Search results for "High Pressure"
showing 10 items of 894 documents
Quantitation of talinolol in rat plasma by LC-MS-MS.
2010
The aim of this study was to develop and validate an assay based on liquid chromatography-tandem mass spectrometry to quantitate talinolol in rat plasma. After a simple protein precipitation step, separation was performed by reversed-phase liquid chromatography using gradient elution with acetonitrile-water-formic acid. Electrospray ionization in the positive ion mode with multiple reaction monitoring was used to analyze talinolol employing propranolol as internal standard. The calibration curve for talinolol was linear over the concentration range 1-250 ng/mL with a correlation coefficient0.995. The method was sensitive (limit of quantitation, 1 ng/mL) and had acceptable accuracy (85-115% …
FTIR determination of Aspartame and Acesulfame-K in tabletop sweeteners.
2004
Two different strategies for sweeteners determination in tabletop samples by Fourier transform middle-infrared (FTIR) spectrometry, an off-line and a fully mechanized extraction of Aspartame and Acesulfame-K with different mixtures of chloroform and methanol, have been developed. The off-line method involves the extraction of both active principles by sonication of samples with 25:75 v/v CHCl3/CH3OH and direct measurement of the peak height values at 1751 cm(-1), corrected using a baseline defined at 1850 cm(-1) for Aspartame, and measurement of the peak height at 1170 cm(-1) in the first-order derivative spectra, corrected by using a horizontal baseline established at 1850 cm(-1), for Aces…
Automated determination of reboxetine by high-performance liquid chromatography with column-switching and ultraviolet detection.
2000
A fully automated method including column-switching and isocratic high-performance liquid chromatography (HPLC) was developed for quantitative analysis of the new antidepressant reboxetine, a noradrenaline reuptake inhibitor. After serum injection into the HPLC system and on-line sample clean-up on a silica C8 (10x4.0 mm I.D.) clean-up column with an eluent consisting of 2.5% acetonitrile in deionized water, the chromatographic separation was performed on an analytical column (Lichrospher CN; 250x4.6 mm I.D.) with an eluent of acetonitrile-aqueous potassium phosphate buffer (0.008 M, pH 6.4) (50:50). The UV detector was set at 273 or 226 nm. The limit of quantification was about 15 ng/ml at…
Determination of abamectin in citrus fruits by liquid chromatography-electrospray ionization mass spectrometry.
2000
Liquid chromatography coupled to electrospray mass spectrometry (LC-ES-MS) with positive ion detection was used to determine abamectin in oranges. MS conditions were optimized to achieve maximum sensitivity. The main ion for abamectin was [M+Na]+ at a fragmentor voltage of 180 V. Abundant structural information can be obtained at different fragmentor voltages. The detection limit for the standard solution was 12 pg injected, and good linearity and reproducibility were observed. Abamectin residues were extracted using matrix solid-phase dispersion. Orange samples were homogenized with C18 bonded silica placed onto a glass column and eluted with dichloromethane. Recoveries of the abamectin fr…
Automated determination of amisulpride by liquid chromatography with column switching and spectrophotometric detection.
2003
A fully automated chromatographic method including on-line blood serum or plasma clean-up, isocratic high-performance liquid chromatography (HPLC) and spectrophotometric detection was developed for quantitative analysis of the new antipsychotic drug amisulpride. After injection of serum or plasma onto the HPLC system and clean-up on a pre-column (10x4.0 mm I.D.) filled with Silica CN 20 micrometer (pore size 10 nm) by an eluent consisting of 8% acetonitrile in deionized water, the chromatographic separation was performed on Lichrospher CN (5 micrometer; 250x4.6 mm I.D.) by an eluent consisting of 50% acetonitrile and 50% aqueous potassium phosphate buffer (0.008 M, pH 6.4). The UV detector …
Selective solid-phase extraction of organophosphorus pesticides and their oxon-derivatives from water samples using molecularly imprinted polymer fol…
2020
Abstract A molecularly imprinted polymer was synthesized and characterized to be used as solid-phase extraction sorbent for simultaneous chlorpyrifos and diazinon and their oxon derivatives. Several imprinted polymers were prepared and evaluated in a retention study of these analytes compared with a non-printed polymer. Several parameters affecting the extraction of imprinted polymer such as washing solvent, composition and volume of the eluting solvent and sample volume, were also investigated. Under the optimum conditions, the developed method provided satisfactory limits of detection ranging between 0.07 µg L−1 to 0.12 µg L−1 and the material showed an excellent reusability (> 50 reuses)…
Evaluation of solid-phase extraction and stir-bar sorptive extraction for the determination of fungicide residues at low-microg kg(-1) levels in grap…
2004
Abstract A liquid chromatography–mass spectrometry method has been developed for determining bitertanol, carboxin, flutriafol, pyrimethanil, tebuconazole and triadimefon. The evaluation of both atmospheric pressure interfaces (API), atmospheric pressure chemical ionization (APCI) and electrospray (ESI) using positive and negative ionization modes, clearly shows that the studied pesticides are more sensitive using APCI in positive mode. Two procedures based on solid-phase extraction (SPE) and stir-bar sorptive extraction (SBSE) have been assessed for extracting these compounds in grape. The recoveries obtained by SPE in samples spiked at the limit of quantification (LOQ) level ranged from 60…
Determination of sulphonamides in human urine by azo dye precolumn derivatization and micellar liquid chromatography
1995
Abstract A high-performance liquid chromatographic method for the determination of sulphonamides in urine is reported. The drugs (sulphadiazine, sulphaguanidine, sulphamethizole, sulphamethoxazole, and sulphathiazole) were diazotized with nitrite and coupled with N-(1-naphthyl)ethylenediamine dihydrochloride in a sodium dodecyl sulphate (SDS) micellar medium. Separation of the sulphonamide azo dyes was performed on a C18 column with a 0.05 M SDS-2.4% pentanol mobile phase, which permitted the direct injection of the urine samples. The limits of detection were in the 0.1–0.3 μg/ml range.
Comparison of different sorbents for on-line liquid-solid extraction followed by high-performance liquid chromatographic determination of nitrogen-co…
1998
Abstract LiChrolut EN [poly(styrene-divinylbenzene), PSDVB], Carbograph (graphitized carbon black, GCB), Isolute CN (cyanopropylsilica), Isolute C 2 (ethylsilica), and LiChrospher RP18 (octadecylsilica) were studied for on-line solid-phase extraction of twelve nitrogen containing pesticides from water. Determination (UV 210 nm) was performed with a Spherisorb C 8 analytical column and an acetonitrile-water gradient. The mean recoveries from 50 ml ranged from 83% for RP18 to 44% for GCB, and decreased in the following order: RP18, CN, LiChrolut EN, C 2 , and GCB. GCB showed poor recoveries due to incomplete desorption with the acetonitrile-water gradient used, and memory effects were detecte…
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…