing, and its application as stationary phase for the chromatographic separation of phosphorylated compounds. In order to obtain the composite column, a two-step procedure was performed. The formation of a glycidyl methacrylate-based monolith inside the activated ETFE tube was firstly carried out. Then, two incorporation approaches of MNPs in monoliths were investigated. The generic polymer was modified with 3-aminopropyltrimethoxysilane (APTMS) to be subsequently attached to MNP surfaces. Alternatively, AP…
Photografted fluoropolymers as novel chromatographic supports for polymeric monolithic stationary phases
2018
[EN] In this study, porous polymer monoliths were in situ synthesized in fluoropolymers tubing to prepare microbore HPLC columns. To ensure the formation of robust homogeneous polymer monoliths in these housing supports, the inner surface of fluoropolymer tubing was modified in a two-step photografting process. Raman spectroscopy and scanning electron microscopy (SEM) confirmed the successful modification of the inner poly(ethylene-co-tetrafluoroethylene) (ETFE) wall and the subsequent attachment of a monolith onto the wall. Poly(glycidyl methacrylate-co-divinylbenzene), poly(butyl methacrylate-co-ethyleneglycol dimethacrylate) and poly(styrene-co-divinylbenzene) monoliths were in situ synt…
Validation of a multi-residue UHPLC-HRMS method for antibiotics screening in milk, fresh cheese, and whey
2022
Abstract The aim of this study was to develop a UHPLC–HRMS methodology as a suitable tool for the screening of antibiotics in milk, fresh cheese, and whey. Compounds were analysed using an Orbitrap Exactive™ analyser working at a resolving power of 50,000 FWHM in full scan, both in positive and negative electrospray ionization mode, and a high mass accuracy (
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…
Organophosphorus pesticides (chlorfenvinphos, phosmet and fenamiphos) photoelectrodegradation by using WO3 nanostructures as photoanode
2021
[EN] The photoelectrocatalytic (PEC) degradation of recalcitrant and toxic organophosphorus pesticides, fenamiphos, chlorfenvinphos and phosmet, has been performed by using an innovative WO3 nanostructure as photoanode. The nanostructure has been synthesized by anodization in acidic media in the presence of a very small amount (0.05 M) of H2O2, and its composition as well as its photoelectrochemical properties have been characterized using X-ray Photoelectron Spectroscopy and X-ray diffraction as composition technique and photoelectrochemical impedance spectroscopy as photoelectrochemical analysis. After 24 h of experiment, a degradation of 95% of chlorfenvinphos, 99.9% of phosmet and 100% …
Natural co-occurrence of ochratoxin A, ochratoxin B and aflatoxins in Sicilian red wines
2015
The natural occurrence of ochratoxin A, ochratoxin B, aflatoxin B1, aflatoxin B2, aflatoxin G1 and aflatoxin G2 (OTA, OTB, AFB1, AFB2, AFG1, AFG2) in red wines was investigated by HPLC/FLD after immunoaffinity column clean-up in 57 market samples produced in Sicily (Italy). The results showed a very low incidence of these mycotoxins in analysed samples, confirming the high degree of quality and safety of Sicilian red wines. The results indicated 71.9% and 64.9% positive samples for OTA and OTB respectively, with an average level of 0.13 μg l(-1), well below the European maximum permitted levels (MLs). The aflatoxin most frequently detected in the samples was AFG1, present in 57.9% of sample…
Mycotoxins in herbal teas marketed in Latvia and dietary exposure assessment
2019
The occurrence of 12 mycotoxins has been analysed by liquid chromatography - time of flight mass spectrometry in the batch of 60 herbal teas purchased from drugstores in Latvia. Among the dry tea samples, 90% were positive for one to eight mycotoxins. Enniatin B and deoxynivalenol (DON) were the most frequently detected mycotoxins in 55% and 45% of the samples, respectively. DON reached the highest level, from 129 µg kg-1 in herbal blend to 5,463 µg kg-1 in wormwood tea. Ochratoxin A (OTA) and aflatoxin B1 (AFB1) were found in 10% and 20% of the samples at the concentrations ranged between 2.99-30.3 µg kg-1 and 3.40-23.7 µg kg-1. Studies of the tea infusion process indicated that 32-100% of…