Search results for "liquid chromatography"
showing 10 items of 942 documents
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…
Analysis of currently used pesticides in fine airborne particulate matter (PM 2.5) by pressurized liquid extraction and liquid chromatography-tandem …
2008
During and after the application of currently used pesticides (CUPs) a significant fraction of applied pesticides can be lost to the air. A confirmatory and rapid procedure has been developed for the determination of four fungicides (carbendazim, thiabendazol, imazalil and bitertanol), three insecticides (imidacloprid, methidathion and pyriproxyfen), one helicide (methiocarb) and one acaricide (hexythiazox) in fine airborne particulate matter (PM 2.5) at trace level. The proposed method includes extraction of PM 2.5-bound pesticides by pressurized liquid extraction (PLE) followed by a direct injection into LC-MS/MS. The main parameters affecting the performance of the electrospray ionizatio…
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.
Identification of the Biotransformation Products of 2-Ethylhexyl 4-(N,N-Dimethylamino)benzoate
2010
Nowadays, 2-ethylhexyl 4-(N,N-dimethylamino)benzoate (EDP) is one of the most widely used UV filters in sunscreen cosmetics and other cosmetic products. However, undesirable processes such as percutaneous absorption and biological activity have been attributed to this compound. The in vitro metabolism of EDP was elucidated in the present work. First of all, the phase I biotransformation was studied in rat liver microsomes and two metabolites, N,N-dimethyl-p-aminobenzoic acid (DMP) and N-monomethyl-p-aminobenzoic acid (MMP), were identified by GC-MS analysis. Secondly, the phase II metabolism was investigated by means of LC-MS. The investigated reactions were acetylation and glucuronidation …
Simple and sensitive reversed-phase liquid chromatographic assay for analysis of chlorthalidone in urine
1993
Abstract This study describes a rapid method for the determination of chlorthalidone in human urine by reversed-phase liquid chromatography and UV detection at 230 nm, after clean-up over a C8 solid-phase extraction column. Liquid chromatography was carried out on a C18-bonded phase using acetonitrile-phosphate buffer (pH=3) gradient elution. Triamterene was used as internal standard. The system has been applied to the determination of chlorthalidone in the 0.10–10.0 μg/mL concentration interval; the limit of detection was 6 ng/mL.
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…
Supercritical fluid extraction of resveratrol from grape skin of Vitis vinifera and determination by HPLC
2000
Supercritical fluid extraction of resveratrol from grape skin of Vitis vinifera was studied. Extraction variables such pressure, modifier concentration (ethanol), and extraction time were optimised. Final extraction conditions were: 40 degrees C, 150 bar, 7.5% ethanol and extraction time 15 min. Extraction recovery and precision (variation coefficient between 0.2 and 1.0%) were calculated. The resveratrol content in the ethanolic extract was determined by HPLC with UV detection at 306 nm. Acetic acid-methanol-water was used as the mobile phase, and C-18 and C-8 columns were tested, instrumental parameters were optimised, and analytical parameters were calculated (lineal interval 0-75 mg l(-…
Determination of glyphosate and aminomethylphosphonic acid in natural water using the capillary electrophoresis combined with enrichment step
2005
A previously elaborated capillary electrophoresis (CE) method used for the determination of glyphosate and aminomethylphosphonic acid (AMPA) was slightly modified in order to improve the sensitivity. However, detection limits attained (5 μg mL−1 for glyphosate and 4 μg mL−1 for AMPA) were still not satisfactory for analytical purposes, thus the addition of a preconcentration step before the CE analysis was proposed. AMBERLITE®IRA-900, a strong anion-exchange resin, was used to preconcentrate both analytes in environmental aqueous samples. The experimental conditions optimised in a previous work were readapted, by decreasing the eluent concentration due to CE limitations. Satisfactory result…
Determination of carbonyl compounds in particulate matter PM2.5 by in-tube solid-phase microextraction coupled to capillary liquid chromatography/mas…
2013
Abstract In this paper, a new procedure based on in-tube solid phase microextraction (IT-SPME)-capillary liquid chromatography hyphenated to mass spectrometry detection by using microelectrospray ionisation (CapLC–MS), has been reported. The device was proposed to quantify 12 carbonyl compounds (10 aliphatic aldehydes, an unsaturated aldehyde and a ketone) derivatized with 2,4-dinitrophenylhidrazine (DNPH) reagent in aqueous extracts of PM 2.5 . This methodology involves the on-line preconcentration of DNPH-carbonyl compounds derivatives coupled to the CapLC–MS system, efficiently providing appropriate sensitivity for the determination of the target analytes. Detection limits for the analyt…
Determination of the UV filters worldwide authorised in sunscreens by high-performance liquid chromatography
2001
Simultaneous determination of organic UV filters worldwide authorised in sunscreen formulations was performed by HPLC with UV spectrophotometric detection. The filters determined were: benzophenone-4, benzophenone-3, butyl methoxydibenzoylmethane, octyl dimethyl PABA, octyl methoxycinnamate, homosalate and octyl salicylate. A C18 stationary phase and an isocratic mobile phase of ethanol-water-acetic acid (70:29.5:0.5) containing 65.4 mM of hydroxypropyl-beta-cyclodextrin, were used with a flow-rate of 0.6 ml/min. UV measurements were carried out at 313 nm. The time required for the analysis was 20 min and the limits of detection were between 1.5 and 2.3 mg/l. The procedure proposed provides…