Search results for "Detection limit"
showing 10 items of 810 documents
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…
Ion mobility spectrometry as a fast analytical tool in benzalkonium chloride homologs determination.
2017
Abstract A novel procedure is proposed for the determination by ion mobility spectrometry (IMS) of C 12 , C 14 and C 16 benzalkonium chloride (BAC) homologs. The proposed method requires minimum sample treatment and the measurement was made in less than one minute. A high sensitivity was obtained for BAC determination by IMS with limit of detection values from 37 to 69 µg L −1 . Accuracy of the proposed methodology was evaluated through the analysis of aqueous and alcoholic samples spiked with BAC at concentration levels from 0.002% to 20% (w/v), providing recovery values from 91% to 104%. BAC was determined in sanitary alcohols, nasal sprays, postharvest products, algaecides, and treated s…
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…
Determination of 129I/127I isotope ratios in liquid solutions and environmental soil samples by ICP-MS with hexapole collision cell
2003
The determination of I-129 in environmental samples at ultratrace levels is very difficult by ICP-MS due to a high noise caused by Xe impurities in argon plasma gas (interference of Xe-129(+)), possible (IH2+)-I-127 interference and an insufficient abundance ratio sensitivity of the ICP mass spectrometer for I-129/I-127 isotope ratio measurement. A sensitive, powerful and fast analytical technique for iodine isotope ratio measurements in aqueous solutions and contaminated soil samples directly without sample preparation using ICP-MS with a hexapole collision cell (ICP-CC-QMS) was developed. Oxygen is used as reaction and carrier gas for iodine thermal desorption via the gas phase from solid…