Search results for "Elution"
showing 10 items of 337 documents
Zur Gelpermeationschromatographie in organischen Lösungsmitteln
1965
Die Gelpermeationschromatographie hat sich vor allem mittels der Sephadexgele fur die Trennung polymerhomologer wasserloslicher Makromolekule als sehr erfolgreich erwiesen. Die Trennung nur in organischen Losungsmitteln loslicher Polymerer ist erst in jungster Zeit gelungen, wobei vernetzte Polystyrol-, Polymethacrylat- und Dextranderivatgele benutzt werden. Der Mechanismus dieses chromatographischen Prozesses wird untersucht. Ein Vergleich dieses Vorganges, bei dem das Polymere nur in einer Phase vorliegt, mit den klassischen Methoden, die mit Auftrennung in zwei Phasen arbeiten, wird durchgefuhrt. Insbesondere werden die Methoden der Dreiecks-Fallungsfraktionierung, der Kolonnentechnik mi…
Application of liquid-liquid partition chromatography in the simultaneous purification of sex-hormone-binding globulin and corticosteroid-binding glo…
1987
Two human serum proteins, corticosteroid-binding globulin (CBG) and sex-hormone-binding globulin (SHBG), were purified to homogeneity by the application of a combination of three different modes of chromatography. Human pregnancy serum was fractionated with ammonium sulphate. SHBG (50% pellet) and CBG (80% pellet) were then purified by affinity chromatography on tresyl-activated Sepharose with 15-aminopentadecanoic acid (for SHBG) and 1,12-diaminododecane (for CBG) as spacers and 17 zeta-aminoethyl-5 alpha-androstan-3 beta,17-diol (for SHBG) and 17 alpha-hydroxy-4-androsten-3-one-17 beta-carboxylic acid (for CBG) as specific ligands for these two proteins. The eluate was injected into a Mon…
Sensitive Screening of New Psychoactive Substances in Serum Using Liquid Chromatography-Quadrupole Time-of-Flight Mass Spectrometry.
2021
Abstract Analysis of new psychoactive substances (NPS) still poses a challenge for many institutions due to the number of available substances and the constantly changing drug market. Both new and well-known substances keep appearing and disappearing on the market, making it hard to adapt analytical methods in a timely manner. In this study we developed a qualitative screening approach for serum samples by means of liquid chromatography--quadrupole time-of-flight mass spectrometry. Samples were measured in data-dependent auto tandem mass spectrometry mode and identified by fragment spectra comparison, retention time and accurate mass. Approximately 500 NPS, including 195 synthetic cannabino…
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…
Porous zirconia and titania as packing materials for high-performance liquid chromatography
1990
Abstract Porous amorphous zirconia (ZrO 2 ) and titania (TiO 2 ) packings were synthesized as rigid microparticulate beads by means of a sol—gel process. Sufficient rigidity and desired mesoporosity of the ZrO 2 and TiO 2 particles were achieved only by a gel hardening process, followed by heat treatment. The mean pore diameter, p d , the specific surface area, a s , and the specific pore volume, ν p , were controlled by the heat treatment. Typical values were p d = 8 nm, a s = 80 m 2 /g and ν p = 0.23 ml/g. ZrO 2 - and TiO 2 -based revesed-phase packings were prepared by subjecting the native materials to a specific activation process and reaction with octadecyltrimethoxysilane. Native ZrO…
Revisited BIA-MS combination: Entire "on-a-chip" processing leading to the proteins identification at low femtomole to sub-femtomole levels
2008
International audience; We present the results of a study in which biomolecular interaction analysis (BIA, Biacore 2000) was combined with mass spectrometry (MS) using entire "on-a-chip" procedure. Most BIA-MS studies included an elution step of the analyte prior MS analysis. Here, we report a low-cost approach combining Biacore analysis with homemade chips and MS in situ identification onto the chips without elution step. First experiments have been made with rat serum albumin to determine the sensitivity and validation of the concept has been obtained with an antibody/antigen couple. Our "on-a-chip" procedure allowed complete analysis by MS-MS of the biochip leading to protein identificat…
The hydration enthalpies of Md3+ and Lr3+
1988
Lawrencium (3-min 260Lr) and lighter actinides were produced in the bombardment of a 249Bk target with 18O ions and loaded onto a cation exchange column in 0.05 M α-hydroxyisobutyrate solution at pH=4.85, together with the radioactive lanthanide tracers 166Ho, 171Er and 171Tm. In elutions with 0.12 M α=hydroxyisobutyrate solution (pH=4.85), trivalent Lr was eluted exactly together with the Er tracer and Md was eluted close to Ho. Lr elutes much later than expected based on the known elution positions of the lighter actinides and the expected analogy to the elution positions of the homologous lanthanides. From the measured elution positions, ionic radii were calculated for Lr3+ and Md3+. Sem…
Effect of ionization and the nature of the mobile phase in quantitative structure-retention relationship studies.
2005
Abstract The octanol–water distribution constant, commonly called partition coefficient, Po/w, is a parameter often retained as a measure of the hydrophobicity of a molecule. log Po/w, for a given molecule, can be conveniently evaluated constructing correlation lines between standard retention factor logarithms (log k) in reversed-phase liquid chromatography (RPLC) and standard log Po/w values. Many compounds of pharmaceutical interest can be quite hydrophobic and have, simultaneously, basic nitrogen atoms or acidic sulfur containing groups in their structure. This renders them ionizable. The hydrophobicity of the molecular drug form (Po/w value) is completely different from its ionic form …
Effect of sodium dodecyl sulphate and Brij-35 on the analysis of sulphonamides in physiological samples using direct injection and acetonitrile gradi…
2016
Micellar liquid chromatography (MLC) is a reversed-phase (RP) mode, which often does not require gradient elution, since the peaks of mixtures of compounds within a large range of polarities appear more evenly distributed in the chromatograms of isocratic elution, giving rise to a “gradient effect”. However, the use of a gradient of organic solvent may still be convenient to shorten the total analysis time. This work compares the separation of 15 sulphonamides using conventional hydro-organic RPLC and MLC with the surfactants sodium dodecyl sulphate (SDS) and Brij-35, and both isocratic and gradient elution with acetonitrile. The observed behaviour is rationalized attending to the interacti…