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At least 1,765 records · Page 98Linked to original sources
PubMed1996

Off-line high-performance liquid chromatography and solid-phase extraction clean-up for confirmation of pesticide residues in fresh produce by gas chromatography-mass spectrometry.

GC-MS or GC-IT in conjunction with the GC-ECD, GC-FPD and HPLC Post-Column Derivatization for multiresidue scan analyses is a great complementary instrument for identification or confirmation purposes. However, MS in EI mode serves as a non-selective detector that is easily susceptible to interference by produce matrices in trace level residue analysis. The development of an effective clean-up method is essential. In this research, a combination of HPLC/C18 and SPE/Florisil clean-up methods were used to reduce matrices in 10 commodities. Using the PBM system, the reference spectra of the computerized Anaheim data base were fingerprint matched to the fortified residues at the 50 ppb level. For most commodities, the PBM quality value was above 90% with the exception of whole oranges. The study demonstrates that the produce matrix of individual commodities varies considerably. The method met difficulties in the analysis of citrus due to the citrus peels. Although the method is commodity dependent, the clean-up procedure has reduced matrix interference in most cases. Efficiency is approximately in a range of 10(5) to 10(6) times, thus the method is effective in confirming trace level pesticide residues in fresh produce.

Atrazine↗
PubMed1997

Evaluation of two solid-phase extraction procedures for the preconcentration of chlorophenols in drinking water.

Two off-line concentration procedures for the determination of sixteen chlorophenols in drinking water were developed. One involves acetylation of the samples and their subsequent preconcentration over graphitized carbon black cartridges. In the other, chlorophenols are derivatized following preconcentration over cross-linked styrene-divinylbenzene. The two proposed procedures are compared in terms of chlorophenol recoveries, throughput and breakthrough volume of the cartridges. The acetylated derivatives of chlorophenols are determined highly selectively at the concentration levels established by international legislation using gas chromatography in combination with microwave induced plasma atomic emission spectroscopy.

Chlorophenols↗
PubMed1998

Determination of a variety of chemical classes of pesticides in surface and ground waters by off-line solid-phase extraction, gas chromatography with electron-capture and nitrogen-phosphorus detection, and high-performance liquid chromatography with post-column derivatization and fluorescence detection.

Octadecyl (C18)-bonded porous silica was evaluated for the extraction of triazines, organochlorine, carbamates and acidic pesticides from surface and ground water. Gas chromatography with selected detection methods (electron-capture detection, nitrogen-phosphorus detection, mass spectrometry) and liquid chromatography-post-column derivatization fluorescence detection was employed for the determination of 32 pesticides. Recoveries varied from 52 to 102%. The recoveries of triazines obtained using C18 extraction cartridges and conventional liquid-liquid extraction (LLE) are compared. The limit of detection for seventeen organochlorine compounds was better than 0.003 microgram/l and the limit of detection for other 15 analytes was better than 0.06 microgram/l. The proposed analytical methodology was applied to analyze pesticides in surface and ground-water samples of the Lassithi Plateau, Crete, Greece.

Chromatography, Gas↗
PubMed1998

Analysis and degradation study of glyphosate and of aminomethylphosphonic acid in natural waters by means of polymeric and ion-exchange solid-phase extraction columns followed by ion chromatography-post-column derivatization with fluorescence detection.

The quantitative trace determination of glyphosate and its major metabolite, aminophosphonic acid (AMPA) in natural waters was achieved by means of ion-exchange chromatography. Fifty ml of natural water sample was preconcentrated by a two-step procedure: first the sample was percolated through a polymeric cartridge, LiChrolut EN, then through an anion-exchange column mechanism, and finally analyzed by ion-exchange chromatography followed by post-column reaction coupled to a fluorimetric detector. Linear calibration graphs were obtained between 5 and 200 micrograms l-1. Limits of detection ranged from 2 micrograms l-1 of glyphosate and 4 micrograms l-1 of AMPA. A study of the degradation of glyphosate in environmental waters under characteristic conditions was carried out to figure out the main degradation pathways of this compound. Half-lives of glyphosate varied from 60 h for ground water samples exposed to sunlight to 770 h for those stored under dark conditions.

Chromatography, Ion Exchange↗
PubMed1999

On-line solid-phase extraction liquid chromatography-continuous flow frit fast atom bombardment mass spectrometric and tandem mass spectrometric determination of hydrolysis products of nerve agents alkyl methylphosphonic acids by p-bromophenacyl derivatization.

For proof of the presence of chemical warfare agents sarin, soman and VX, a rapid, accurate and sensitive method which allows us to determine their hydrolysis products ethyl methylphosphonic acid, isopropyl methylphosphonic acid and pinacolyl methyl phosphonic acid was explored by using continuous flow frit fast atom bombardment (FAB) LC-MS and LC-MS-MS. After derivatization of analytes with p-bromophenacyl bromide, LC-MS-MS analyses for screening were performed by a flow injection method. The three alkyl methylphosphonic acids (AMPAs) were eluted within 5 min, and the detection limits for the three AMPAs ranged from 1 to 5 ng/ml. For confirmation of the screening results, LC-MS-MS analysis with chromatographic separation was conducted by using a narrow bore column. The three AMPAs were all eluted with excellent separation within 25 min, and the detection limits ranged from 1 to 20 ng/ml. Quantitative measurement was performed by LC-MS in selected ion monitoring (SIM) mode with chromatographic separation. Linear calibration curves were obtained for the three AMPAs and the detection limits ranged from 0.5 to 3 ng/ml. The relative standard deviation for peak area ranged from 3.4 to 6.0% at 50 ng/ml for the three AMPAs.

Chemical Warfare Agents↗
PubMed2000

Analysis of tetrahydro-beta-carboline-3-carboxylic acids in foods by solid-phase extraction and reversed-phase high-performance liquid chromatography combined with fluorescence detection.

The presence and analysis of two tetrahydro-beta-carboline-3-carboxylic acids in foods are studied. Sample preparation with benzenesulfonic acid strong cation-exchange columns followed by RP-HPLC-fluorescence allowed a reliable analysis and spectral characterization of 1,2,3,4-tetrahydro-beta-carboline-3-carboxylic acid (THCA) and 1-methyl-1,2,3,4-tetrahydro-beta-carboline-3-carboxylic acid (MTCA). Experimental data showed that upon oxidation tetrahydro-beta-carboline-3-carboxylic acids gave rise to beta-carbolines (norharman and harman) that were also chromatographically separated and their fluorescent profile monitored. This approach was useful to confirm identification of tetrahydro-beta-carboline-3-carboxylic acids in foods. Several foods and beverages contained THCA and MTCA in varying proportions. Their occurrence in foods implies that diet is a source of these compounds in humans.

Carbolines↗
PubMed2000

Determination of triazine herbicides in natural waters by solid-phase extraction and non-aqueous capillary zone electrophoresis.

Capillary zone electrophoresis (CZE) in an organic medium was used to analyse triazines at sub-ppb concentration levels in natural waters after a preconcentration step using conventional C18 cartridges and new Oasis HLB devices. With both sorbents, satisfactory results were obtained on analysing deionized water. However, on analysing natural waters, both sorbents showed very different types of behaviour. The different variables affecting the elution of both sorbents were studied, resulting in the choice of Oasis HLB as the most suitable for later separation by CZE in non-aqueous medium. Combination of a preconcentration step with electrokinetic injection revealed that capillary electrophoresis with simple UV detection can also be used satisfactorily for the quantification of micropollutants in natural waters. The detection limits obtained varied between 0.01 and 0.05 microg l(-1), depending on the type of matrix analysed. The day-to-day precision varied between 0.9% and 2.3%, expressed as the relative standard deviation.

Electrophoresis, Capillary↗
PubMed2000

High-performance liquid chromatographic determination of morphine and its 3- and 6-glucuronide metabolites by two-step solid-phase extraction.

To provide more accurate measurement of morphine and its metabolites for a study of the genetic differences on morphine response, a method for the analysis of morphine and its metabolites is described which has the advantages of increased sensitivity and specificity by using a cleaner extraction. The new extraction method involves both the hydrophobic isolation on a carbon cartridge and ion-exchange isolation on ion-exchange resin which has not preliminary been described for morphine analysis. The combination of these two steps successfully purified drugs from human plasma with maximum removal of interfering substance comparing with a conventional C18 cartridge alone. The analytes are quantified by high-performance liquid chromatography on a reversed-phase C18 column employing a mobile phase consisting of 25% acetonitrile in 0.05 M phosphate buffer (pH 2.1), and 2.5 mM sodium dodecyl sulfate as the pairing ion with a combination of electrochemical and fluorometric detections. The recoveries for morphine (M), morphine-3-glucuronide (M3G), morphine-6-glucuronide (M6G) and hydromorphone after the SPE procedure were 86+/-7.1%, 82+/-6.9%, 79+/-6.0% and 85+/-6.0%, respectively. Limits of detection for this method are 0.1 ng/ml for M, and 0.18 ng/ml for M3G and M6G. Limits of quantitation were approximately 0.25 ng/ml for M, and 0.45 ng/ml for M3G and M6G. The present assay was applied to measure M, M3G and M6G content in human plasma to test the applicability and suitability of this method for clinical and research use.

Chromatography, High Pressure Liquid↗
PubMed2000

Solid-phase extraction and liquid chromatographic quantitation of quinfamide in biological samples.

This paper describes a high-performance liquid chromatographic method for the assay of quinfamide and its main metabolite, 1-(dichloroacetyl)-1,2,3,4,-tetrahydro-6-quinolinol, in plasma, urine and feces. It requires 1 ml of biological fluid, an extraction using Sep-Pack cartridges and acetonitrile for drug elution. Analysis was performed on a CN column (5 microm) using water-acetonitrile-methanol (40:50:10) as a mobile phase at 269 nm. Results showed that the assay was linear in the range between 0.08 and 2.0 microg/ml. The limit of quantitation was 0.08 microg/ml. Maximum assay coefficient of variation was 14%. Recovery obtained in plasma, urine and feces ranged from 82% to 98%.

Amebicides↗
PubMed2001

Practice of solid-phase extraction and protein precipitation in the 96-well format combined with high-performance liquid chromatography-ultraviolet detection for the analysis of drugs in plasma and brain.

C18 Empore 96-well extraction disc plates have been employed for the analysis of three drugs with different polarities in plasma in conjunction with HPLC-UV, rufinamide, ICL670 and an anticonvulsant agent (AA1) in an early stage of development. With the most polar compound (AA1), ion-pair extraction at pH 12 was applied. The method developed for the assay of AA1 in plasma was applied to its determination in brain using an Oasis HLB plate following homogenisation in a pH 7.4 buffer and protein precipitation with NaOH-ZnSO4, thereby saving time for method development. Protein precipitation in the 96-well format with filtration of the precipitate was applied to the determination of ICL670, a highly protein-bound compound (>99.5%), with a good recovery (78%). Reversed-phase chromatography was applied using a short 5 cm column packed with 3 microm particles for the determination of ICL670 and AA1 and two parallel columns (15 cm long) for the determination of rufinamide. The methods were used routinely, one plate per analysis day being processed, resulting in increase in sample throughput and saving in solvents.

Animals↗
PubMed1988

Isolation of basic drugs from plasma using solid-phase extraction with a cyanopropyl-bonded phase.

The use of a CN sorbent for the isolation of basic compounds from plasma is described. Adsorption from water and plasma was investigated for a test set of 30 basic drugs. It was found that compounds with a carbon chain length greater than or equal to 11 are totally retained and that the competitive effect of the matrix on the adsorption is minimal. Methanol-phosphate buffer (pH 3, mu = 0.05) (50:50) yielded good recoveries for more polar compounds; apolar basic drugs can be efficiently eluted using methanol containing 0.1% propylamine. Water up to 3 ml can be used for the washing step. This approach was applied to the determination of eight drugs in plasma at therapeutic levels. The absolute recoveries (n = 6) obtained were 98.8 +/- 7.3% for papaverine, 82.3 +/- 3.9% for practolol, 83.4 +/- 2.6% for metoclopramide, 87.3 +/- 5.8% for imipramine, 82.8 +/- 3.3% for procaine, 82.7 +/- 4.6% for morphine, 87.5 +/- 7.2% for propranolol and 90.4 +/- 6.2% for yohimbine.

Adsorption↗
PubMed1986

Solid-phase extraction of acetazolamide from biological fluids and subsequent analysis by high-performance liquid chromatography.

A sensitive, relatively fast and simple to operate high-performance liquid chromatographic method for the determination of acetazolamide in plasma and saliva is described. Quantitative extraction of the drug from both plasma and saliva was achieved using commercially available reversed-phase octadecylsilane-bonded silica column (Bond-Elut C18, 2.8 ml capacity). Acetazolamide and the internal standard are retained on the Bond-Elut C18 column and reproducibly recovered by elution with methanol. Liquid-liquid partition chromatography, carried out on a 30-cm mu Porasil column (10-microns porous silica) using a mobile phase consisting of dichloromethane-ethanol-water-glacial acetic acid (500:65:65:1), provided adequate separation with acceptable retention times. Acetazolamide levels in the region 50-100 ng/ml can be determined in 100 microliters of plasma or 200 microliters of saliva employing ultraviolet detection at 254 nm with a sensitivity of 0.005 absorbance units full scale. Although the method is primarily used to determine steady-state drug levels in paediatric patients, its general applicability is illustrated by the 24-h plasma and saliva concentration profiles obtained from a male volunteer following oral administration of acetazolamide.

Acetazolamide↗