Search results for "LIMIT"
showing 10 items of 2826 documents
Sensitive determination of parabens in human urine and serum using methacrylate monoliths and reversed-phase capillary liquid chromatography-mass spe…
2014
A method for the determination of parabens in human urine and serum by capillary liquid chromatography (cLC) with UV-Vis and mass spectrometry (MS) detection using methacrylate ester-based monolithic columns has been developed. The influence of composition of polymerization mixture was studied. The optimum monolith was obtained with butyl methacrylate monomer at 60/40% (wt/wt) butyl methacrylate/ethylene dimethacrylate ratio and 50wt% porogens (composed of 36wt% of 1,4-butanediol, 54wt% 1-propanol and 10wt% water). Baseline resolution of analytes was achieved through a mobile phase of acetonitrile/water in gradient elution mode. Additionally, dispersive liquid-liquid microextraction (DLLME)…
Flow-injection determination of water in organic solvents by near-infrared spectrometry
1993
Abstract A flow-injection (FI) procedure was developed for the direct determination of water in organic solvents by using the O-H stretch absorbance band of water in the near-infrared (NIR) region. Dichloromethane was employed as a test solvent to study the influence of the flow parameters (carrier flow and sample injection volume) and time interval on the sensitivity and repeatability of the FI-NIR measurements. The developed procedure permits the determination of water in dichloromethane and isobutyl methyl ketone samples with limits of detection of 0.01 and 0.005% (v/v), respectively. Real and spiked samples of solvents were analysed by FI-NIR and accurate results were found. The method …
On-line bidirectional electrostacking of chromium(III) and chromium(VI) for flame atomic absorption spectrometry determination
2000
Abstract An on-line bidirectional electrostacking-flow injection-flame atomic absorption spectrometry method has been developed for the simultaneous separation, pre-concentration and determination of Cr(III) and Cr(VI). The electrostacking-flow injection unit was established, the pH and components of the support buffer and sample medium were investigated. Results indicated that the ionic mobility, electric field strength and sample area cross-section are the main influence factors on the electrostacking. The calibration range for both, Cr(III) and Cr(VI), was from 20 to 400 μg l −1 . The limit of detection was 7 μg l −1 for three-times the standard deviation of blank values using a electros…
Microwave-assisted saponification of animal greases for cholesterol determination
1998
Abstract An alternative method for the hydrolysis of cholesterol esters in animal grease samples has been developed. The method consists of the microwave-assisted treatment of 4 g of animal fat or oil with 40 ml of an ethanolic KOH solution inside a 115 ml closed reactor in which samples were irradiated for 2.5 min at 50% power level of an exit power of 700 W. After extraction with petroleum ether and dissolution of the unsaponifiables in toluene, total cholesterol was determined spectrophotometrically by using p-anisidine as a test reagent of the enzymatic reaction of cholesterol through a bienzymic reactor in which cholesterol oxidase and horseradish peroxidase were noncovalently immobili…
Determination of phenolic antioxidants in vegetal and animal fats without previous extraction by dilution with n-propanol and micellar liquid chromat…
1999
Abstract A simple and rapid HPLC method for the determination of phenolic antioxidants (propyl and octyl gallates, tert -butylhydroquinone and 3- tert -butyl-4-hydroxyanisole) in sunflower, corn and olive oils, margarine, lard and butter oil is described. The samples are diluted with n -propanol, filtered and injected; solutions containing 30% (w/w) sample can be injected. The analytes are separated with a C18 column and a micellar mobile phase containing 0.1 M SDS, 2.5% n -propanol and 10 mM phosphate of pH 3, and detected at 290 nm. Calibration curves are linear ( r > 0.9999) and the limits of detection range from 0.2 to 1.3 ng, which correspond to antioxidant concentrations well below t…
Anthrylmethylamine functionalised mesoporous silica-based materials as hybrid fluorescent chemosensors for ATP
2005
A number of functionalised mesoporous solids containing anchored anthrylmethylamine groups have been prepared using different co-hydrolysis or grafting synthetic routes. The solids have been characterised using standard solid-state techniques. Solids with a low loading of the anthrylmethylamine probe show typical well defined and structured emission bands centred at ca. 415 nm. Addition of ATP to suspensions of these solids at pH 2.8 resulted in a quenching of the anthracene emission. These solids showed a cooperative effect that resulted in quite a remarkable improvement in ATP response with respect to the free anthrylmethylamine probe in solution. Certain prepared solids showed a remarkab…
Determination of carbonates in waters by on-line vapor generation FTIR
1998
Abstract An electrically heated gas-permeation unit (GPU) has been employed for the vapor-generation Fourier transform infrared (FTIR) determination of total carbonate in waters. The developed method is based on the simultaneous injection of 100 μ l sample and 100 μ l nitric acid in a two-channel manifold with a merging zone, which provides the generation of CO 2 through the GPU, heated at 90°C, from which CO 2 is swept by a stream of N 2 to a long-path infrared gas cell. Absorbance measurements were made in the range from 2500 to 2150 cm −1 and the corresponding flow injection recordings were obtained as a function of time. The areas of these peaks are interpolated in a calibration equatio…
Gas-chromatographic elemental analysis via di(trifluorethyl)dithiocarbamato-chelates
1986
The capillary-gas-chromatographic conditions for the determination of trace metals after extraction from aqueous solution are optimized by coupling of capillaries and improvement of injection technique. Different detectors (FID and ECD) are tested. pH range and buffer systems for extraction of metal chelates are discussed.
Fourier-transform infrared determination of nicotine in tobacco samples by transmittance measurements after leaching with CHCl3
1998
Abstract A new procedure is proposed for the FT-IR spectrometric determination of nicotine in tobacco. The method is based on the extraction of nicotine in CHCl 3 from tobacco samples, wetted with an aqueous solution of NH 3 (0.1 M), and the measurement of absorbance in the stopped-flow mode at 1316 cm −1 , using a spectral baseline correction established from 1334 to 1300 cm −1 . The procedure developed does not requires a complex sample preparation, and provides a limit of detection of 0.045 mg ml −1 nicotine, a sampling frequency of 3.3 h −1 and a coefficient of variation of 0.3% for five independent measurements of a tobacco sample with a nicotine content of 1.5% w/w. The accuracy of th…
Development of a gas chromatography-mass spectrometry method for the determination of ultraviolet filters in beach sand samples
2014
An analytical method for the determination of eight fat-soluble ultraviolet (UV) filters in beach sand samples is presented for the first time. The method is based on a leaching process of the target compounds from sand samples using vortex mixer agitation and further centrifugation, followed by dispersive liquid–liquid microextraction (DLLME) of the supernatant and gas chromatography-mass spectrometry (GC-MS) analysis of the DLLME extract. The variables involved in the leaching and in the DLLME processes were studied to provide the best enrichment factors. In the first case, the leaching solvent type and volume, and the vortex mixer agitation time were studied. In the case of the DLLME, th…