Search results for "Pressure"
showing 10 items of 4493 documents
Homochiral Metal-Organic Frameworks for Enantioselective Separations in Liquid Chromatography
2020
Selective separation of enantiomers is a substantial challenge for the pharmaceutical industry. Chromatography on chiral stationary phases is the standard method, but at a very high cost for industrial-scale purification due to the high cost of the chiral stationary phases. Typically, these materials are poorly robust, expensive to manufacture, and often too specific for a single desired substrate, lacking desirable versatility across different chiral analytes. Here, we disclose a porous, robust homochiral metal–organic framework (MOF), TAMOF-1, built from copper(II) and an affordable linker prepared from natural l-histidine. TAMOF-1 has shown to be able to separate a variety of model…
Interpretive optimisation of organic solvent content and flow-rate in the separation of β-blockers with a Chromolith RP-18e column
2009
The chromatographic performance of a Chromolith RP-18e column was comprehensively examined for a group of basic drugs (beta-blockers), eluted with isocratic ACN-water mixtures at increasing flow-rate up to 6 mL/min. As the flow-rate increases at fixed mobile phase composition, peak distribution (selectivity) is maintained, but the relative peak widths increase. This reduces the resolution below satisfactory values for closely eluting compounds. With the monolithic column, flow-rate becomes thus an important factor to be optimised, in addition to the mobile phase composition. Since, theoretically, retention factors (k) are independent of the flow-rate, the classical quadratic model relating …
Net analyte signal as a deconvolution-oriented resolution criterion in the optimisation of chromatographic techniques
2003
The performance of two multivariate calibration measurements, multivariate selectivity (SEL(s)) and scalar net analyte signal (scalar NAS), as chromatographic objective functions (COFs), was investigated. Since both assessments are straightforwardly related to the quantification of analytes in the presence of interferents, they were expected to confer new features in the optimisation of compound resolution, not present in conventional assessments. These capabilities are especially interesting in situations of low resolution, where peak deconvolution becomes an attractive alternative. For comparison purposes, chromatographic resolution (R(s)) and peak purity (p(s)) were used as reference COF…
Robust interpretive optimisation in high-performance liquid chromatography considering uncertainties in peak position.
2005
In the context of interpretive chromatographic optimisation, robustness is usually calculated by introducing deliberated shifts in the nominal optimal conditions and evaluating their effects on the monitored objective function, mimicking thus the experimental procedures used in method validation. However, such strategy ignores a major source of error: the uncertainties associated to the modelling step, that may give rise to deceiving results when conditions that were expected to yield baseline separation are reproduced in the chromatograph. Two approaches, based on the peak purity concept, are here proposed to evaluate the robustness of the objective function under the perspective of measur…
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.
Critical study of and improvements in chromatographic methods for the analysis of type B trichothecenes
2001
Various analytical methods used in the analysis of type B trichothecenes (deoxynivalenol, nivalenol, 3- and 15-acetyldeoxynivalenol) in cereals were compared and optimised in this work. These methods use either GC-electron-capture detection (ECD) of trimethylsilyl, trifluoroacetyl and heptafluorobutyryl derivatives or HPLC with UV or photodiode array detection of analytes. A new HPLC procedure using fluorescence detection prior derivatisation with coumarin-3-carbonyl chloride has been also tested. Five extraction solvents and two solid-phase extraction cartridges (silica, Florisil) plus a especial clean-up column (MycoSep 225) were compared in order to obtain the best recovery of the mycoto…
Retrospective screening of pesticide metabolites in ambient air using liquid chromatography coupled to high-resolution mass spectrometry
2015
A new methodology for the retrospective screening of pesticide metabolites in ambient air was developed, using liquid chromatography coupled to Orbitrap high-resolution mass spectrometry (UHPLC-HRMS), including two systematic workflows (i) post-run target screening (suspect screening) and (ii) non-target screening. An accurate-mass database was built and used for the post-run screening analysis. The database contained 240 pesticide metabolites found in different matrixes such as air, soil, water, plants, animals and humans. For non-target analysis, a "fragmentation-degradation" relationship strategy was selected. The proposed methodology was applied to 31 air samples (PM10) collected in the…
Liquid/Gas and Liquid/Liquid Phase Behavior of n-Butane/1,4-Polybutadiene versus n-Butane/1,2-Polybutadiene
2005
Solutions of 1,4-polybutadiene (1,4-PB, 98% cis) and of 1,2-polybutadiene (1,2-PB) in n-butane (n-C 4 ) were studied with respect to their vapor pressure and to their demixing into two liquid phases under isochoric conditions within the temperature range from 25 to 75 °C. 1,2-PB mixes homogeneously with n-C 4 at any ratio, in contrast to 1,4-PB, which exhibits a miscibility gap extending from practically pure solvent to approximately 40 wt % polymer. Corresponding to these solubility differences, the vapor pressures for the system n-C 4 /1,4-PB are considerably higher than for n-C 4 /1,2-PB at the same concentration and temperature. The experimental results are modeled accurately and consis…
Pressurized liquid extraction of organic contaminants in environmental and food samples
2015
Pressurized liquid extraction (PLE) is an automated technique that uses elevated temperature and pressure to achieve exhaustive extraction from solid matrices, so reducing solvent consumption and enhancing sample throughput when compared with traditional procedures. Hence, it can be considered an environment-friendly technique, generating small volumes of waste and reducing costs and time. This review focuses on application of this green technique to the analysis of organic contaminants in food and environmental matrices for monitoring purposes. We examine fundamentals and key aspects of the development of a PLE method, including pressurized hot-water extraction, together with some relevant…
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…