Search results for "Solid phase extraction"
showing 10 items of 297 documents
Spectrophotometric determination of phenols in water samples by the GHPSAM method
2001
Abstract The generalized H-point standard-additions method (GHPSAM) is proposed in order to obtain the phenol concentration in water samples when the matrix is completely unknown. The procedure involves solid-phase extraction in BondElut PPL cartridges and data handling of the UV-visible spectrophotometry measurements. The spectral regions where the unknown interferent behaviour can be considered as linear are found and the analyte concentration free from bias error is estimated. The percentages of recovery of phenols in spiked samples were similar to those obtained by HPLC. Cresols or chlorophenols can be also determined in real samples by this method. The concentration range tested was 0.…
Exploring hand-portable nano-liquid chromatography for in place water analysis: Determination of trimethylxanthines as a use case.
2020
Abstract Analytical performance and optimization of figures of merit of a portable nano liquid chromatograph (NanoLC) with UV detection at 255 nm have been established for in place analysis. Methylxanthines: caffeine, theophylline and theobromine were selected as target analytes. A fast lab method based on IT-SPME coupled on line with capillary liquid chromatograph (CapLC) with diode array detection (DAD) was employed for comparative studies. IT-SPME and solid phase extraction were coupled off-line to NanoLC for improving instrumental parameters, mainly detection capacity and selectivity. IT-SPME or SPE/portable NanoLC based methods were superior in terms of chromatographic resolution and o…
Stir bar sorptive-dispersive microextraction mediated by magnetic nanoparticles-nylon 6 composite for the extraction of hydrophilic organic compounds…
2016
A new and sensitive analytical method based on the recently developed approach termed stir bar-sorptive dispersive microextraction (SBSDME) using a magnetic CoFe2O4@SiO2-nylon 6 composite as sorbent material is presented for the extraction of hydrophilic organic compounds. The simultaneous determination of four hydrophilic UV filters in environmental water samples has been chosen as a model analytical application due to the increasing awareness regarding the occurrence of sunscreen residuals in natural waters. The developed SBSDME approach combines the principles and benefits of stir bar sorptive extraction (SBSE) and dispersive solid phase extraction (DSPE) but allows for lower extraction …
Sequential injection analysis for benzophenone-4 and phenylbenzimidazole sulphonic acid in sunscreen sprays by solid-phase extraction coupled with ul…
2002
Abstract A sequential injection UV method was developed to determine benzophenone-4 (BZ4) and phenylbenzimidazole sulphonic acid (PBS) simultaneously, these being the most commonly used UV-filters in aqueous formulations used as sunscreen sprays. The selective elution of both was performed by on-line solid-phase extraction, by retention on a SAX microcolumn and separation by varying the pH of elution. The sensitivity obtained was 0.042±0.001 ml μg −1 for PBS and 0.0159±0.0003 ml μg −1 for BZ4. The limit of detection was 1.6 μg ml −1 for PBS and 0.6 μg ml −1 for BZ4. The R.S.D. of the results was 1–6% for PBS and 1–12% for BZ4. The method was validated using commercial sunscreen formulations…
Urine polyamines determination using dansyl chloride derivatization in solid-phase extraction cartridges and HPLC
1999
The derivatization of biogenic amines such as putrescine, cadaverine, spermidine and spermine with dansyl chloride in solid phase extraction cartridges is described. Different types of filling materials were tested in order to have the highest retention of the different analytes. The best results were obtained by using C18 cartridges. The optimal conditions were: amine solution buffered at pH 12, 2 mM dansyl chloride (acetone-bicarbonate solution 20 mM (pH 9-9.5), 2 + 3 v/v) as reagent concentration, room temperature and 30 min reaction time. The developed procedure was applied to the determination of these polyamines in urine samples from healthy controls and cancer patients using HPLC wit…
Determination of fungicide residues in fruits and vegetables by liquid chromatography–atmospheric pressure chemical ionization mass spectrometry
2002
Abstract A liquid chromatography (LC) method for the quantitative determination of five fungicide residues (dichloran, flutriafol, o -phenylphenol, prochloraz and tolclofos methyl) in oranges, lemons, bananas, peppers, chards and onions is described. The residues were extracted by matrix solid-phase dispersion (MSPD) using C 8 . Quantitative analysis was performed by isocratic LC coupled to quadrupole mass spectrometer using atmospheric pressure chemical ionization in the negative ionization mode. The limit of quantification was 0.01 mg kg −1 for flutriafol, o -phenylphenol and dichloran, and 0.1 mg kg −1 for prochloraz and tolclofos methyl. The MSPD method is also suitable for LC–UV analys…
Determination of carbamate residues in fruits and vegetables by matrix solid-phase dispersion and liquid chromatography-mass spectrometry.
2000
Abstract Thirteen carbamates were analysed in orange, grape, onion and tomatoes by matrix solid-phase dispersion (MSPD) followed by liquid chromatography–mass spectrometry (LC–MS). Electrospray (ES) and atmospheric pressure chemical ionisation (APCI) were compared and both gave similar results in terms of sensitivity and structural information because at 20 V fragmentor voltages the fragmentation is minimal. The efficiency of different solid-phases (C18, C8, cyano, amine and phenyl) for the MSPD was compared. Mean recoveries using C8 varied from 64 to 106% with relative standard deviations of 5–15% in the concentration range of 0.01–10 mg kg−1. Matrix constituents did not interfere signific…
Miniaturized matrix solid phase dispersion procedure and solid phase microextraction for the analysis of organochlorinated pesticides and polybromina…
2009
Abstract This work has developed a miniaturized method based on matrix solid phase dispersion (MSPD) using C18 as dispersant and acetonitrile–water as eluting solvent for the analysis of legislated organochlorinated pesticides (OCPs) and polybrominated diphenylethers (PBDEs) in biota samples by GC with electron capture (GC-ECD). The method has compared Florisil®-acidic Silica and C18 as dispersant for samples as well as different solvents. Recovery studies showed that the combination of C18–Florisil® was better when using low amount of samples (0.1 g) and with low volumes of acetonitrile–water (2.6 mL). The use of SPME for extracting the analytes from the solvent mixture before the injectio…
Fishing for a drug: solid-phase microextraction for the assay of clozapine in human plasma
1999
Solid-phase microextraction (SPME) was investigated as a sample preparation method for assaying the neuroleptic drug clozapine in human plasma. A mixture of human plasma, water, loxapine (as internal standard) and aqueous NaOH was extracted with a 100-micron polydimethylsiloxane (PDMS) fiber (Supelco). Desorption of the fiber was performed in the injection port of a gas chromatograph at 260 degrees C (HP 5890; 30 m x 0.53 mm I.D., 1 micron film capillary; nitrogen-phosphorous selective detection). Fibers were used repeatedly in up to about 75 analyses. The recovery was found to be 3% for clozapine from plasma after 30 min of extraction. However, in spite of the low recovery, the analyte was…
Resin and fatty-acid analysis by solid-phase extraction coupled to atmospheric pressure chemical ionization–mass spectrometry
2007
Using gas-chromatographic analysis, the suitability of liquid–liquid extraction and solid-phase extraction (SPE) methods was studied for the rapid separation of resin and fatty-acid fractions from papermaking process waters. In the second phase of this study, a novel procedure (correlation coefficient >0.99 and repeatability RSD <8%) for on-line monitoring of selected individual acid components (limits of detection 11–78 µg L−1) by SPE combined with atmospheric pressure chemical ionization–mass spectrometry was developed. The suitability of this technique for quality control of papermaking process waters was tested by means of industrial samples. The method was also found suitable for the a…