Search results for "performance liquid chromatography"

Separation of the enantiomers of primary and secondary amphetamines by liquid chromatography after derivatization with (−)-1-(9-fluorenyl)ethyl chlor…

2003

The chiral reagent (−)-1-(9-fluorenyl)ethyl chloroformate (FLEC) has been evaluated for the enantioselective analysis of amphetamines by liquid chromatography. For separation of the FLEC diastereomers conventional reversed-phase conditions were used. The conditions affording the best enantiomeric resolution and sensitivity were determined for amphetamine, methamphetamine, ephedrine, pseudoephedrine, 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxymethamphetamine (MDMA), and 3,4-methylenedioxyethylamphetamine (MDE). All the amphetamines assayed could be separated with resolution factors ranging from 0.91 to 1.92. Although FLEC is typically used as a fluorogenic reagent, it was shown t…

Biopartitioning micellar chromatography to pedict mutagenicity of aromatic amines

2007

[EN] Mutagenicity is a toxicity endpoint associated with the chronic exposure to chemicals. Aromatic amines have considerable industrial and environmental importance due to their widespread use in industry and their mutagenic capacity. Biopartitioning micellar chromatography (BMC), a mode of micellar liquid chromatography that uses micellar mobile phases of Brij35 in adequate experimental conditions, has demonstrated to be useful in mimicking the drug partitioning process into biological systems. In this paper, the usefulness of BMC for predicting mutagenicity of aromatic amines is demonstrated. A multiple linear regression (MLR) model based on BMC retention data is proposed and compared wi…

Extraction of polycyclic aromatic hydrocarbons from cookies: a comparative study of ultrasound and microwave-assisted procedures.

2008

The chromatographic determination of 15 polycyclic aromatic hydrocarbons (PAHs) in cookies has been improved in order to obtain a fast method with a low limit of detection through the combination of microwave-assisted extraction (MAE), oil saponification and solid-phase extraction clean-up before the injection of purified extracts in a C18 201TP52 (5 microm, 250 x 2.1 mm) column. Using acetonitrile-water as mobile phase, with a 50% to 95% w/w acetonitrile gradient for a fixed flow of 0.250 ml min(-1), 15 PAHs were separated in 45 min. The column temperature was maintained at 15 degrees C; and fluorimetric detection was made at a fixed excitation wavelength of 264 nm and emission measurement…

Direct optical resolution of trans-dihydrodiol enantiomers of fjord-region polycyclic aromatic hydrocarbons by high-performance liquid chromatography…

1998

Abstract Enantioselective separation of trans -dihydrodiol metabolites of a series of fjord-region polycyclic aromatic hydrocarbons (PAHs), such as benzo[ c ]phenanthrene and dibenzo[ a , l ]pyrene, was evaluated by HPLC using commercially available cellulose-based CSPs as chiral columns. A baseline separation ( R s ≥1.6) with sharp, well-defined peaks of individual enantiomers was attained using cellulose-tris-( N -3,5-dimethylphenylcarbamate) and n -heptane-ethanol (9:1, v/v) as mobile phase. These chromatographic conditions permit a direct, simple and rapid (mostly within 30 min) enantiomeric resolution of PAH dihydrodiols. CD spectra were obtained for all optically pure enantiomers and …

HPLC study on the ‘history’ dependence of gramicidin A conformation in phospholipid model membranes

1989

AbstractA novel HPLC methodology for the study of gramicidin A reconstituted in model membranes has been tested in comparison with circular dichroism data. It is shown that this chromatographic technique not only corroborates most of the recent spectroscopic results but allows one to explain them in terms of mass fractions of different actual conformational species of GA in the phospholipid assemblies. In particular, the dependence of the inserted peptide configuration on the organic solvent and other parameters involved in the ‘history’ of the sample preparation and handling has been analyzed by HPLC in two phospholipid model systems: small unilamellar vesicles and micelles. Moreover, a sl…

Liquid chromatographic–mass spectrometric determination of post-harvest fungicides in citrus fruits

2001

Liquid chromatography (LC)-atmospheric pressure ionisation (API)-mass spectrometry (MS) has been used to determine residues of five fungicides in oranges with a minimum sample cleanup. Atmospheric pressure chemical ionisation (APCI) and electrospray (ES) were compared and both gave similar results in terms of sensitivity and structural information. The main ions were [M+H]+ for carbendazim, imazalil, thiophanate methyl and thiabendazole, and [M+H-C4H9NHCO]+ for benomyl. Samples were extracted with sodium sulphate and ethyl acetate. Although benomyl and thiophanate methyl were transformed through the extraction procedure to carbendazim, the method showed good precision (13%) and recovery (70…

Comparison of several methods used for the determination of cephalosporins. Analysis of cephalexin in pharmaceutical samples

2002

The precision of UV absorbance of intact and acid degraded cephalosporins, ninhydrin, high performance liquid chromatography and iodometric methods used for analysis of cefoxitin, cefotaxime, cephazolin and cephalexin were compared. To obtain the calibration graphs the analytical signal used were: absorbance, first derivative absorbance, second derivative absorbance and H-point Standard Additions Method by using absorbance values at two selected wavelengths as analytical signal. These methods and calibration graphs were also used for the determination of cephalexin in pharmaceutical samples.

Determination of pharmaceutical residues in wastewater using high performance liquid chromatography coupled to quadrupole-Orbitrap mass spectrometry

2016

Abstract A multi-class method for the determination of 24 emerging pharmaceutical residues has been developed and validated. The method is based on solid-phase extraction of wastewater samples using Strata-X cartridges followed by high performance liquid chromatography coupled to hybrid quadrupole − Orbitrap high resolution mass spectrometry (HPLC-Q-Orbitrap-HRMS). A single-laboratory validation procedure showed satisfactory analytical performance. The analysis of 21 samples collected at the wastewater treatment plant in Riga revealed the occurrence of 20 compounds of different therapeutic classes. The highest concentration was found for the central nervous system stimulator caffeine − up t…

Reversed Phase Liquid Chromatography

2015

On-line high-pressure extraction-high-performance liquid chromatography

1983

Abstract A coupling unit is described that allows on-line operation of a high-pressure extraction apparatus with a high-performance liquid chromatograph. The unit consists of two high-pressure sample-injection valves, connected in series. The first valve operates as a switching valve to the loop and controls the release of pressure along a packed microbore column. Two short, packed microbore columns are positioned between the first and second valve, sampling the extracted compounds over a desired period and simultaneously operating as sample loop for the second valve; the latter is the injector for the high-performance liquid chromatographic column. The unit was tested by continuous extract…