Search results for "LIMIT"
showing 10 items of 2826 documents
Simultaneous determination of third-generation synthetic cannabinoids in oral fluids using cyclodextrin-silica porous sorbents
2022
Abstract A microporous material made of cyclodextrin units covalently immobilized into a silica network has found an innovative bioanalytical application in the sample clean-up and simultaneous isolation of three synthetic cannabinoids (ADB-CHMICA, MMB-CHMICA, and MDMB-CHMCZCA) from human oral fluid through solid-phase extraction. The subsequent quantitation is carried out using liquid chromatography coupled to fluorescence detection. The optimized experimental procedure gives recoveries ranging from 76% to 96% in oral fluid samples spiked with the studied cannabinoids at the µg L-1 level. High selectivity is obtained through the extraction procedure due to the presence of cyclodextrin in t…
Species-Specific GC/ICP-IDMS for Trimethyllead Determinations in Biological and Environmental Samples
2005
An accurate and sensitive species-specific isotope dilution GC/ICPMS method was developed for the determination of trimethyllead (Me3Pb+) in biological and environmental samples. A trimethyllead spike was synthesized from 206Pb-enriched metallic lead by reaction of lead halide with methyllithium and subsequent formation of trimethyllead iodide. The isotopic composition of the spike solution was determined by GC/ICPMS after derivatization with tetraethylborate, and its concentration was determined by reverse isotope dilution analysis. The species-specific GC/ICP-IDMS method was validated by reference material CRM 605 (urban dust) certified for Me3Pb+. The method was also applied to determine…
Methylmercury and inorganic mercury determination in fish by cold vapour generation atomic absorption spectrometry
2000
Abstract Given that organic mercury is more dangerous than the inorganic form and that it is converted into methylmercury by biological methylation, we have studied and optimized a simple method for measuring both organic and inorganic mercury contents in fish, using a spectroscopic vapour generation technique, with a sequential reduction of the digested sample with stannous chloride and sodium tetrahydroborate. Prior to applying the method the sample was subjected to alkaline wet digestion. Due to the matrix interferences calibration curves with matrix addition were needed for mercury determinations. The analytical parameters of the method were: linearity from 10 to 200 ng of Hg in the red…
Chromatographic Separation of Cresol Isomers by a β‐Cyclodextrin: Application for the Determination of Volatile Phenols in Alcoholic Beverages
2006
Abstract The chromatographic separation of o‐cresol, m‐cresol, and p‐cresol by using β‐cyclodextrin as a chiral reagent has been studied. Conditions for the chromatographic separation of these isomers by using the cyclodextrin in the mobile phase or bonded in the stationary phase were optimized, and both procedures provided good results for the resolution of the chromatographic peaks. The use of fluorimetric detection (λexc 275 nm λem 300 nm) allows detection and quantification limits of the µg/L for eight studied phenols by using both procedures. The determination of volatile phenols in alcoholic beverages must be carried out using the cyclodextrin in the mobile phase because of the co‐elu…
Determination of the UV filters worldwide authorised in sunscreens by high-performance liquid chromatography
2001
Simultaneous determination of organic UV filters worldwide authorised in sunscreen formulations was performed by HPLC with UV spectrophotometric detection. The filters determined were: benzophenone-4, benzophenone-3, butyl methoxydibenzoylmethane, octyl dimethyl PABA, octyl methoxycinnamate, homosalate and octyl salicylate. A C18 stationary phase and an isocratic mobile phase of ethanol-water-acetic acid (70:29.5:0.5) containing 65.4 mM of hydroxypropyl-beta-cyclodextrin, were used with a flow-rate of 0.6 ml/min. UV measurements were carried out at 313 nm. The time required for the analysis was 20 min and the limits of detection were between 1.5 and 2.3 mg/l. The procedure proposed provides…
Separation and determination of homologues of linear alkylbenzenesulfonates by nonaqueous capillary zone electrophoresis using alkylammonium salts in…
2001
The separation of linear alkylbenzene sulfonates (LAS) by nonaqueous capillary electrophoresis (NACE) using negative polarity, and a buffer containing acetic acid and an alkylamine in nonaqueous ethanol, has been investigated. Several primary, secondary, and tertiary alkylamines with alkyl chains of different length were compared. The solutes travelled against the electroosmotic flow (EOF), and at the same time were braked by association with the alkylamine molecules or with the alkylammonium ions. The best resolution between adjacent LAS homologues (R approximately 2.1), partial isomer resolution in two peaks, and at the same time an excellent repeatability, was obtained with a small dipen…
Flow-injection spectrophotometric determination of arylamines and sulphonamides by diazotization and coupling in a micellar medium
1991
Abstract In a sodium dodecyl sulphate (SDS) micellar solution, the rate of coupling of a diazonium ion with N-(1- naphthyl)ethylenediamine (NED) increases greatly, the protonation of the resulting azo dyes takes place at higher pH values and the dyes are more soluble. These favourable features were applied to the development of a simple flow-injection spectrophotometric procedure for the determination of diazotizable substances of pharmaceutical interest. Limits of detection in the range 0.2–0.5 μg ml−1 (signal-to-noise ratio=3), with relative standard deviation of 0.7–3% (n=3) for 5 μg ml−1 standards, were obtained.
Determination of sulfide in waters by flow-injection solid phase spectrophotometry
2000
A highly sensitive flow injection solid-phase spectrophotometric method was developed for the determination of sulfide in waters. The method is based on the formation of Methylene Blue (MB) by reaction between sulfide and N,N-dimethyl-p-phenylenediamine chloride in presence of Fe(III) in acidic medium. The MB formed was adsorbed on C18 bonded silica, located inside a laboratory-made flow cell, which was placed in the optical path of the spectrophotometer. Analyte retention and detection at 666 nm were performed simultaneously, followed by elution with a mixture of methanol and hydrochloric acid. Several variables of the system, such as amine concentration, acidity of the reaction medium, re…
Some observations on the automation by flow injection analysis of the spectrophotometric determination of amino acids and proteins witho-phthalaldehy…
1992
Automation by flow injection analysis with Spectrophotometric detection of the determination of total amino acids and proteins witho-phthalaldehyde is not straightforward. The use of spectrophotometry, instead of spectrofluorimetry, and of N-acetyl-L-cysteine, instead of the conventional mercaptoethanol is advantageous because of the lower variability of absorptivities with respect to fluorescence yields, and the larger stability of the derivatives. Under adequate working conditions and with leucine as reference, the procedure can be used for the evaluation of total amino acids. A similar procedure is proposed for the analysis of proteins in a sample. Limits of detection are ≈ 1 × 10−5M for…
Arsenic content of Spanish cows' milk determined by dry ashing hydride generation atomic absorption spectrometry.
1994
SummaryThe arsenic content of cows' milk consumed in Spain was determined. A procedure using dry ashing hydride generation atomic absorption spectrometry was developed for the purpose. Experimental conditions for the destruction of organic matter were established and an interference study was carried out. The method developed has a detection limit of 0·1 ng/g, a relative SD of 5%, and a recovery (mean ± CSI) of 100 ± 4%. The accuracy of the method was checked by analysis of a certified sample of IAEA milk powder (mean ± CSI: certified, 4·85 ± 0·32 ng/g; found, 5·04 ± 0·81 ng/g). The proposed procedure was used to analyse cows' milk samples. The extremely low arsenic levels found do not pres…