Search results for " Phase"

Selective extraction of small proteins from biological samples using a novel restricted access column with cation exchange properties

2000

The determination of proteins utilising a polymer-based restricted access suppor material with ion exchange properties (IERAM) is outlined. Solid phase extraction coupled on-line with a mincrobore reversed phase HPLC system for the quantitation of small marker proteins is demonstrated. The cation-exchange restricted access packings were characterised with respect to their adsorption and desorption kinetics. The IERAM material was also investigated by capacity, selectivity, and biocompatibility determinations when applied to the quantification of small molecular weight proteins such as cytochrome C, Lysozyme, Ribonuclease A, Myoglobin, Insulin, human serum albumin, and a Tryptic inhibitor.

Fast high performance liquid chromatography analysis in lipidomics: Separation of radiolabelled fatty acids and phosphatidylcholine molecular species…

2006

Abstract HPLC procedures using conventional C 18 columns are usually used to separate simple and complex lipid mixtures but these methods of separation remain often laborious and very slow. Here, monolithic columns were successfully applied to separate lipids – radiolabelled fatty acid mixtures and individual phosphatidylcholine (PC) molecular species. For that, isocratic elution was performed using two Chromolith™ Performance RP-18e columns connected in series. Detection was achieved by online measurement of radioactivity for radiolabelled fatty acids and by UV absorbance at 205 nm for PC molecular species. The performances of such silica rods were compared to conventional reverse-phase si…

Selective solid phase extraction of a drug lead compound using molecularly imprinted polymers prepared by the target analogue approach

2002

Molecularly imprinted polymers have been evaluated at the sample clean-up stage in the analysis of a drug lead compound. In order to circumvent quantification problems related to bleeding of the template, a structurally related analogue of the latter was used. This was selected based on criteria related to interaction site location, solubility, availability and stability of the analogue. Selection of suitable polymerisation conditions was then made using a small batch format (ca. 50 mg) and rapid assessment of binding in the equilibrium mode. It was found that the amount of template could be greatly reduced compared to the conventional protocol, requiring only 5 μmol of template per gram of…

Prediction of the retention in reversed-phase liquid chromatography using solute-mobile phase-stationary phase polarity parameters.

2002

Abstract A previously reported algorithm, based on the equation: log k=( log k) 0 +p(P N m −P N s ) , that relates the retention in reversed-phase liquid chromatography with solute (p), mobile phase (PmN) and stationary phase (PsN) relative polarity parameters, is improved. The retention data reported by several authors for different sets of compounds, eluted with acetonitrile–water and methanol–water mixtures, are used to test the algorithm and elaborate a database of p values. The methodology is successfully applied to predict the retention using PmN values calculated as PmN=1.00−(2.13ϕ)/(1+1.42ϕ) for acetonitrile–water and PmN=1.00−(1.33ϕ)/(1+0.47ϕ) for methanol–water, ϕ being the organi…

Direct Solid Phase Microextraction for the Determination of BTEX in Water and Wastewater

1996

Heterogeneity at the glass transition: a review

1999

Theoretical concepts and experimental evidence of heterogeneity in glass-forming liquids and polymers are reviewed. The main purpose is to provide an introduction to theoretical developments and recent experiments which have led to rapidly increasing knowledge. Realizing that there is no consensus in regard to the various scenarios of the glass transition starting from rather different assumptions we try to give a balanced overview although we also compare and interrelate some of the approaches. The experimental part describes recent nuclear magnetic resonance, dielectric, and optical experiments from which dynamically distinguishable subensembles can be selected thus proving the existence …

In-tube solid-phase microextraction coupled by in valve mode to capillary LC-DAD: Improving detectability to multiresidue organic pollutants analysis…

2009

Abstract A simple and fast capillary chromatographic method has been developed to identify and quantify organic pollutants at sub-ppb levels in real water samples. The major groups of pesticides (organic halogens, organic phosphorous, and organic nitrogen compounds), some hydrocarbons (polycyclic aromatic hydrocarbons), phthalates and some phenols such as phenol and bisphenol A (endocrine disruptors) were included in this study. The procedure was based on coupling, in-tube solid-phase microextraction (IT-SPME) by using a conventional GC capillary column (95% methyl–5% phenyl substituted backbone, 80 cm × 0.32 mm i.d., 3 μm film thickness) in the injection valve to capillary liquid chromatog…

Indirect analysis of urea herbicides from environmental water using solid-phase microextraction.

2000

We described here a solid-phase microextraction procedure used to extract six urea pesticides-- chlorsulfuron, fluometuron, isoproturon, linuron, metobromuron and monuron--from environmental samples. Two polydimethylsiloxanes and a polyacrylate fiber (PA) are compared. The extraction time, pH control, addition of NaCl to the water and the influence of organic matter such as humic acid on extraction efficiency were examined to achieve a sensitive method. Determination was carried out by gas chromatography with nitrogen-phosphorus detection. The proposed method requires the extraction of 2 ml of sample (pH 4, 14.3%, w/v, NaCl) for 60 min with the PA fiber. The limits of detection range from 0…

Host-guest interactions for extracting antibiotics with a γ-cyclodextrin poly(glycidyl-co-ethylene dimethacrylate) hybrid sorbent

2021

Abstract A procedure for the solid-phase extraction of antibiotics (enoxacin, ofloxacin, norfloxacin, ciprofloxacin, and sparfloxacin) in water has been developed. The sorbent used is based on a poly(glycidyl-co-ethylene dimethacrylate) network, whose previously modified surface has been functionalized with γ-cyclodextrin through a click-chemistry reaction. The architecture of the material has been characterized by thermogravimetric analysis, N2 adsorption-desorption, Raman spectroscopy, confocal microscopy, and scanning electron microscopy, showing good capability to be used as a filler for extraction cartridges. The optimization of the extraction methodology shows good intra-day and inter…

Role of hexagonal structure-forming lipids in diadinoxanthin and violaxanthin solubilization and de-epoxidation

2005

In this study, we have examined the influence of different lipids on the solubility of the xanthophyll cycle pigments diadinoxanthin (Ddx) and violaxanthin (Vx) and on the efficiency of Ddx and Vx de-epoxidation by the enzymes Vx de-epoxidase (VDE) from wheat and Ddx de-epoxidase (DDE) from the diatom Cyclotella meneghiniana, respectively. Our results show that the lipids MGDG and PE are able to solubilize both xanthophyll cycle pigments in an aqueous medium. Substrate solubilization is essential for de-epoxidase activity, because in the absence of MGDG or PE Ddx and Vx are present in an aggregated form, with limited accessibility for DDE and VDE. Our results also show that the hexagonal st…