Search results for "Column chromatography"

Stability of nitroaromatic specialty explosives in reversed-phase liquid chromatographic systems

2008

Abstract In this study, the stability of 2,4-dinitroanisole, 2,2′,4,4′,6,6′-hexanitrodiphenylsulfide, 2,3,4,6-tetranitroaniline, 2,4,6-trinitroaniline, 2,4,6-trinitroanisole, and 2,4,6-trinitrochlorobenzene in liquid chromatographic systems was studied under different solvent/eluent conditions. Stock solutions of the explosives were prepared in acetonitrile and diluted with acetone/water, acetonitrile/water, or methanol/water mixtures. Within 48 h, these working solutions were repeatedly injected onto a silica column and eluted with acetonitrile/water or methanol/water mobile phases. Under all conditions, 2,4-dinitroanisole was stable, whereas 2,4,6-trinitroaniline was stable only in the me…

Trimeprazine is enantioselectively degraded by an activated sludge in ready biodegradability test conditions

2018

[EN] A great number of available pharmaceuticals are chiral compounds. Although they are usually manufactured as racemic mixtures, they can be enantioselectively biodegraded as a result of microbial processes. In this paper, a biodegradability assay in similar conditions to those recommended in OECD tests of enantiomers of trimeprazine (a phenothiazine employed as a racemate) is carried out. Experiments were performed in batch mode using a minimal salts medium inoculated with an activated sludge (collected from a Valencian Waste Water Treatment Plant, WWTP) and supplemented with the racemate. The concentration of the enantiomers of trimeprazine were monitored by means of a chiral HPLC metho…

On-line coupling of gel electrophoresis and inductively coupled plasma-sector field-mass spectrometry for the determination of dsDNA fragments.

2005

The on-line coupling of gel electrophoresis (GE) and inductively coupled plasma-mass spectrometry (ICPMS) is described for the first time. The new method combines the separation power of GE for large biomolecules and the high sensitivity and elemental selectivity of ICPMS. This coupling has been achieved by means of gels housed in glass tubes (length 2.5-20 cm; i.d. 0.5-5 mm). The gel is fixed by glass frits permeable for the analytes. After the electrophoretic separation at voltages up to 500 V, the analytes are transferred to the nebulizer of the ICPMS by an eluent stream, which is separated from the electrode chamber by a membrane. This filter blocks molecules with molecular masses large…

Separation of pesticides, related compounds, polychlorobiphenyls and other pollutants into four groups by silica‐gel microcolumn chromatography (appl…

1991

Multi‐residue analyses of pesticides and related compounds generally require clean‐up procedures for the elimination of interfering substances. An analytical procedure for use in the recovery and determination of pesticides and other pollutants in water samples is described, in which the purification of the extracts is improved by the separation of pesticides into four groups. The separation of pesticides by silica‐gel microcolumn chromatography is explained in detail. Copyright © 1991 John Wiley & Sons, Ltd

Solution properties of polyelectrolytes. I. Exclusion chromatography of sodium polystyrene sulphonate in salt-free water as eluent

1987

The effect of concentration of sodium polystyrene sulphonate on the elution volume in exclusion chromatography has been investigated using salt-free water as eluent. A non-linear increase in the elution volume has been observed with increasing injected sample concentration. Concentration-dependent calibrations have been obtained which approach the universal calibration for uncharged polymers (dextrans) as polyelectrolyte concentration increases. The separation mechanisms are interpreted in terms of electrostatic and hydrodynamic interactions. A semi-empirical model is proposed to predict concentration effects of linear polyions in exclusion chromatography and good agreement has been found b…

Gel permeation chromatography, calibration, and distributions of cellulose trinitrates

1967

Separation and identification of petroporphyrins extracted from the oil shales of Tarfaya: geochemical study

2002

Abstract Vanadyl and nickel porphyrins were isolated from the oil shales of Tarfaya (Morocco) by extraction followed by column chromatography. The ratios and characteristics of these porphyrin complexes were essentially obtained on the basis of UV–visible and mass spectrometry data. Geochemical information could be drawn from these data. The nature and the contents of the metals coordinated and non-coordinated to porphyrin systems were also determined in this study.

π-Extended Pyrene-Fused Double [7]Carbohelicene as a Chiral Polycyclic Aromatic Hydrocarbon

2019

A π-extended double [7]carbohelicene 2 with fused pyrene units was synthesized, revealing considerable intra- and intermolecular π–π interactions as confirmed with X-ray crystallography. As compared to the previous double [7]carbohelicene 1, the π-extended homologue 2 demonstrated considerably red-shifted absorption with an onset at 645 nm (1: 550 nm) corresponding to a smaller optical gap of 1.90 eV (1: 2.25 eV). A broad near-infrared emission from 600 to 900 nm with a large Stokes shift of ∼100 nm (2.3 × 103 cm–1) was recorded for 2, implying formation of an intramolecular excimer upon excitation, which was corroborated with femtosecond transient absorption spectroscopy. Moreover, 2 revea…

HPLC-SEC: a new approach to characterise complex wastewater effluents

2016

ABSTRACTThis work investigates the use of HPLC-SEC to characterise dissolved organic matter (DOM) of complex wastewater effluents. A silica-based column, sodium acetate eluent and multiple detections were employed: UV-254 absorbance for humictype, and tryptophan-like (Ex/Em = 270/355) and tyrosine-like (Ex/Em = 270/310) fluorescence for protein type compounds. Effects of eluent pH, eluent ionic strength and injection volume on separation efficiency were tested. Humic-type and protein-type fractions were clearly differentiated and eluted within and out of calibration range. Eluent ionic strength had the greatest influence on global resolution; the lowest eluent concentration of 0.01 M produc…

Chemical profiling of the synthetic cannabinoid MDMB-CHMICA: Identification, assessment, and stability study of synthesis-related impurities in seize…

2019

In this work, the most discriminating synthesis-related impurities found in samples from seizures and controlled synthesis of the synthetic cannabinoid MDMB-CHMICA (methyl (S)-2-(1-(cyclohexylmethyl)-1H-indole-3-carboxamido)-3,3-dimethylbutanoate) were characterized. Based on 61 available powder samples of MDMB-CHMICA, 15 key-impurities were assessed, isolated in larger quantities via flash chromatography and structurally elucidated and characterized via high resolution mass spectrometry and nuclear magnetic resonance spectroscopy. Apart from verifying the relation of the impurities to the major component, the interpretation of their chemical structures with distinct structural elements pro…