Search results for "Column chromatography"
showing 10 items of 143 documents
Resveratrol-Related Dehydrodimers: Laccase-Mediated Biomimetic Synthesis and Antiproliferative Activity
2012
Seven resveratrol-related monomeric stilbenoids were submitted to biomimetic oxidative coupling in the presence of laccase from Trametes versicolor (TvL), and gave racemic dihydrobenzofuran dehydrodimers (±)-15 to (±)-21. These products, after spectral characterization, were submitted to an antiproliferative activity bioassay against SW480 human colon cancer cells. Five racemates were found to be active, and were resolved by chiral HPLC. The pure enantiomers were subjected to circular dichroism measurements to establish their absolute configurations at C-7 and C-8. These enantiomerically pure compounds were submitted to the antiproliferative activity assay towards SW480 cells, and were all …
Chemical constituents, total phenolic content, antioxidant activity and bactericidal effect of Dicliptera verticillate (Acanthaceae)
2021
Abstract This study investigated the phytochemical constituents and evaluated the total phenolic content, it also determined the antioxidant and antibacterial activities of the ethanol (EtOH) extract of the whole plant of Dicliptera verticillata. The phytochemical study was carried out using repeated silica gel column chromatography followed by Sephadex LH-20 to purify the extract which afforded three known compounds: lutein (1), shikimic acid (2) and guaiacylglycerol (3). The structures of these compounds were identified after analyses of their NMR and MS data and comparison of these data with those reported in the literature. The antioxidant and antibacterial activities were evaluated by …
Measurement of Duloxetine in Blood Using High-performance Liquid Chromatography with Spectrophotometric Detection and Column Switching
2007
A method using high-performance liquid chromatography (HPLC) with column switching and ultraviolet (UV) spectroscopy was developed for the determination of duloxetine in human plasma. After centrifugation and addition of venlafaxine as internal standard, plasma samples were injected into the HPLC system and precleaned on a column (10 x 4.0 mm) filled with cyanopropyl (CN)-modified silica of 20 microm particle size, with use of 8% (vol/vol) acetonitrile in deionized water as eluent. Duloxetine was eluted and separated on a LiChrospher 100 CN (5-microm particle size; column size, 250 x 4.6 mm I.D.) using acetonitrile-water-potassium dihydrogenphosphate trihydrate buffer (pH, 6.4; 50:50 vol/vo…
Automated determination of clomipramine and its major metabolites in human and rat serum by high-performance liquid chromatography with on-line colum…
1998
A fully automated method including column-switching and isocratic high-performance liquid chromatography (HPLC) was developed for simultaneous determination of the tricyclic antidepressant clomipramine and its metabolites demethylclomipramine, 2-, 8-, and 10-hydroxyclomipramine, 2-, and 8-hydroxydemethylclomipramine and didemethylclomipramine in serum. After serum injection into the HPLC system and on-line sample clean-up on a clean-up column (Hypersil CN; 10 x 4.6 mm) by an eluent consisting of 35% acetonitrile and 65% deionized water, the chromatographic separation was performed on an analytical column (LiChrospher CN; 250 x 4.6 mm I.D.) by an eluent consisting of 38% acetonitrile and 62%…
Determination of microcystins in biological samples by matrix solid-phase dispersion and liquid chromatography–mass spectrometry
2005
A method for the detection and quantification of the microcystins (MCs)-MC-LR, MC-RR and MC-YR-in biological samples by matrix solid-phase dispersion (MSPD) has been developed. The optimum extraction conditions were 500 mg of liver or kidney, C18 bonded silica as dispersant, and a mixture methanol-water (70:30) as eluent. The MCs were determined by liquid chromatography electrospray mass spectrometry (LC/ES/MS). Recoveries of biological extracts at three different spiked levels (1-10 mg kg(-1)) ranged from 40.5 to 87.0% in liver, and from 52.5 to 74.5 in kidney. R.S.D.s were < 15.6% and < 10.6%, respectively. The detection and quantification limits were 0.05 and 0.5 mg kg(-1), for all MCs. …
Sympathetic Nerve Stimulation on the perfused rat heart. Affinities of N-methylatropine and pirenzepine at pre- and postsynaptic muscarine receptors.
1982
Rat isolated hearts with the sympathetic nerves attached were perfused with (-)-3H-noradrenaline in order to label the storage vesicles of the adrenergic nerves. Release was induced either by electrical stimulation of the nerves (3 Hz, 1 min) or by perfusion with high K+ solution (54 mM). The overflow of 3H-noradrenaline and its metabolites was determined by liquid scintillation counting after separation of the compounds by column chromatography. The experimental conditions ensured a minor contribution of 3H-metabolites to the evoked total tritium overflow. The release of 3H-noradrenaline evoked by nerve stimulation or high K+ solution was decreased in the presence of the muscarinic agonist…
Application of matrix solid phase dispersion to the determination of imidacloprid, carbaryl, aldicarb, and their main metabolites in honeybees by liq…
2005
Abstract A method based on matrix solid phase dispersion (MSPD) using C18 as dispersant and dichloromethane–methanol as eluent and liquid chromatography–atmospheric pressure chemical ionization–mass spectrometry (LC–APCI–MS) has been developed for the simultaneous determination of imidacloprid, 6-chloronicotinic acid, carbaryl, aldicarb, aldicarb sulfoxide, and aldicarb sulfone in honeybees. The proposed method was compared with liquid–liquid extraction (LLE) combined with LC–APCI–MS analysis. Spiked blank samples were used as standards to counteract the matrix effect observed in the chromatographic determination. Recovery studies were performed at different fortification levels. Average re…
Nebenreaktionen der radikalisch ausgelösten Cyclisierung von 2,2′-Methylen-bis(4-methyl-1,2-phenylen)-dimethacrylat
1979
2,2′-Methylene-bis(4-methyl-1,2-phenylene) dimethacrylate (1) was reacted with an excess of 2,2′-azoiso-butyronitrile (mole ratio 1:15) highly diluted in boiling benzene. The reaction products were separated by column chromatography. It was found that the 1-cyano-1-methylethyl radical induced the cyclization of 1 to yield the product of a head to tail addition (2) in 55% yield. In addition, the product of a head to head addition (3) was isolated in 4% yield. 35% of 1 reacted in the same way as it has already been observed as suppression of polymerization in the case of p-tolyl methacrylate to give the products 4 and 5. The structures of the products were confirmed by elemental analyses, by …
Rapid determination of ochratoxin A in cereals and cereal products by liquid chromatography.
2004
A new method based on extraction with octylsilica (C8) followed by liquid chromatography coupled with fluorescence detection (LC-FLD) was studied to determine ochratoxin A (OTA) from cereals and cereal products. Optimization of different parameters, such as type and amount of solid phase, type and volume of eluent and amount of sample were carried out. Recovery of OTA from rice samples spiked at 10 ng/g level was of 86% with relative standard deviation of 5%. The limits of detection and quantification of the proposed method were 0.25 and 0.75 ng/g, respectively. Furthermore, LC-FLD after of OTA methylation and liquid chromatography coupled to mass spectrometry with an electrospray interface…
Automated multi-dimensional liquid chromatography
2004
A comprehensive on-line sample clean-up with an integrated two-dimensional HPLC system was developed for the analysis of natural peptides. Samples comprised of endogenous peptides with molecular weights up to 20 kDa were generated from human hemofiltrate (HF) obtained from patients with chronic renal failure. The (poly-)peptides were separated using novel silica-based restricted access materials with strong cation-exchange functionalities (SCX-RAM). The size-selective sample fractionation step is followed by cation-exchange chromatography as the first dimension. The subsequent second dimension of separation is based on hydrophobic interaction using four parallel short reversed-phase (RP) co…