Search results for "performance"
showing 10 items of 4457 documents
Analysis of LSD in human body fluids and hair samples applying ImmunElute columns.
2000
Immunoaffinity extraction units (LSD ImmunElute) are commercially available for the analysis of lysergic acid diethylamide (LSD) in urine. The ImmunElute resin contains immobilized monoclonal antibodies to LSD. We applied the ImmunElute procedure to serum and also to human hair samples. For hair analysis the samples were first extracted with methanol under sonication. The extracts were then purified using the ImmunElute resin. LSD analysis was carried out with HPLC and fluorescence detection. The immunoaffinity extraction provides highly purified extracts for chromatographic analysis. The limit of detection (signal-to-noise ratio = 3) has been determined to be < 50 pg regardless of which sa…
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…
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…
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…
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 …
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…
Automated high-performance liquid chromatographic determination of amphetamine in biological fluids using column-switching and on-column derivatizati…
1999
A rapid and simple liquid-chromatographic method has been developed for on-line quantification of amphetamine in biological fluids. Untreated samples (20 μL) are injected directly into the chromatographic system and purified on a 20 mm×2.1 mm i.d. pre-column packed with 30 μm Hypersil C18 stationary phase. After clean-up the analyte is transferred to the analytical column (125 mm×4 mm i.d., 5 μm LiChrospher 100 RP18) for derivatization and separation using a mixture of acetonitrile and the derivatization reagent (o-phthaldialdehyde andN-acetyl-L-cysteine) as the mobile phase. The experimental conditions for on-line derivatization and resolution of the amphetamine have been optimized, and th…
Improving analysis of apolar organic compounds by the use of a capillary titania-based column: Application to the direct determination of faecal ster…
2010
This article reports a new procedure for the direct determination of faecal sterols coprostanol and cholesterol in wastewater samples as tracers of human sewage contamination. The method combines in-tube solid-phase microextraction (IT-SPME) for analyte enrichment and capillary liquid chromatography (LC) for separation with diode array detection for identification and quantification. A titania-based polymeric capillary column and a conventional octadecyl silica (ODS) capillary column were evaluated and compared for their ability to separate the analytes. The titania-based column allowed the separation of the analytes in much shorter chromatographic times and with better chromatographic prof…
Spectrophotometric determination of phenols in water samples by the GHPSAM method
2001
Abstract The generalized H-point standard-additions method (GHPSAM) is proposed in order to obtain the phenol concentration in water samples when the matrix is completely unknown. The procedure involves solid-phase extraction in BondElut PPL cartridges and data handling of the UV-visible spectrophotometry measurements. The spectral regions where the unknown interferent behaviour can be considered as linear are found and the analyte concentration free from bias error is estimated. The percentages of recovery of phenols in spiked samples were similar to those obtained by HPLC. Cresols or chlorophenols can be also determined in real samples by this method. The concentration range tested was 0.…