Search results for "Spectroscopy"
showing 10 items of 10293 documents
Micellar-organic versus aqueous-organic mobile phases for the screening of β-blockers
2002
A comparative study of the performance of reversed-phase liquid chromatography with micellar-organic (MLC) and aqueous-organic (RPLC) mobile phases is reported for the separation of 16 -blockers (acebutolol, alprenolol, atenolol, bisoprolol, carteolol, celiprolol, esmolol, labetalol, metoprolol, nadolol, oxprenolol, pindolol, practolol, propranolol, sotalol, and timolol). MLC with hybrid mobile phases of sodium dodecyl sulfate (SDS) and propanol is revealed as a very competitive technique for the screening of these drugs. Using a conventional Spherisorb C18 column, the theoretical plates ( N) and asymmetry factors (B/A) for the optimal mobile phase compositions were in the ranges N = 2200–4…
Analysis of tricyclic antidepressants in pharmaceuticals by microemulsion liquid chromatography
2021
Abstract Basic compounds yield long retention times and broad and asymmetric peaks in reversed-phase liquid chromatography, due to interaction with residual silanols in the columns. The addition of the surfactant sodium dodecyl sulphate in the so called micellar liquid chromatography enhances the efficiency, but long retention is achieved, due to electrostatic interaction between the cationic species of basic compounds and the anionic sulphate group of the surfactant. This forces the addition of a strong organic solvent to get appropriate times. An alternative is the use of a microemulsion (ME), formed by mixing surfactant, oil and an alcohol as co-surfactant. Association of hydrophobic com…
Solid phase extraction of amines
2005
Abstract The objective of this paper is to provide information about solid phase extraction (SPE) as an alternative to liquid–liquid extraction of amines from several matrices. Different sorbents ranging from non-polar phases, such as C 18 silica to more polar such as cyanopropylsilica (CN) have been tested for analysis of aliphatic amines as monoamines, diamines and polyamines. Phenylalkylamines such as amphetamine or methamphetamine and heterocyclic amines such as histamine or cephalosporins (which also contain a carboxylic group), have also been studied. The different steps involved in the extraction procedure have been tested (conditioning, retention, pre-concentration, washing and elut…
Determination of theophylline and paraxanthine in urine samples by liquid chromatography using the H-point standard additions method
1992
Abstract The simultaneous determination of theophylline and paraxanthine in urine samples by the H-point standard additions method (HPSAM) is described. Samples are extracted with C 18 solid-phase extraction cartridges and chromatographed using a Hypersil C 18 -ODS column and a mobile phase consisting of acetonirile-phosphate buffer in the gradient elution mode. Under these conditions theophylline and paraxanthine are eluted with short retention times. Although their chromatographic peaks are overlapped and their spectra are very similar, the H-point standard additions method provides excellent results in the determination of both xanthines at therapeutic levels.
Chromium(VI) oxide oxidation of non-ethoxylated and ethoxylated alcohols for determination by electrospray ionization mass spectrometry
2010
A new derivatization procedure to increase the sensitivity of electrospray ionization mass spectrometry (ESI-MS) to non-ethoxylated and ethoxylated alcohols was investigated. The analytes were oxidized with chromium(VI) oxide and the resulting carboxylic and ethoxy-carboxylic acids were isolated by extraction with ethyl acetate; the extracts were alkalinized and infused into the ESI-MS system working in the negative-ion mode. The yields of the combined oxidation-extraction were ca. 100% for non-ethoxylated fatty alcohols dissolved in acetone and they decreased moderately in samples containing increasing amounts of water (e.g., a 75% yield was obtained with 50% water). Ethoxylated alcohols w…
Determination of sialic acid and gangliosides in biological samples and dairy products: A review
2009
Gangliosides are sphingolipids containing one or more moieties of sialic acid in their structure. Both gangliosides and sialic acid are bioactive compounds related to animal physiology. Due to their biological relevance, analytical methods adapted to each type of matrix have been developed over time. The present study reviews the main methods applied to the analysis of sialic acid and gangliosides in biological samples and dairy products.
Determination of pyrethroid insecticide residues in vegetable oils by using combined solid-phases extraction and tandem mass spectrometry detection
2005
Abstract A methodology has been developed for the determination of pyrethroid insecticide residues in vegetable oils, based in a solid-phase extraction (SPE) with combined solid supports phases. Several solid phases such as florisil, alumina, C18 and graphitized carbon black were tested in order to minimize fat residues, being a combination of treated alumina and C18 which provided the best results. Oil samples were partitioned with acetonitrile–hexane (1:1) and then eluted through a combined column packed with deactivated basic-alumina and C18, employing the acetonitrile extract as elution solvent. Gas chromatography tandem mass spectrometry was used for determination. Tetramethrin, Bifent…
Continuous-flow spectrophotometric determination of sulfadiazine by diazotisation with in situ preparation of nitrite
1995
Abstract Nitrite is prepared in situ for the determination of sulfadiazine. The method is based on solid-phase reduction of copperized cadmium of nitrate; the nitrite reagent merges with the sample stream in hydrochloric acid medium and the resulting mixture is injected into the water carrier, pure distilled water, and then merges with the N-(1-naphthyl)ethylendiamine reagent and is measured spectrophotometrically at 542.0 nm. The calibration graph is linear over the range 0.5–50 μg ml−1 sulfadiazine, mid-range R.S.D. = 0.3% (n = 5) and sample throughput 72 h−1. The procedure is applied to sulfadiazine determination in a pharmaceutical formulation and to in vitro dissolution studies of two …
Determination of hydroquinone and metal in photographic developer by reversed-phase ion-pair chromatography with amperometric detection
1988
Abstract Sodium 1-heptanesulphonate is used as an ion-pair reagent for the chromatographic separation of the two developing agents on a phenylsilica micro-column, with amperometric detection at an applied potential of + 0.75 V (vs. Ag/AgCl). No pretreatment of the developer is necessary. Linear calibration graphs were obtained in the range 10 −5 -1.5 × 10 −4 M.
Determination of alternative and conventional chelating agents as copper(II) complexes by capillary zone electrophoresis—The first use of didecyldime…
2006
Abstract A capillary zone electrophoresis (CZE) method for analyzing 11 chelating agents [β-alaninediacetic acid (β-ADA), trans-1,2-diaminocyclohexane- N , N , N ′, N ′-tetraacetic acid (CDTA), diethylenetriaminepentaacetic acid (DTPA), ethylenediaminetetraacetic acid (EDTA), N -(2-hydroxyethyl)ethylenediamine- N , N ′, N ′-triacetic acid (HEDTA), N -(2-hydroxyethyl)iminodiacetic acid (HEIDA), iminodiacetic acid (IDA), methylglycinediacetic acid (MGDA), nitrilotriacetic acid (NTA), 1,3-diaminopropane- N , N , N ′, N ′-tetraacetic acid (PDTA) and triethylenetetraaminehexaacetic acid (TTHA)] as negatively charged copper(II) complexes has been established. Both conventional and alternative che…