Search results for "LIMIT"
showing 10 items of 2826 documents
On-line analysis of carbonyl compounds with derivatization in aqueous extracts of atmospheric particulate PM10 by in-tube solid-phase microextraction…
2011
Abstract A new device for carbonyl compounds based on coupling on-line and miniaturizing both, sample pretreatment and chromatographic separation, is reported. Two capillary columns, a GC capillary column (95% methyl–5% phenyl substituted backbone, 70 cm × 0.32 mm i.d., 3 μm film thickness) in the injection valve for in-tube solid-phase microextraction (IT-SPME) and a Zorbax SB C18 (150 mm × 0.5 mm i.d., 5 μm particle diameter) LC capillary column were employed. Different combinations of IT-SPME and derivatization using 2,4-dinitrophenylhydrazine (DNPH) were examined for mixtures containing 15 carbonyl compounds (aliphatic, aromatic and unsaturated aldehydes and ketones). A screening analys…
Detection of banned drugs in sport by micellar liquid chromatography
1992
Abstract A rapid method for the determination of banned drugs in sport (including stimulants, anabolic steroids and diuretics) based on micellar liquid chromatography is proposed. The mobile phase is an aqueous solution of a surfactant (sodium dodecyl sulphate in this instance) and the stationary phase is octadecylsilica. The retention parameters of the drugs were established and the effect of a mobile phase organic modifier on the chromatographic behaviour of the compounds was studied. Improvements in efficiency were achieved by control of the temperature of the mobile phase. This method allows the direct injection of urine samples for the determination of drugs excreted free in urine: ami…
Determination of nitrogen in hydrolyzed protein formulations by continuous vapour phase FTIR.
2006
An on-line system with vapour generation (VG) and Fourier transform infrared (FTIR) spectrometric detection has been developed for the determination of free ammonium and organic nitrogen in agrochemical formulations containing hydrolyzed proteins. Commercial samples were digested, in batch mode, with sulphuric acid and the obtained solution was alkalinized on-line to transform the NH(4)(+) to NH(3) that was continuously monitored by FTIR. Free ammonium was determined in the same system after simple dilution of undigested samples with water. Different gas phase separators were assayed in order to introduce gaseous NH(3) into a home made IR gas cell of 10 cm pathlength, where the correspondin…
Fluorimetric determination of 1-naphthol and mixtures of carbaryl and 1-naphthol in micellar media
1990
The interaction of 1-naphthol with different types of anionic, cationic and non-ionic surfactants has been studied spectrofluorimetrically in order to obtain a sensitivity enhancement in the determination of this compound. At neutral pH, cetyl trimethyl ammonium bromide (CTAB) provides a 2-fold sensitivity enhancement of 1-naphthol and exhibits a weak interaction with carbaryl. In strong alkaline medium carbaryl is hydrolyzed to 1-naphthol and in the presence of CTAB micells, a 5-fold sensitivity enhancement and a limit of detection of 0.2 μg·ml−1 with a 101±3% percentage of recovery is obtained. These facts permit the development of an accurate method for the fluorimetric analysis of 1-nap…
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…
Determination of Phenol by Preconcentration‐Direct Chemiluminescence in a FIA Assembly
2005
Abstract The determination of phenol in water samples is proposed with the aid of a flow‐injection system. The analytical procedure is based on the direct chemiluminometric emission by oxidation of the analyte with potassium permanganate in acidic medium. The flow assembly is provided with a solid‐phase reactor filled with a resin type XAD‐4 for analyte preconcentration. A large study of potential interferences, namely, amino acids reaching water through degradation of organic matter; metals and inorganic metal ions typically present in water interfering with the CL emission of the parent compound, was performed. The calibration graph was linear over the phenol concentration range 1.0–20.0 …
Analysis of drugs including illicit and new psychoactive substances in oral fluids by gas chromatography-drift tube ion mobility spectrometry
2021
Abstract In this study, a gas chromatograph (GC) has been coupled to a drift tube ion mobility spectrometer (IMS) in order to develop an analytical procedure for the determination of psychoactive substances in oral fluids. Working parameters, including the GC-IMS interface ones, were adjusted in order to obtain sensitive and robust signals. A volume of 500 μL of oral fluid was extracted with 250 μL chloroform and, after centrifugation, were injected into the GC-IMS system. Amphetamine, methylone, α-PVP, ketamine, lidocaine, MPHP, cocaine, THJ-2201, and 5F-ADB were employed as model compounds, providing limits of detection from 6 to 15 μg L−1 and recoveries from 70 to 115% for field oral flu…
Determination of tea tree oil terpenes by headspace gas chromatography mass spectrometry
2016
An alternative procedure was developed for determining quality control of terpenes in tea tree oil commercial samples. The method is based on static headspace gas chromatography mass spectrometry measurements. Absolute limits of detection ranged from 1 ng for p-cymene to 71 ng for terpinen-4-ol. The accuracy of the developed methodology was evaluated by comparing the obtained eucalyptol and terpinen-4-ol concentrations with those provided for a certified sample and by comparing the developed procedure with literature tea tree oil analysis methodology. In the same way, spiked commercial samples provided recovery values ranging between 94% and 100% for all the target analytes with relative st…
Liquid Chromatographic Analysis of Amphetamine and Related Compounds in Urine Using Solid-Phase Extraction and 3,5-Dinitrobenzoyl Chloride for Deriva…
1997
A chromatographic method for the analysis of amphetamine and related compounds in urine using 3,5-dinitrobenzoyl chloride (3,5-DNB) as a labeling reagent is presented. This assay is based on the employment of solid-phase extraction (SPE) cartridges for sample cleanup and derivatization. Experimental conditions are optimized for the simultaneous derivatization of ephedrine, norephedrine, pseudoephedrine, beta-phenylethylamine, amphetamine, methamphetamine, and 3-phenylpropylamine. The derivatives formed are separated in a LiChrospher 1000 RP18 (125 x 4-mm i.d., 5-microns film thickness) analytical column using a water-acetonitrile gradient elution and detected at 254 nm. Derivatization in C1…
Ionic liquid-based single-drop microextraction followed by liquid chromatography-ultraviolet spectrophotometry detection to determine typical UV filt…
2009
Abstract A user-friendly and inexpensive ionic liquid-based single-drop microextraction (IL-SDME) procedure has been developed to preconcentrate trace amounts of six typical UV filters extensively used in cosmetic products (i.e., 2-hydroxy-4-methoxybenzophenone, isoamyl 4-methoxycinnamate, 3-(4′-methylbenzylidene)camphor, 2-ethylhexyl 2-cyano-3,3-diphenylacrylate, 2-ethylhexyl 4-dimethylaminobenzoate and 2-ethylhexyl 4-methoxycinnamate) from surface water samples prior to analysis by liquid chromatography-ultraviolet spectrophotometry detection (LC-UV). A two-stage multivariate optimization approach was developed by means of a Plackett–Burman design for screening and selecting the significa…