Search results for "Solid phase extraction"
showing 10 items of 297 documents
Organochlorine residue analysis of commercial milks by capillary gas chromatography
1991
The determination of organochlorine pesticides and polychlorinated biphenyls in milks requires the use of efficient extraction methods. A rapid procedure has been developed, based on extraction of organochlorine residues from milk on to octadecylsilica solid phase extraction cartridges and elution with hexane. The addition of different organic solvents to the milk before solid phase extraction has been studied. The use of methanol to disrupt the fat globules enables almost complete recovery of the residues with minimum extraction of fatty substances. Recovery experiments were performed for eighteen compounds present at ppb levels in whole, two per cent, and skimmed milks. The average recove…
Extraction of clenbuterol from calf urine using a molecularly imprinted polymer followed by quantitation by high-performance liquid chromatography wi…
2002
A method for the extraction of clenbuterol from calf urine samples using a molecularly imprinted polymer (MIP) has been developed. The aim was that the final extracts from the MIP should allow quantitation of clenbuterol down to 0.5 ng/mL urine using HPLC with UV detection. The MIP was produced using brombuterol as a template and the selectivity of the MIP, for clenbuterol, was tested against a non-imprinted polymer (produced without template) and was found to be high. After loading of 5 mL diluted centrifuged urine, selective binding was established in acetonitrile-acetic acid (98:2). For further elution of interferences, 0.5 M ammonium acetate buffer pH 5 and 70% acetonitrile in water was…
Solid-Phase Extraction Techniques for Assay of Diuretics in Human Urine Samples
1991
Abstract Solid-phase extraction techniques were evaluated for the treatment of urine samples in the analysis of diuretics before injection into an HP-Hypersyl ODS-C18 column. Six different reversed-phase extraction columns were tested, and the results obtained are compared with those obtained in a classical liquid-liquid extraction with ethyl acetate. The solid-phase extraction procedures are the best overall choice for all the diuretics tested, due to their versatility, the minor time-consuming, and the good recovery percentages obtained. C18 and C8 packings give the highest recoveries for a majority of the diuretics studied. However, CH or PH columns, due to their greater selectivity, can…
Green Analytical Chemistry
2021
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…
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…
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.