Search results for "solid phase"
showing 10 items of 360 documents
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…
Evaluation of C18 adsorbent cartridges for sampling and derivatization of primary amines in air
2004
Abstract The sampling efficiency of C18 solid-phase extraction cartridges was investigated for methylamine, ethylamine, propylamine, butylamine and pentylamine, in air. Determination of these analytes was based on derivatization with o-phthaldialdehyde–N-acetylcysteine (OPA–NAC) on the solid support and fluorescence detection at λexcitation=330 nm and λemission=440 nm of the eluted derivatives. The calibration model derived from aqueous standards was statistically comparable with the calibration model for air standards. Aqueous amines can be used as standards. The method was useful for calculating short-term exposure limits (STEL). A sampling time of 15 min at 30 ml min−1 was employed. Good…
Simultaneous quantification of 18 different phytocannabinoids in serum using a highly sensitive liquid chromatography-tandem mass spectrometry (LC-MS…
2021
Abstract The potential therapeutic effects of various phytocannabinoids and the availability of multiple cannabis-based medicines make it desirable to have an analytical method that simultaneously quantifies a wide range of cannabinoids in blood, beyond delta-9-tetrahydrocannabinol and its metabolites. A liquid chromatography tandem mass spectrometry (LC-MS/MS) method for quantification of 18 phytocannabinoids and cannabinoid metabolites in serum was developed and validated. The method enables simultaneous detection of delta-9-tetrahydrocannabinol, cannabidiol, cannabinol, cannabigerol, cannabichromene, cannabicyclol, tetrahydrocannabivarin and cannabidivarin and their acidic precursors tet…
Analysis of post-harvest fungicides by micellar electrokinetic chromatography.
2001
A method based on solid-phase extraction (SPE) and micellar electrokinetic chromatography (MEKC) was developed for the simultaneous determination of carbendazim, imazalil, methylthiophanate, O-phenylphenol, prochloraz, procimidone, thiabendazole and triadimefon residues in grape, lettuce, orange and tomato. Selectivity and resolution were studied changing the pH and the concentration of the buffer, the type and concentration of surfactant and the methanol content in the mobile phase. A buffer consisting of 4 mM borate with 75 mM sodium cholate (pH 9.2) gave the best results. The recoveries of the fungicides in spiked fruit and vegetable samples ranged from 30 to 105%, and the limits of dete…
On-line preconcentration strategies for analyzing pesticides in fruits and vegetables by micellar electrokinetic chromatography.
2007
Five pesticides (fludioxonil, procymidone, pyriproxyfen, dinoseb and carbendazim) were separated in reversed migration micellar electrokinetic chromatography (RM-MEKC) using 20 mmol l(-1) phosphate buffer at pH 2.3, containing 25 mmol l(-1) sodium dodecylsulfate and 10% methanol. Three on-line concentration strategies, sweeping (SW), normal stacking with reversed migration and a water plug (SRW) and stacking with reverse migration and removal of sample matrix using polarity switching (SRMM), were compared. About 10-, 30- and 50-fold increases in detection sensitivity, compared with standard hydrodynamic injection (5 s at 0.5 psi), were observed with SW, SRW and SRMM, respectively. Limits of…
Improved Solid Phase Extraction Procedure for Assay of Cephalosporins in Human Urine Samples
1998
Abstract Solid phase extraction technique has been evaluated for the treatment of urine samples in the analysis of cephalosporins before injection into an HP-Hypersil ODS-C18 column. Cephalexin, cefotaxime, cefazolin, cefuroxime, and cefoxitin were tested with seven different reversed-phase extraction column cartridges and the obtained urine extracts were not clean. However, 3M Empore extraction disk cartridges packed with octadecyl (C18) bonded silica provided clean extracts with a single extraction. The recoveries of the five cephalosporins ranged from 56 to 60 % in the 1.25–500 g/mL concentration range. The assay was accurate, precise, and adequate for testing the drug content in urine s…