Search results for "Spectroscopy"
showing 10 items of 10293 documents
HPLC in the characterisation of conformational species of linear gramicidins
1997
Abstract High-performance size-exclusion chromatography (HPSEC) has proved to be a highly simplified and rapid procedure to investigate the conformational behaviour of gramicidin A inserted in different model membrane systems (lipid dispersions, liposomes, micelles) based on the separation of double-stranded dimers and monomers present in the lipid assemblies. The HPSEC approach has been extended to the characterisation of acylated analogs of gramicidin (palmitoyl- and oleoyl-derivatives) and a series of peptide analogs where tryptophan residues were chemically modified or replaced by less polar residues (phenylalanine or naphtylalanine) lacking H-bonding ability. The Chromatographic result…
Determination of the four major surfactant classes in cleaning products by reversed-phase liquid chromatography using serially connected UV and evapo…
2016
Abstract A method for the simultaneous determination of the most frequently used surfactant families –linear alkyl benzenesulphonates (LAS), alkyl ether sulphates (AES), fatty alcohol ethoxylates (FAE) and oleins (soaps, fatty acid salts) – in cleaning products, has been developed. The common reversed phase octyl (C8), pentafluorophenyl and biphenyl columns were not capable of separating the anionic LAS and AES classes; however, since only LAS absorbs in the UV, these two classes were independently quantified using a C8 column and serially connected UV and ELSD detection. The best compromise to resolve the four surfactant classes and the oligomers within the classes was achieved with a C8 c…
Microwave-assisted extraction of OCPs, PCBs and PAHs concentrated by semi-permeable membrane devices (SPMDs)
2005
Abstract Microwave-assisted extraction (MAE) has been evaluated as an alternative to dialysis for extraction of some water-borne hydrophobic contaminants sampled by semi-permeable membrane devices (SPMDs). Seven organochlorine pesticides (OCPs), 11 polychlorinated biphenyls (PCBs) and 13 polycyclic aromatic hydrocarbons (PAHs) were accumulated in SPMDs at nanogram levels and extracted with three 3-min irradiation cycles with 33 mL of a solvent mixture hexane–water (10:1,v/v) in each cycle. The developed MAE method gave for all analytes investigated statistically comparable extraction yields with those found by dialysis carried out with a total volume of 250 mL hexane for 48 h at room temper…
Characterization of aquatic humic substances and their metal complexes by immobilized metal-chelate affinity chromatography on iron(III)-loaded ion e…
2001
The analytical fractionation of aquatic humic substances (HS) by means of immobilized metal-chelate affinity chromatography (IMAC) on metal-loaded chelating ion exchangers is described. The cellulose HYPHAN, loaded with different trivalent ions, and the chelate exchanger Chelex 100, loaded to 90% of its capacity with Fe(III), were used. The cellulose HYPHAN, loaded with 2% Fe(III), resulted in HS distribution coefficients Kd of up to 10(3.7) mL/g at pH 4.0 continuously decreasing down to 10(1.5) at pH 12, which were appropriate for HS fractionation by a pH-depending chromatographic procedure. Similar distribution coefficients Kd were obtained for HS sorption onto Fe(III)-loaded Chelex 100. …
Development of a semiautomated procedure for the synthesis and evaluation of molecularly imprinted polymers applied to the search for functional mono…
2001
Abstract A previously described scaled-down version of the established monolith procedure, where molecularly imprinted polymers (MIPs) are prepared on the bottom surface of chromatographic vials [Anal. Chem. 71 (1999) 2092] has been here further optimised with respect to its full automation. The protocol results in savings of time and reagents compared to the monolith procedure, allowing ca. 60 polymers (∼50 mg each) to be synthesised in parallel. Both blank and imprinted polymers are then evaluated in situ by equilibrium batch rebinding tests. Each step in the synthesis and evaluation was considered with the aim of achieving an automated method with wide applicability with regards to templ…
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…
Non-porous polybutadiene-coated silicas as stationary phases in reversed-phase chromatography
1990
Abstract Non-porous silica of mean particle diameter 1.7 μm (Monospher) was coated with polybutadiene (PBD) following a published procedure. The silicas were prepared with graduated polymer loads up to 8% (w/w). Examination of the PBD-coated packings by means of electron spectroscopy for chemical analysis, scanning electron microscopy, diffuse reflection infrared fourier transform spectroscopy and differential thermal gravimetry indicated that the optimum polymer load was between 1 and 3% (w/w) with regard to a dense coverage corresponding to an average layer thickness of about 4 nm. No silanophilic interactions could be monitored using 1–3% (w/w) coated silicas under reversed-phase conditi…
Determination of indoor air quality of a phytosanitary plant.
2011
A new methodology has been developed to determine volatile organic compounds (VOCs) and pesticides in ambient air using membrane based devices as passive samplers. Pesticides were determined by gas chromatography with mass spectrometry detection (GC-MS) after their microwave-assisted extraction (MAE) from the passive sampler and the required clean-up. On the other hand, VOCs were also caught with the same samplers and directly determined by head space (HS) coupled to GC-MS. The use of samplers filled with florisil and activated carbon allows us to catch with a simple device both, VOCs and pesticides, with a high vapor pressure. Results obtained in the deployment of samplers in different sit…
Flow-injection spectrophotometric determination of amino acids based on an immobilised copper(II) -zincon system
1993
Abstract The flow-injection spectrophotometric determination of different amino acids was carried out by reaction with copper(II) ions entrapped in a polymeric material and filling a packed-bed reactor; the released copper(II), complexed with the amino acid, reacted with zincon in a basic medium producing a blue colour that was monitored at 600 nm. The method was applied to determine the contents of different amino acids in pharmaceutical formulations. The calibration graph for glycine was linear over the range 0.5–20 μg ml −1 with a relative standard deviation of 0.8% ( n = 6) at 10 μg ml −1 and a sample throughput of 108 h −1 .
New acetylenes fromChrysanthemum coronarium L.
1990
The investigation of the aerial parts of Chrysanthemum coronarium yielded, in addition to several known compounds, two new acetylenic sulfoxides 9 and 10, and a new thiophene spiroacetal enol ether 11. Their structures were deduced by spectroscopic and chemical methods.