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showing 10 items of 3539 documents
Development of standard operation procedures for the manufacture of n-octadecyl bonded silicas as packing material in certified reference columns for…
2004
The development of standard operation procedures for the manufacture of a n-octadecyl bonded spherical silica packing from partially condensed tetraethoxysilane as silica source is described. The synthesis comprises five intermediate products and six synthesis steps which were examined according to their reproducibility and robustness. The results led to the optimisation of the manufacturing process for a n-octadecyl bonded silica. Correlations were drawn between the dynamic viscosity of the poly(ethoxy)siloxane (PES), the synthesis parameters, the resulting pore structural properties and particle size distribution of the silicas. Validated procedures were developed to manufacture spherical…
Determination of Anticonvulsant Drugs in Pharmaceutical Preparations by Micellar Liquid Chromatography
2004
A micellar liquid chromatographic method for quality control of pharmaceutical preparations (capsules, pills, tablets, injections, drops, and suppositories) containing the anticonvulsant drugs acetazolamide, carbamacepine, chlordiazepoxide, diazepam, ethosuximide, phenytoin, phenobarbital, and zopiclone has been developed. This methodology involves the use of micellar solutions of cetyltrimethylammonium bromide (CTAB) as mobile phases and UV detection. The proposed approach is rapid and reproducible. Sample preparation only requires dissolution with micellar solvent and adequate dilution with the mobile phase before injection into the chromatographic system.
Separation of selected peptides by capillary electroendoosmotic chromatography using 3 μm reversed-phase bonded silica and mixed-mode phases
1999
The retention behaviour and selectivity of selected basic, neutral and acidic peptides have been studied by capillary electroendoosmotic chromatography (CEC) with Hypersil C8, C18, Hypersil mixed-mode, and Spherisorb C18/SCX columns, 250 (335) mm x 100 microns, packed with 3 microns particles, and eluted with mobile phases composed of acetonitrile-triethylamine-phosphoric acid (TEAP) at pH 3.0 using a Hewlett-Packard Model HP3DCE capillary electrophoresis system. The selected peptides were desmopressin (D), two analogues (A and B) of desmopressin, oxytocin (O) and carbetocin (C). The peptides eluted either before or after the electroendoosmotic flow (EOF) marker, depending on the concentrat…
Comparative study of Zorbax Bio Series GF 250 and GF 450 and TSK-Gel 3000 SW and SWXL columns in size-exclusion chromatography of proteins.
1988
Abstract A reduction of the mean particle diameter of silica-based packings in the size-exclusion chromatography (SEC) of proteins to about 5 μm generates the expected increase in column plate number over the traditional 10 μm SEC columns, as demonstrated for the Zorbax Bio Series GF 250 and GF 450 and TSK-Gel 3000 SWXL columns. The slightly lower column efficiency of the TSK-Gel 3000 SWXL compared with the GF 250 column is compensated by the fact that the phase ratio of the 3000 SWXL column is higher by a factor of two. Hence both columns show nearly the same peak capacity of about 20–30. When the ionic strength of the eluent was changed by varying the salt concentration, the elution volum…
Enhanced styrene removal in a two-phase partitioning bioreactor operated as a biotrickling filter: Towards full-scale applications
2017
Abstract Styrene vapor abatement was investigated in a two-phase partitioning bioreactor operated as a biotrickling filter (TPPB-BTF). The removal performance of the TPPB-BTF was simultaneously compared with a conventional BTF, which served as a control. Industrial-grade silicone oil was used as the non-aqueous phase in the TPPB-BTF due to its high affinity for styrene. Both bioreactors were operated at styrene inlet concentrations ranging from 55 to 323 mg C m −3 and empty bed residence times (EBRT) of 15–30 s, corresponding to pollutant loading rates of 13–77 g C m −3 h −1 . Both bioreactors exhibited styrene removal efficiencies (REs) higher than 90% at an EBRT of 30 s. Nevertheless, th…
Determination of SiO 2 in lime mud by gravimetry
1999
A simple and rapid method for the determination of SiO2 in lime mud used in current sulfate pulping practice is reported. The lime mud samples are treated three times with 2.5 mL of 6 mol/L hydrochloric acid. The samples are nearly evaporated to dryness two times and the third time to complete dryness. To determine the exact SiO2 content of the residue, it is treated with an excess of concentrated hydrofluoric acid and a little hydrochloric acid, and the silica is expelled as volatile silicon tetrafluoride. The sample treatments take about 1.5 h and the heating periods take a total of about 3.5 h. The SiO2 results were evaluated by analyzing National Institute of Standards and Technology St…
Silica Entrapment for Significantly Stabilized, Energy-Conducting Light-Harvesting Complex (LHCII)
2014
The major light-harvesting chlorophyll a/b complex (LHCII) of the photosynthetic apparatus in green plants consists of a membrane protein and numerous noncovalently bound pigments that make up about one-third of the molecular mass of the pigment-protein complex. Due to this high pigment density, LHCII is potentially interesting as a light-harvesting component in synthetic constructs. However, for such applications its stability needs to be significantly improved. In this work, LHCII was dramatically stabilized by enclosing it within polymerizing colloidal silica. The entrapped LHCII stayed functional at 50 °C for up to 24 h instead of a few minutes in detergent solution and clearly showed e…
Impact of pore structural parameters on column performance and resolution of reversed-phase monolithic silica columns for peptides and proteins
2007
In this work, monolithic silica columns with the C4, C8, and C18 chemistry and having various macropore diameters and two different mesopore diameters are studied to access the differences in the column efficiency under isocratic elution conditions and the resolution of selected peptide pairs under reversed-phase gradient elution conditions for the separation of peptides and proteins. The columns with the pore structural characteristics that provided the most efficient separations are then employed to optimize the conditions of a gradient separation of a model mixture of peptides and proteins based on surface chemistry, gradient time, volumetric flow rate, and acetonitrile concentration. Bo…
Complete decontamination and regeneration of DNA purification silica colum
2008
Silica columns are among the most used DNA purification systems, allowing a good yield of high-quality nucleic acids without organic extractions. Silica column regeneration protocols reported up to now to remove DNA traces are time-consuming, and their effectiveness on genomic DNA has not been demonstrated. Here we report a very rapid regeneration procedure that ensures no DNA carryover, independent of its size, without impairing column efficiency. The method takes advantage of the improved DNA removal by low concentrations of Triton X-100.
Study of conformational effects of recombinant interferon gamma adsorbed on a non-porous reversed-phase silica support.
1995
Abstract Reversed-phase chromatography is a powerful method for separating recombinant interferon γ and one of its analogues differing only by a single amino acid residue. Structural differences of the proteins explain this separation ability as demonstrated from adsorption studies on a non-porous reversed-phase support. To reveal the structural differences occurring in the adsorbed state, two different and independent methods were employed. The variation of the retention with the slope of the linear gradient gave information about the molecular contact area of the protein with the support. For different experimental conditions, these data were correlated with the adsorbent capacities measu…