Search results for " extraction"

Determination of phenoxy acid herbicides in drinking waters by HPLC and solid phase extraction

1998

Abstract An HPLC procedure for determining phenoxy acid herbicides in waters is described. A LichroSpher RP select B octadecyl-silane analytical column and spectrophotometric detection at 230 nm were used. Adequate retention was achieved with a mobile phase containing MeOH/phosphate buffer 10−2 M pH 2.5/PnOH (50/42/8, v/v). The herbicides were isolated from water samples by using a single solid phase extraction procedure with C18 solid-phase columns. An enrichment factor of 500 is achieved. The coefficients of variation of the method were generally lower than 2.7% at 0.4 μg L−1 herbicide concentration levels. Recoveries ranged between 93 and 118%. The results obtained indicate that the prop…

Near-critical carbon dioxide extraction and liquid chromatography determination of UV filters in solid cosmetic samples: A green analytical procedure

2005

Near-critical carbon dioxide extraction of four UV filters used as sunscreens in lipsticks and makeup formulations is reported. Extraction parameters were optimized. Efficient recoveries were obtained after 15 min of dynamic extraction with a 80:20 CO2/ethanol mixture at 300 atm and 54 degrees C, using a 1.8 mL/min flow rate. Extracts were collected in ethanol, and appropriately diluted with ethanol and 1% acetic acid to obtain a 70:30 v/v ethanol/1% acetic acid solution. The four UV filters were determined by LC with gradient elution using ethanol/1% acetic acid as mobile phase. The accuracy of the analytical procedure was estimated by comparing the results with those obtained by methods b…

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…

Study of polychlorinated biphenyls in street dust by supercritical fluid extraction-gas chromatography/mass spectrometry

1996

Street dust samples have been collected from highways, urban streets, a gasoline station, a pedestrian tunnel, and railway stations in some German cities. Nine polychlorinated biphenyls (PCBs from tri- to heptachlorobiphenyls) were quantitatively extracted by supercritical fluid extraction with CO2 at 200 bar and 40°C and analyzed by gas chromatography/mass spectrometry. The highest PCB loads (sum of the nine studied PCBs) of ca. 1 to 4 μg/g have been found in the samples from motorway A60 near Mainz, while in almost all other samples PCBs could be detected at only ca. 0.1 to 1 μg/g. At three sampling sites, a winter maximum of the PCB concentrations has been found.

Green Analytical Chemistry

2021

Supported liquid membrane extraction of glyphosate metabolites

2001

Use of the supported liquid membrane (SLM) technique for (aminomethyl)phosphonic acid (AMPA) extraction is presented. For the extraction of this analyte a suitable SLM system involves a liquid membrane containing Aliquat 336 – a cationic carrier that facilitates AMPA transport. The extraction of this compound, as in the case of glyphosate, is dependent on the donor phase pH and the concentration and type of counter-ion in the acceptor phase, although some differences are also observed. In both cases the transport mechanism is counter-coupled transport in which the driving force of mass transport over the membrane is created by the gradient of chloride anions from the acceptor to donor phase.

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…