Search results for " Phase"
showing 10 items of 1862 documents
Determination of tetracyclines in multi-specie animal tissues by pressurized liquid extraction and liquid chromatography–tandem mass spectrometry
2009
Abstract A specific, sensitive and robust pressurized liquid extraction (PLE) and liquid chromatography tandem mass spectrometry (LC–MS/MS) method for determining tetracycline, chlortetracycline, oxytetracycline and doxycycline in bovine, swine, poultry and lamb muscle tissues is presented. PLE was performed using an ASE ® 200 from Dionex and water as extractant, followed by solid-phase extraction (SPE) using an Oasis HLB cartridge. The method was validated for beef, chicken, pork and lamb meat in compliance with the requirements set by Commission Decision, 2002/657/EC [Commission Decision 2002/657/EC (2002). Implementing Council Directive 96/23/EC concerning the performance of analytical m…
A new derivatization procedure for the determination of cephalexin with 1,2-naphthoquinone 4-sulphonate in pharmaceutical and urine samples using sol…
1998
Abstract The present report shows how to derivatize cephalexin with 1,2-naphthoquinone-4-sulphonate (NQS) into solid-phase extraction cartridges (C18) using UV–visible detection. Optimum conditions for this new procedure are: hydrogen carbonate/carbonate buffer pH=10.5, 5 min reaction time at 25°C and NQS concentration of 7.1×10−3 mol l−1. The accuracy and the precision of the method were tested. The procedure was used to measure cephalexin in pharmaceutical and urine samples. The results obtained were contrasted with those reported by UV-spectrophotometric and HPLC methods for pharmaceutical samples and with HPLC method for urine samples. The H-point standard additions method was used to m…
Chromatographic Efficiency in Micellar Liquid Chromatography: Should it Be Still a Topic of Concern?
2013
Micellar liquid chromatography (MLC) was first proposed as an attractive alternative to avoid the use of organic solvents. It was soon apparent that pure micellar solutions yield poor efficiencies. This problem was remediated by the addition of a small amount of an organic solvent. However, the general opinion of the poor peak shape has prevailed as a handicap for MLC, in spite of the fact that the hybrid mode often offers similar or even improved efficiencies (for basic compounds) relative to that attained in the hydro-organic mode. Only the efficiencies for apolar non-ionizable compounds are still clearly inferior. This work describes the type of interactions and polarity changes with org…
Evaluation of extraction alternatives for Fourier transform infrared spectrometric determination of oil and greases in water
1997
Abstract Liquid-liquid extraction (LLE), solid phase extraction (SPE) and microwave-assisted extraction are evaluated for Fourier transform infrared (FTIR) spectrometric determination of oil and grease in polluted waters. A fast microwave-assisted quantitative procedure is proposed for the total extraction of oil and grease into CCl 4 from water samples, with an irradiation time of 1 min at an exit power of 520 W using closed PTFE vessels. The FTIR quantification of oil and grease is carried out by the measurement of the area under the absorbance spectra in the range between 3058 and 2780 cm −1 , with a baseline established between 3200 and 2700 cm −1 . The analytical features of the propos…
Profiling of endogenous peptides by multidimensional liquid chromatography: On-line automated sample cleanup for biomarker discovery in human urine.
2009
A simple and flexible system, employing a column switching technique, has been designed to allow the analysis of peptides and proteins smaller than 15 kDa by molecular weight in filtered urine samples by performing a direct on-column injection utilising simultaneous sample clean-up and trace enrichment. The positively charged peptides and small proteins in the sample are attracted to the inner, negatively charged pore structure of the RAM-SCX column while the larger proteins and uncharged or negatively charged compounds are excluded. After preconditioning with the biological sample, large amounts of sample can be injected. Several important and adjustable parameters for the proper use of a …
Liquid chromatographic determination of aliphatic amines in water using solid support assisted derivatization with 9-fluorenylmethyl chloroformate
2002
A simple and sensitive method has been developed for the liquid chromatographic determination of short-chain aliphatic amines in water. Analytes are retained in solid-phase extraction (SPE) cartridges, and then derivatized by drawing an aliquot of the fluorogeneic reagent 9-fluorenylmethyl chloroformate (FMOC) through the cartridges. After a certain reaction time the derivatives formed are desorbed with acetonitrile. The collected extracts are then chromatographed on a LiChrospher 100 RP18 125 mm×4 mm i.d., 5 μm, column using an acetonitrile-water gradient. The influence of experimental conditions (SPE material, volume of sample, concentration of FMOC, time of reaction and pH) has been inve…
Gas-liquid chromatographic analyses of chlorination products of propionyl chloride
1981
Abstract Photochlorination of propionyl chloride with chlorine in the liquid phase at room temperature gives all eleven chloropropionyl chlorides from the mono-to the pentachloro isomer. The process was investigated every 2 h by gas-liquid chromatography, and the products were identified and estimated as their methyl esters by comparison with model compounds. The isomer distribution of the products was studied in detail. Because the process favours the 3-position, the main components were 3-chloropropionyl chloride up to 15 h, 3,3-dichloropropionyl chloride between 15 and 29 h, 3,3,3-trichloropropionyl chloride between 29 and 56 h and pentachloropropionyl chloride after 56 h of chlorination.
Gas-liquid chromatographic analyses
1984
A mixture of all nine chlorinated 4-hydroxybenzaldehydes and the parent homologue was separated on a non-polar SE-30 capillary column using various isothermal and temperature-programmed operating conditions. The relative retention data for the compounds are given and the retention indices together with the retention index increments for each position of chlorine substitution are examined. The retention order 3-Cl<parent<2,5-di-Cl<2,3-di-Cl<3,5-di-Cl<2-Cl<2,3,5-tri-Cl<2,3,6-tri-Cl<2,6-di-Cl<tetra-Cl isomer obtained indicates that the effect of the position of substitution on the retention behaviour is greater than that of the number of chlorine atoms. The retention is maximal with 2-Cl and 2…
Molecular connectivity as a relevant new tool for predicting analytical behavior: A survey of chemiluminescence and chromatography
2005
Abstract We present a critical presentation and discussion on molecular connectivity applied to analytical fields, giving special attention to predicting the chemiluminescent behavior of pharmaceuticals and pesticides. Molecular connectivity has been largely applied to predict the therapeutic effects of pharmaceuticals and rarely to predictions in analytical chemistry – basically to chromatographic processes and recently to liquid-phase chemiluminescence.
Determination of triazines and organophosphorus pesticides in water samples using solid-phase extraction.
1991
Abstract Octadecyl (C 18 )-bonded porous silica was evaluated for the extraction of triazine and organophosphorus pesticides from natural water. The extraction results showed an effective performance when 1 l of water was passed through small glass columns containing 500 mg of 50–100-μm C 18 bonded porous silica. The absorbed compounds were removed with ethyl acetate, evaporated to 200 μl and determined by gas chromatography. The overall average recoveries were greater than 85% except for dimethoate and trichlorfon. Application of this procedure to the analysis of natural water samples gave results that agree well with those obtained by solvent extraction methods.