Search results for "high-performance liquid chromatography"
showing 10 items of 629 documents
A validated and fast procedure for FTIR determination of Cypermethrin and Chlorpyrifos.
2005
Abstract A FTIR methodology has been developed for the simultaneous determination of Cypermethrin and Chlorpyrifos in pesticide commercially available formulations. The method involves the extraction of both active principles with CHCl3 and direct measurement of the peak area values between 1747 and 1737 cm−1 corrected with a baseline defined at 2000 cm−1 for Cypermethrin and peak height values established at 1549 cm−1 corrected using a baseline situated at 1650 cm−1 for Chlorpyrifos. The limits of detection achieved were of the order of 0.7 and 0.4% (w/w), and the relative standard deviation 0.4 and 0.2% for Cypermethrin and Chlorpyrifos, respectively. The developed procedure provided stat…
A bioluminescence technique for quantitative and structure-associated imaging of pyruvate
2006
A novel bioluminescence assay has been developed for measuring pyruvate within sections of snap-frozen tissue in a quantitative manner as well as with a spatial resolution on a microscopical level. The assay was verified via HPLC and two independent photometric tests. The novel assay makes it possible to determine pyruvate concentrations in cryosections in the range of 0-5.0 micromol/g tissue (dry weight). Based on the analysis of samples of given pyruvate concentrations, the assay exhibits a recovery with a deviationor =15%. The minimal detectable amount was 0.02 pmol based on a 20 microm thick tissue section with an area of 1 cm(2). Combination of the already established imaging biolumine…
The pyrrole moiety as a template for COX-1/COX-2 inhibitors
2000
Aroyl- and thiophene-substituted pyrrole derivatives have been synthesized as a new class of COX-1/COX-2 inhibitors. The inhibition of COX-1 was evaluated in a biological system using bovine PMNLs as the enzyme source, whereas LPS-stimulated human monocytes served as the enzyme source for inducible COX-2. The determination of the concentration of arachidonic acid metabolites was performed by HPLC for COX-1 and RIA for COX-2. Variation of the substitution pattern led to a series of active compounds which showed inhibition for COX-1 and COX-2. Structural requirements for the development of COX-1/COX-2 inhibitors are discussed.
Sensitive determination of aliphatic amines in water by high-performance liquid chromatography with chemiluminescence detection.
2004
A sensitive method has been developed for liquid chromatographic determination of short aliphatic amines in water samples. Analytes are preconcentrated and dansylated on solid sorbents (C18 solid-phase extraction cartridges). The dansyl derivatives are chromatographed and post-column mixed with peroxyoxalate (TCPO) and H2O2 in order to perform chemiluminescence detection. Optimal results have been obtained using a sample volume of 5 ml. The method has been applied to the quantification or screening of several aliphatic amines: methylamine, ethylamine, butylamine, diethylamine, pentylamine and hexylamine. The screening procedure has been developed including also polyamines (putrescine, cadav…
Silver ion chromatography and gas chromatography-mass spectrometry in the structural analysis of cyclic dienoic acids formed in frying oils
1995
The nature of the cyclic monoenoic fatty acids formed from linoleic acid in sunflower oil heated to 275°C has been determined by gas chromatography-mass spectrometry of the picolinyl ester derivatives, before and after hydrogenation and deuteration, and following simplification by silver ion high-performance liquid chromatography. In addition, they were examined by gas chromatography-Fourier transform infrared spectroscopy. Cyclopentene fatty acids (50% of the total monoenes) were formed from C-8 to C-12 and C-10 to C-14 of the original chain in equal amounts with unique stereochemistry. In some isomers the double bond appeared to remain in its original position, and in others it migrated t…
Stability of tacrolimus ophthalmic solution
2017
Purpose The stability of 0.3-mg/mL tacrolimus ophthalmic solution at different storage temperatures was studied. Methods A sterile ophthalmic solution of 0.3 mg/mL tacrolimus was prepared in triplicate under aseptic conditions by diluting tacrolimus in eye drops. Three aliquots of this solution were transferred into polypropylene bottles and stored at 25, 2–8, or −15 to −25 °C. Samples were collected immediately after preparation and at selected time points and assayed in triplicate using high-performance liquid chromatography (HPLC). Samples were also visually examined for macroscopic changes. The 0.3-mg/mL tacrolimus solution was also exposed to acidic treatment and heat to force its degr…
Micellar electrokinetic capillary chromatography for therapeutic drug monitoring of carbamazepine and its main metabolites.
1998
In carbamazepine (CBZ) therapy the concomitant monitoring of concentrations of CBZ and its metabolites is strictly recommended, primarily to avoid toxic side effects. Currently, clinical routine monitoring of CBZ is accomplished by high-performance liquid chromatography or immunological methods. In this study a micellar electrokinetic capillary chromatographic (MECC) method was developed for routine drug monitoring of CBZ and its main metabolites, carbamazepine 10,11-diol and carbamazepine 10,11-epoxide, in human serum or plasma samples. The MECC method enabled baseline separation of all analytes within 2.5 min. The assay revealed sufficient precision and sensitivity and the results of eith…
Automated analysis of quetiapine and other antipsychotic drugs in human blood by high performance-liquid chromatography with column-switching and spe…
2004
Abstract An automated HPLC method with column switching is described for the determination of quetiapine, clozapine, perazine, olanzapine and metabolites in blood serum. After clean-up on silica C8 material (20 μm particle size) drugs were separated on ODS Hypersil C18 material (5 μm; column size 250 mm × 4.6 mm i.d.) within 25 min and quantified by ultraviolet (UV) detection at 254 nm. The limit of quantification ranged between 10 and 50 ng/ml. At therapeutic concentrations of the drugs, the inter-assay reproducibility was below 10%. Analyses of drug concentrations in serum of 75–295 patients treated with therapeutic doses of the antipsychotic drugs revealed mean ± S.D. steady state concen…
Comparison of Dialysis and Dispersion Methods for In Vitro Release Determination of Drugs from Multilamellar Liposomes
2008
The aim of these studies was to compare dialysis and dispersion methods for determining in vitro release of propranolol, metoprolol, pindolol, and atenolol from multilamellar liposomes. Multilamellar vesicles (MLV) were prepared using hydrogenated soy-lecithin phospholipon 90H (Ph 90H) as the primary lipid. The same volume of pH 7.4 phosphate buffered saline was used as a receptor medium for both methods. Samples were withdrawn, and drug concentration was determined using HPLC. All drug-containing liposomes exhibited an initial burst release followed by a slower rate of release. The rate and extent of drug release from MLV was dependent on the physicochemical properties of the drug. For all…
Therapeutic Monitoring of Aripiprazole by HPLC with Column-Switching and Spectrophotometric Detection
2005
Aripiprazole is a novel atypical antipsychotic drug for the treatment of schizophrenia and schizoaffective disorders (1)(2)(3). The drug is metabolized by the cytochrome P450 isoenzymes 3A4 and 2D6 (4). Because of high interindividual variability in the expression of these enzymes, the aripiprazole concentration varies among healthy individuals after administration of the drug (5). In patients, insufficient response or side effects, such as somnolence, akathisia, or nausea, may result from too low or too high drug concentrations. Therapeutic drug monitoring (TDM), which is established practice for many antipsychotic drugs (6)(7), may be helpful for patients treated with aripiprazole. We mea…