Search results for "Analytical"
showing 10 items of 9586 documents
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…
Polymer support synthesis
1989
Non-porous silica gel microbeads of diameter 1.5 microns have been investigated as supports for oligonucleotide synthesis. In the preparation of oligothymidylates of chain length up to 150 bases, with 5'-di-p-anisylphenylmethyl-3'-phosphoramidite as an intermediate, the average yields per chain elongation were up to 99%. Lower overall yields were observed in the case of a support which developed a strong tendency towards aggregation after the build up of an oligonucleotide coating.
Alkylation of acidic organic compounds for gas chromatographic analysis
1973
A new alkylation method is proposed. Organic solutions of fatty acids, phenols or barbituric acids are refluxed with an alkylating reagent and solid K2CO3. The reaction mixture is injected directly into the gas chromatograph. The scope of this convenient method for quantitative and qualitative analyses is considerable as different classes of alkylating agents can be used.
Separation of polycyclic aromatic hydrocarbons under isocratic conditions by a column switching technique
1994
A simple and efficient method of separating a 20-component PAH-mixture (RSM 1647 standard mixture +benzene, toluene, perylene and coronene) by RP-HPLC is described. Separation was by using two Superspher-100 RP-18 cartridges thermostatted at different temperatures under isocratic conditions with water-acetonitrile eluent. The analysis time with complete resolution of all components can be reduced to 15 min.
A micellar liquid chromatographic method for quality control of pharmaceutical preparations containing tricyclic antidepressants
2002
Micellar liquid chromatography methods for quality control of pharmaceutical preparations (capsules, pills, tablets, injections) containing the tricyclic antidepressants amineptine, amitriptiline, clomipramine, doxepin, imipramine, melitracen and nortriptyline alone or together with other CNS drugs like diazepam, medazepam and perphenazine are described. The methods using micellar solutions of cetyltrimethylammonium bromide as mobile phases and UV detection are rapid and reproducible. Due to the versatility of interactions in micellar liquid chromatography, it is possible determine highly hydrophobic compounds such as TCAs in a short time using mobile phases containing low organic solvent c…
Selective solid phase extraction of a drug lead compound using molecularly imprinted polymers prepared by the target analogue approach
2002
Molecularly imprinted polymers have been evaluated at the sample clean-up stage in the analysis of a drug lead compound. In order to circumvent quantification problems related to bleeding of the template, a structurally related analogue of the latter was used. This was selected based on criteria related to interaction site location, solubility, availability and stability of the analogue. Selection of suitable polymerisation conditions was then made using a small batch format (ca. 50 mg) and rapid assessment of binding in the equilibrium mode. It was found that the amount of template could be greatly reduced compared to the conventional protocol, requiring only 5 μmol of template per gram of…
Preparation of monodisperse polyethylene oxides by gel permeation chromatography of discontinuous polymer-homologous series
1970
Abstract Starting from triethylene glycol, monodisperse polyethylene oxides of a molecular weight (MW) up to 2000 (degree of polymerisation (DP) During the first step the ditosylate of triethylene glycol is reacted with the sodium alkoxide of the same diol at room temperature. The condesation product (polymer homologues of triethylene glycol) was separated by molecular distillation and yielded the pure oligomers nonaethylene glycol (DP = 9, MW 414) and pentadecaethylene glycol (DP = 15, MW = 678), as proved by gel chromatography. During the next step the polymer homologues of nonaethylene glycol were synthesised in a similar way. The pure oligomers hepteicosa (DP = 27, MW = 1207) and pentat…
Effect of polystyrene coating on pore, structural and chromatographic properties of silica packings
1990
Abstract A series of mesoporous and macroporous silicas with a mean pore diameter (PD), between 6 and 200 nm were reacted with a copolymer of styrene and vinyl-methyldiethoxysilane. The mass load of coated silicas corresponded to the monolayer capacity of the polymer calculated on the basis of the molecular cross-sectional area, except for the two mesoporous silcias of PD = 6 and 7.5 nm. Depending on the pore size, changes occurred in the specific surface area, as, between the native and the coated product. A comparison of the specific pore volume, νp, of silicas before and after polymer immobilization indicated a major loss of νp for the two mesoporous silicas whereas this effect was much …
Structural selectivity provided by starburst dendrimers as pseudostationary phase in electrokinetic chromatography
1995
Abstract Starburst dendrimers (SBDs) were used as a pseudostationary phase in electrokinetic chromatography (EKC) of hydrophobic compounds. The selectivity of SBD-mediated EKC (SBD-EKC) was different from those in micellar EKC (MEKC) systems, in spite of the apparent structural resemblance between micelles and SBDs. The SBDs provided similar selectivity as polymer gel packing materials in reversed-phase liquid chromatography (RPLC), showing little selectivity for alkyl groups and clear preference for aromatic compounds, especially for rigid, planar polynuclear aromatic hydrocarbons. The alkylation of SBDs resulted in the increased retention and hydrophobic selectivity while maintaining the …
Interactions of the mitochondrial membrane rat liver d-3-hydroxybutyrate dehydrogenase with glass beads during adsorption chromatography
1991
D-3-Hydroxybutyrate dehydrogenase (BDH) is an NAD(+)-dependent dehydrogenase of the mitochondrial inner membrane involved in the energetic balance between the liver and peripheral organs in mammals. It allows the conversion of ketone bodies (acetoacetate and D-3-hydroxybutyrate) and it is one of the best documented lipid-requiring enzymes with a dependence on lecithins. After release of proteins from the membrane by phospholipase A2 treatment of salt-treated mitochondria, the rat liver enzyme is absorbed on controlled-pore glass beads. After batch washing, the enzyme, devoid of lipids (apoBDH), is specifically eluted at pH 8.05-8.15 with a 0.1 M Tris-1 M LiBr buffer under reducing condition…