Search results for "liquid"
showing 10 items of 4351 documents
Multiple-stage mass spectrometric analysis of six pesticides in oranges by liquid chromatography–atmospheric pressure chemical ionization–ion trap ma…
2004
Abstract Six pesticides were determined by liquid chromatography (LC) with positive ion (PI) atmospheric pressure chemical ionization quadrupole ion-trap tandem mass spectrometry (APCI–MS–MS). Ion fragmentation was studied by MS, MS 2 and MS 3 . Fragmentation of the pesticides produced ions formed by various losses from the side-chains and through heterocyclic ring opening, but without any common fragmentation pathway. Multiple reaction monitoring (MRM) of MS, MS 2 and MS 3 was used to identify and quantify the pesticides. The samples were extracted with ethyl acetate and dried over anhydrous sodium sulfate. Comparison of the three MS modes showed that MS 3 is slightly less sensitive but mu…
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…
Analysis of organophosphorus pesticides in honeybee by liquid chromatography-atmospheric pressure chemical ionization-mass spectrometry.
2001
Pesticides applied in extended agricultural fields may be controlled by means of bioindicators, such as honeybees, in which are the pesticides bioaccumulate. Liquid chromatography-atmospheric pressure chemical ionization-mass spectrometry (LC-APCI-MS) experiments with positive (PI) and negative (NI) ion modes were optimized for the analysis of 22 organophosphorus pesticides in honeybee samples. The extraction required 3 g of sample, which was extracted with acetone. The extract was purified with coagulating solution and reextracted with Cl(2)CH(2). Pesticides studied could be detected by both ionization modes except for parathion, parathion-methyl, and bromophos, which did not give signals …
Comparative evaluation of liquid chromatography versus gas chromatography using a β-cyclodextrin stationary phase for the determination of BTEX in oc…
2009
An HPLC method for the determination of benzene, toluene, ethylbenzene and o-xylene, m-xylene and p-xylene in occupational environments was developed and compared with a GC-MS method. Chromatographic analysis using a beta-cyclodextrin stationary phase was performed after active and passive air sampling by adsorption on activated charcoal and pressurized fluid extraction. The analytes were completely separated and quantified using both methods, although GC-MS provided better resolutions and lower detection limits than HPLC. The HPLC method was unsuccessfully applied to the determination of benzene in real samples because its sensitivity was too low. Both methods were applied to the analysis …
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…
Automated Fourier Transform near Infrared Determination of Buprofezin in Pesticide Formulations
2005
An automated procedure has been developed for Fourier transform near infrared (FT-NIR) determination of buprofezin in pesticide formulations. This methodology is based on on-line pesticide extraction with acetonitrile from solid samples and its determination by using peak area absorbance measurements between 2147 and 2132 nm, corrected with a horizontal baseline established at 2091 nm. The repeatability, as a relative standard deviation of five independent analyses of 18.9 mg g−1 of buprofezin, was 0.06% and the limit of detection 5 mg L−1. The reagent consumption was clearly reduced compared with a chromatographic reference procedure from 40.4 mL acetonitrile per sample, required by high …
A simple novel configuration for in-vial microporous membrane liquid–liquid extraction
2009
Abstract A novel arrangement for microporous membrane liquid–liquid extraction from the aqueous donor phase to the organic acceptor phase within a micro-vial, which is compatible with the chromatograph autosampler is presented. The device consisted of a stoppered glass micro-vial containing the organic solvent where the septum of the screw stopper was replaced by a sized piece of membrane which is hermetically assembled to the volumetric flask containing the aqueous donor solution. The placement of the membrane in alternative contact with the solutions was achieved by orbital agitation. As a preliminary study, 2-ethylhexyl 4-(dimethylamino)benzoate has been determined (limit of quantificati…
Determination of water-soluble UV-filters in sunscreen sprays by liquid chromatography.
2002
Abstract Liquid chromatography was used for the determination of the three most used water-soluble UV filters, benzophenone-4 (BZ4), terephthalylidene dicamphor sulfonic acid (TDS), and phenylbenzimidazole sulphonic acid (PBS), in aqueous sunscreen sprays. A C 18 stationary phase and an isocratic mobile phase of EtOH–20 m M sodium acetate buffer of pH 4.6 (30:70, v/v) were used at a flow-rate of 0.5 ml min −1 . Mobile phase was also used as solvent for samples and standards. UV detection was at 313 nm. The analytical run took 5.5 min. The limits of detection were 0.5, 0.9 and 2 μg ml −1 for BZ4, TDS and PBS, respectively. The proposed method does not involve highly toxic solvents.
Determination of atranol and chloroatranol in perfumes using simultaneous derivatization and dispersive liquid-liquid microextraction followed by gas…
2013
Abstract A new analytical method based on simultaneous derivatization and dispersive liquid–liquid microextraction (DLLME) followed by gas chromatography–mass spectrometry (GC–MS), for the determination of the allergenic compounds atranol and chloroatranol in perfumes, is presented. Derivatization of the target analytes by means of acetylation with anhydride acetic in carbonate buffer was carried out. Thereby volatility and detectability were increased for improved GC–MS sensitivity. In addition, extractability by DLLME was also enhanced due to a less polar character of the solutes. A liquid–liquid extraction was performed before DLLME to clean up the sample and to obtain an aqueous sample …
Determination of Parabens in Cosmetics without Previous Extraction by Micellar Liquid Chromatography
1999
A simple and rapid micellar liquid chromatography method for the determination of p-hydroxybenzoic acid esters (methyl-, ethyl-, n-propyl-, and n-butylparaben) in cosmetics (bath foam, milk lotion, hand cream, cream base, and shampoo) is described. The samples are solved with n-propanol, further diluted with more n-propanol or with an aqueous sodium dodecyl sulphate (SDS) micellar solution, and injected. Separations are performed with a micellar mobile phase containing 0.1M SDS, 2.5% n-propanol, 10mM phosphate (pH 3), and with an octadecyl silica column (C 18 ). Calibrations are linear (correlation coefficient r > 0.999) and the limits of detection range from 0.03 to 0.3 ng paraben. The det…