Search results for "Standard addition"
showing 10 items of 72 documents
Comparison of several methods used for the determination of cephalosporins. Analysis of cephalexin in pharmaceutical samples
2002
The precision of UV absorbance of intact and acid degraded cephalosporins, ninhydrin, high performance liquid chromatography and iodometric methods used for analysis of cefoxitin, cefotaxime, cephazolin and cephalexin were compared. To obtain the calibration graphs the analytical signal used were: absorbance, first derivative absorbance, second derivative absorbance and H-point Standard Additions Method by using absorbance values at two selected wavelengths as analytical signal. These methods and calibration graphs were also used for the determination of cephalexin in pharmaceutical samples.
Analyser of chromium and/or cobalt
2003
Abstract Two stopped-flow manifolds have been proposed for individual or simultaneous determination of chromium and cobalt in water samples. Automated procedures based on multicommutation systems have emphasised the differences of their catalytic effect in luminol–hydrogen peroxide chemiluminescence reaction. A more rapid decay of signal was observed for Co for both configurations (flow injection or continuous injection). The influence of chemical and hydrodynamic variables has been studied in order to establish the robustness of method. The analysis rate was lower 1.5 min per replicate. Chemometric tools have been employed for the resolution of their contributions. Partial least squares (P…
Sequential-injection determination of traces of disodium phenyl dibenzimidazole tetrasulphonate in urine from users of sunscreens by on-line solid-ph…
2005
Abstract A sensitive and selective method to determine disodium phenyl dibenzimidazole tetrasulphonate (PDT) in the urine of sunscreen users, which is suitable for studies on body accumulation/excretion is proposed. On-line solid-phase extraction allows the analyte to be retained and subsequentely eluted, using a strong anion exchange (SAX) microcolumn. Standard addition calibration was carried out with only one standard. The wavelengths of excitation and emission were 330 and 454 nm, respectively. The method allows PDT to be determined in both, spiked and unspiked human urine samples, without any pre-treatment. Results obtained for spiked urine samples (40–200 ng ml −1 ) showed the accurac…
A solid-phase extraction liquid chromatography-tandem mass spectrometry method for the percutaneous absorption assessment of 3-(4′-methylbenzylidene)…
2013
The UV filter 3-(4′-methylbenzylidene)camphor (MBC) is a common ingredient in sunscreen cosmetic products. However, different in vitro and in vivo studies suggest that MBC can cause endocrine disrupting effects. This report focuses on the development of an analytical method based on solid-phase extraction (SPE) prior to liquid chromatography tandem mass spectrometry (LC-MS/MS) for the determination of MBC and its main phase I metabolite, named 3-(4′-carboxybenzylidene)camphor (CBC), in urine from users of sunscreen cosmetic products containing MBC. The formation of phase II metabolites (i.e., glucuronide and sulphate conjugates) was also considered by carrying out an enzymatic hydrolysis of…
Development of a fully automated sequential injection solid-phase extraction procedure coupled to liquid chromatography to determine free 2-hydroxy-4…
2010
Abstract 2-Hydroxy-4-methoxybenzophenone and 2-hydroxy-4-methoxybenzophenone-5-sulphonic acid, commonly known as benzophenone-3 (BZ3) and benzophenone-4 (BZ4), respectively, are substances widely used as UV filters in cosmetic products in order to absorb UV radiation and protect human skin from direct exposure to the deleterious wavelengths of sunlight. As with other UV filters, there is evidence of their percutaneous absorption. This work describes an analytical method developed to determine trace levels of free BZ3 and BZ4 in human urine. The methodology is based on a solid-phase extraction (SPE) procedure for clean-up and pre-concentration, followed by the monitoring of the UV filters by…
Determination of aluminum at the parts per billion level by solvent extraction and flame atomic emission spectrometry
1991
A new method for the determination of aluminum at the parts per billion level, by N 2 O/ C 2 H 2 flame emission spectrometry with prior solvent extraction with acetylacetone or 8-hydroxyquinoline in 4-methylpentan-2-one, has been performed. The influence of extraction conditions and instrumental parameters on the sensitivity, precision, and dynamic range of the emission calibration curves have been studied. The limit of detection is between 5 and 10 ppb for both ligands, the variation coefficient being 0.2 and 3% at levels of 75 and 25 ppb, respectively. The method has been applied to the determination of Al in water and the results obtained are compared with those found by the standard add…
Determination of chromium(III) and chromium(VI) in mineral water by bidirectional electrostacking and electrothermal atomic absorption spectrometry
2001
Abstract A feasibility investigation was carried out on the use of bidirectional electrostacking for simultaneous separation and pre-concentration of Cr(III) and Cr(VI) and their electrothermal atomic absorption spectrometry (ETAAS) determination. The bidirectional electrostacking manifold was improved, and the effects of sample tube cross-section and electrostacking time on the pre-concentration factor were investigated. Results indicate that the sample tube cross-section and electrostacking time are the main influence factors on the electrostacking pre-concentration, as well as the electric field strength and ionic mobility. The method developed was suitable for the simultaneous separatio…
Multicommutation Fourier transform infrared determination of benzene in gasoline
2004
A fully mechanized method to determine benzene in motor gasolines has been developed based on the use of Fourier transform infrared spectroscopy (FT-IR) and multicommutation. The flow network comprised a set of three-way solenoid valves and was controlled by means of a microcomputer furnished with an electronic interface and running by a software written in QUICK BASIC 4.5. The flow network and control software were designed to implement the multicommutation approach providing facilities to handle sample and reagent solutions, so that, sample dilution, external calibration and standard addition could be easily performed on-line. The method permits the direct determination of benzene without…
Direct determination of benzene in gasoline by flow-injection Fourier transform infrared spectrometry
1993
Abstract A Fourier transform infrared spectrometric procedure for the automated determination of benzene in gasoline was developed, based on the use of flow-injection analysis. The method permits the direct determination of benzene without any pretreatment of samples, with a limit of detection of 0.02% (v/v) and a relative standard deviation of ca. 1% [for five independent analyses of a diluted sample containing a 0.4% (v/v) of benzene]. Results found by direct analysis agreed with those obtained by off-line and on-line standard addition methods. A rapid quality control procedure was developed, based on the on-line injection of gasoline samples (diluted 1 + 9 in hexane) into a carrier strea…
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 …