Search results for "Detection limit"
showing 10 items of 810 documents
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.…
Protein mapping by two-dimensional high performance liquid chromatography.
2000
Current developments in drug discovery in the pharmaceutical industry require highly efficient analytical systems for protein mapping providing high resolution, robustness, sensitivity, reproducibility and a high throughput of samples. The potential of two-dimensional (2D) HPLC as a complementary method to 2D-gel electrophoresis is investigated, especially in view of speed and repeatability. The method will be applied for proteins of a molecular mass <20 000 which are not well resolved in 2D-gel electrophoresis. The 2D-HPLC system described in this work consisted of anion- or cation-exchange chromatography in the first dimension and reversed-phase chromatography in the second dimension. We …
A direct Capillary Liquid Chromatography with electrochemical detection method for determination of phenols in water samples
2010
A fast and direct method based on the use of Capillary Liquid Chromatography (LC) with electrochemical (EC) detection has been described for phenols pollutants in water samples. Concretely, phenol, o-cresol, 2-chlorophenol and bisphenol A have been selected as target analytes. The combination of Capillary LC with EC detection avoided the necessity of preconcentration steps typically used in environmental analysis. The sample injected volume was 2 μL. The achieved detection limits were between 1 and 2 μg/L and the linear dynamic range was up to 50 μg/L for all studied phenols. The precision and uncertainty were satisfactory. The analysis time per sample was 10 min. The proposed procedure has…
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…