Search results for "Column chromatography"
showing 10 items of 143 documents
Isolation From Human Calcium Oxalate Renal Stones of Nephrocalcin, a Glycoprotein Inhibitor of Calcium Oxalate Crystal Growth. Evidence That Nephroca…
1987
We have determined that the organic matrix of calcium oxalate kidney stones contains a glycoprotein inhibitor ofcalcium oxalate crystal growth (nephrocalcin) that resembles nephrocalcin present in the urine of patients with calcium oxalate stones and differs from nephrocalcin from the urine of normal people. Pulverized calcium oxalate renal stones were extracted with 0.05M EDTA, pH 8.0; nephrocalcin eluted in five peaks using DEAE-cellulose column chromatography, and each peak was further resolved by Sephacryl S-200 column chromatography. Four ofthe fiveDEAE peaks corresponded to those usually found in nephrocalcin from urine; the fifth eluted at a lower ionic strength than any found in uri…
Optimisation of fast protein separations on non-porous silica-based strong anion exchangers
1993
The adsorbed coating technology using various vinylpyrrolidone-vinylimidazole copolymer compositions was carried out on 1.7 μm non-porous monodisperse silica. It was shown that the retention properties and the loading capacity for bovine serum albumin (BSA) increases with the amount of vinylimidazole in the copolymer composition. The retention behavior of various proteins as a function of the salt composition in the eluent has been applied to find the optimal conditions for the synthesis of the anion-exchange stationary phase. The suitability of these supports for the fast separation of biological molecules is demonstrated. The best resolution and the highest speed in protein analysis was o…
Synthesis of Highly Functionalized Cyclopentanes as Precursors of Hydroxylated Azidocarbonucleosides
2009
Regio- and stereoisomers of functionalized azido amino alcohols with a cyclopentane skeleton were synthesized in enantiomerically pure forms. Enzymatic ring cleavage of racemic 2-azabicyclo[2.2.1]hept-5-en-3-one gave the corresponding amino acid and one enantiomer of the lactam stereospecifically. These were protected by esterification and carbamoylation, and then epoxidized. The resulting oxiranes underwent cleavage by sodium azide with complementary stereoselectivities. The regioisomeric products were easily separated by crystallization or column chromatography.
Solution properties of polyelectrolytes. II. Comparison of the effects of both polyion and eluent salt concentrations on the calibrations in aqueous …
1987
The elution behaviour of charged water-soluble polymers (sodium polystyrene sulphonate) in both salt-free and NaCl-containing aqueous mobile phases has been investigated by size-exclusion chromatography. A comparative analysis has been established between the results as a function of polyion and salt concentrations, which demonstrates that the chromatographic behaviour is similar in both cases. The variation of the slopes of the different concentration-dependent calibration curves is discussed in terms of polyelectrolyte conformational changes. Finally, a semi-empirical model has been developed to predict the dependence of the elution volume in either polyion or salt concentration, and its …
Synthesis and pharmacological evaluation of enantiomerically pure endo-configured KOR agonists with 2-azabicyclo[3.2.1]octane scaffold
2021
Conformationally restricted bicyclic KOR agonists 10 with an endo configured amino moiety were synthesized to analyze the bioactive conformation of conformationally flexible KOR agonists such as 2-5. A seven-step, chiral pool synthesis starting with (S)-configured 4-oxopiperidine-2-carboxylate 13 was developed. cis and trans configured diesters 12 were obtained in a 3:1 ratio via hydrogenation of the α,β unsaturated ester 14. After establishment of the bicyclic scaffold, a diastereoselective reductive amination of ketone 11 provided exclusively the endo configured bicyclic amines 10a,b. The 3:1 mixtures of enantiomers were separated by chiral HPLC, respectively, leading to enantiomerically …
Chiroptical inversion of a planar chiral redox-switchable rotaxane.
2019
Reversible redox-switching of a planar chiral [2]rotaxane with a tetrathiafulvalene-bearing crown ether macrocycle generates a complete sign reversal of the main band in the ECD spectrum, as shown by experiment and rationalised by DFT calculations.
A new ceramide from the leaves of Lannea schimperi (Hochst. ex A.Rich.) Engl.
2020
A new ceramide is being reported herein together with six known compounds from the methanol extract of the leaves of Lannea schimperi (Hochst. ex A.Rich.) Engl. The metabolites were obtained through repeated open column chromatography and were characterized by spectroscopic and spectrometric techniques. The radical-scavenging activity of the crude extract and isolated compounds was evaluated using the DPPH radical. The obtained results suggest the studied species as prominent candidate to fight reactive oxygen species (ROS).
Study of silica-structured materials as sorbents for organophosphorus pesticides determination in environmental water samples
2018
Abstract A novel sorbent based on a UVM-7 mesoporous silica doped with Ti has been synthesized and used for solid-phase extraction of several organophosphorus pesticides in environmental water samples followed by gas chromatography coupled to a nitrogen-phosphorus selective detector. Thus, mesoporous silica materials doped with Ti and Fe as well as immobilized cyclodextrin silica-based supports were prepared and morphologically characterized by several techniques such as transmission electronic microscopy, nitrogen adsorption-desorption and X-ray diffraction. These sorbents were comparatively evaluated, and Ti25-UVM-7 material was selected as the best solid phase. After optimization of extr…
Quantitative separation of Trichoderma lipid classes on a bonded phase column.
1992
Bond Elut aminopropyl columns were used to purify the different lipid classes of Trichoderma harzianum and Trichoderma viride. This methodology permitted good separation of the fungal lipid classes in less time than traditional techniques. The incorporation of [1 (14)C]linoleic acid into neutral lipids, free fatty acids and phospholipids was quantified for both strains. The fatty acid profile of the different lipid classes of these fungal strains was determined as a function of culture time.
Simultaneous Automated Determination of Catecholamines, Serotonin, and Their Metabolites in Brain Tissue by HPLC and Electrochemical Detection
1993
Abstract A robust procedure with minimal tissue sample pretreatment, based on reversed-phase, ion-pair high performance liquid chromatography (HPLC) combined with electrochemical detection has been developed for the automated and simultaneous determination of the biogenic amines norepinephrine (NE), epinephrine (E), dopamine (DA), 5-hydroxytryptamine (5-HT) and their metabolites 3-methoxy-4-hydroxyphenylethyleneglycol (MHPG), 3,4-dihydroxyacetic acid (DOPAC), homovanillic acid (HVA) and 5-hydroxyindolacetic acid (H I A A) in as little as 0.5 mg brain tissue. The chromatographic conditions remain stable for at least 8 weeks. In particular small amounts of samples which do not allow reexamina…