Search results for "LIMIT"
showing 10 items of 2826 documents
Analysis of methylamine by solid-phase microextraction and HPLC after on-fibre derivatization with 9-fluorenylmethyl chloroformate
2004
Abstract A method for the determination of methylamine (MA) in aqueous matrices is reported which uses solid-phase microextraction (SPME) for enrichment and derivatization of the analyte, and high performance liquid chromatography (HPLC). The fluorogenic reagent 9-fluorenylmethyl chloroformate (FMOC) has been used for derivatization. The SPME fibres were successively immersed in the samples and in the derivatization solutions to extract MA and FMOC, respectively. After a defined time of reaction, the derivatized analyte was desorbed into the chromatographic system, and chromatographed in a LiChrosphere 100 RP18, 125 mm ×4 mm i.d., 5 μm, column under gradient elution. In order to improve the…
Green determination of eight water-soluble B vitamins in cosmetic products by liquid chromatography with ultraviolet detection.
2021
Abstract B vitamins are a group of compounds with beneficious properties for dermatologic care, and therefore they are included in the cosmetic formulations as high added-value ingredients. In this paper, an analytical method for the simultaneous determination of eight water-soluble B vitamins in cosmetic products is reported for the first time. This method is based on liquid chromatography with ultraviolet detection (LC-UV) analysis after simple water leaching of the analytes from the cosmetic matrix. No organic solvents are required, beyond the ethanol used in the chromatographic mobile phase. The proposed method has been successfully validated showing good linearity, limits of detection …
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…
Determination of 3-(4′-methylbenzylidene)camphor and its metabolite 3-(4′-carboxybenzylidene)camphor in human semen by solid-phase extraction and liq…
2015
An analytical method for the determination of the controversial UV filter 3-(4′-methylbenzylidene)camphor (MBC) and its metabolite 3-(4′-carboxybenzylidene)camphor (CBC) in human semen is presented. The method is based on the simultaneous hydrolysis of phase II conjugates and protein precipitation, followed by solid-phase extraction (SPE) and liquid chromatography tandem mass spectrometry (LC-MS/MS) detection. The proposed method was validated by analyzing spiked analyte-free human semen samples. Matrix-matched calibration using an analyte-free semen pool was employed. Satisfactory recoveries (92–114%) were obtained using this calibration methodology, thus showing the accuracy of the propos…
High-performance liquid chromatographic determination of spironolactone and its major metabolite canrenone in urine using ultraviolet detection and c…
1994
A rapid and simple column liquid chromatographic method involving a column-switching system for the determination of spironolactone and its main metabolite canrenone in urine is described. Purification and concentration was performed using an Hypersil ODS-C18, 30 microns (20 x 2.1 mm I.D.) pre-column. The most polar urinary compounds were removed by washing the pre-column with water, and the analytes were subsequently switched to a LiChrospher RP C18, 5 microns (125 x 4 mm I.D.) analytical column and separated by means of an acetonitrile-water mobile-phase. Under the proposed conditions, the extraction efficiency was approximately 100% over the 0.5-10.0 micrograms/ml concentration range. Th…
Recent developments and future trends in solid phase microextraction techniques towards green analytical chemistry.
2013
Solid phase microextraction find increasing applications in the sample preparation step before chromatographic determination of analytes in samples with a complex composition. These techniques allow for integrating several operations, such as sample collection, extraction, analyte enrichment above the detection limit of a given measuring instrument and the isolation of analytes from sample matrix. In this work the information about novel methodological and instrumental solutions in relation to different variants of solid phase extraction techniques, solid-phase microextraction (SPME), stir bar sorptive extraction (SBSE) and magnetic solid phase extraction (MSPE) is presented, including prac…
New micromethod combining miniaturized matrix solid-phase dispersion and in-tube in-valve solid-phase microextraction for estimating polycyclic aroma…
2008
Abstract Miniaturized matrix solid-phase dispersion (MSPD) was developed for the extraction of common polycyclic aromatic hydrocarbons (PAHs) from bivalve samples (100 mg, dry weight). Additional clean-up and analyte enrichment was accomplished by in-tube solid-phase microextraction (SPME). For this purpose the extracts collected after MSPD were diluted with water and injected into a capillary column coated with the extractive phase. This capillary column was connected to the analytical column by means of a switching valve. Separation and quantification of the PAHs were carried out using a monolithic LC column and fluorescence detection. Since the in-tube SPME device allowed the processing …
Sensitive determination of ethacrynic acid in urine samples by reversed-phase liquid chromatography with ultraviolet detection using solid-phase extr…
1992
Abstract A rapid method is described for the identification and determination of ethacrynic acid in human urine samples by liquid chromatography with UV detection, the retention time of the analyte being 4.9 min. The samples were previously conditioned using C 18 solid-phase extraction columns and chromatographed on an HP-LiChrospher RP C 18 column (5 μm; 125 mm × 4 mm i.d.) with gradient elution with acetonitrile-acetate buffer (pH 4). The detector was set at 275 nm and furosemide was used as an internal standard. The procedure was applied to the determination of ethacrynic acid at concentrations of 0.01-10 μg ml -1 and the limit of detection was 6 ng ml -1 .
On-line trace enrichment for the determination of ethacrynic acid in urine by liquid chromatography and column-switching
1993
Abstract A chromatographic method based on liquid chromatography (LC) using column-switching for the determination of ethacrynic acid in urine samples, is described. The proposed system uses a Hypersil ODS-C18, 30 μm (20 mm × 2.1 mm i.d.) pre-column for the pre-concentration and separation of ethacrynic acid from the biological matrix. Polar urinary compounds are removed by flushing the pre-column with purified water, and the enriched analyte is then switched in back-flush mode onto an HP-LiChrospher RP C18, 5 μm (125 × 4 mm i.d.) analytical column, where it is chromatographed using an acetonitrile-acetate buffer gradient elution. The UV detector was set at 275 nm. The recovery of drug was …
Photo‐Induced Chemiluminometric Determination of Acrolein in a Multicommutation Flow Assembly
2007
Abstract This paper deals with the determination of acrolein based on a strategy provided with a sensitive detection, the chemiluminescence; a “clean chemical” analyte treatment, the on‐line UV‐irradiation; and, a simple and quick automated system, the emergent multicommutation continuous‐flow methodology. The pesticide solution is irradiated (stopped‐flow) for 30 s; then, the resulting solution is introduced to the flow‐cell after being alternated with segments of the stream formed by potassium permanganate in strong acid solution and ethanol segments. The calibration range, from 1 to 1 mg l−1, resulted in a linear behavior over the range 5–100 µg l−1 and fitting the linear equation: I=75.…