Search results for "PRESSURE"
showing 10 items of 4493 documents
Sub- and supercritical fluid extraction of trichloropyridinol from soil prior to immunoassay
1997
A comparative study on the extraction of TCP (3,5,6-trichloro-2-pyridinol, a metabolite of chlorpyrifos) from soil with CO2 and H2O is reported. The polarity of the analyte requires the presence of both a cosolvent (methanol) and an ion-pair reagent [(1R)-(-)-10-camphorsulfonic acid ammonium salt] for 95% extraction in 30 min when supercritical CO2 at 40 degrees C and 383 bar is used as extractant. Subcritical water (250 degrees C and 200 bar) enables complete extraction within 15 min without additives. Quantitation of the target analyte is performed by specific immunoassay using a non-commercial monoclonal antibody which provides a linear determination range between 0.005 and 5 micrograms/…
On-Line Derivatization into Precolumns for the Determination of Drugs by Liquid Chromatography and Column Switching: Determination of Amphetamines i…
1996
A chromatographic system for the on-line derivatization of drugs using column switching is described. The system uses a 20 mm × 2.1 mm i.d. precolumn packed with a unmodified ODS stationary phase. This column is used for sample cleanup and enrichment of the analytes. Next, the trapped analytes are derivatized by injection of the derivatization reagent into the precolumn. Finally, the derivatives are transferred to the analytical column for their separation under reversed-phase conditions. The influence of several parameters such as the reaction time, the amount of derivatization reagent, or the system design has been studied using some amphetamines as model compounds and three derivatizatio…
Analytical capabilities of high performance liquid chromatography – Atmospheric pressure photoionization – Orbitrap mass spectrometry (HPLC-APPI-Orbi…
2015
A new analytical method was established and validated for the analysis of 27 brominated flame retardants (BFRs), including so called "emerging" and "novel" BFRs (EBFRs and NBFRs) in fish samples. High performance liquid chromatography (HPLC) coupled to Orbitrap mass spectrometry (Orbitrap-MS) employing atmospheric pressure photoionization (APPI) interface operated in negative mode was used for the identification/quantitation of contaminants. HPLC-Orbitrap-MS analysis provided a fast separation of selected analytes within 14 min, thus demonstrating a high throughput processing of samples. The developed methodology was tested by intralaboratory validation in terms of recovery, repeatability, …
o-Phthalaldehyde–N-acetylcysteine polyamine derivatives: formation and stability in solution and in C18 supports
2001
A comparative study of different derivatization procedures has been performed in order to improve the stability of the reaction products o-phthalaldehyde-N-acetylcysteine (OPA-NAC) polyamines. Procedures such as solution derivatization, solution derivatization followed by retention on a packing support, derivatization on different packing supports and on-column derivatization, have been optimized and compared. The degradation rate constant (k) of the derivative was dependent on the procedure used and on the analyte. For the spermine (the most unstable isoindol tested) k was 8 +/- 2 x 10(-2) min(-1) in solution versus 7.7 +/- 1.1 x 10(-4) min(-1) on the (C18) solid support. The results obtai…
Column-switching techniques for high-performance liquid chromatography of drugs in biological samples.
1993
In recent years, an increasing number of publications have demonstrated the potential of column-switching techniques for the chromatographic separation, determination and preparative isolation of analytes from biological matrices. Column-switching systems greatly facilitate drug analysis, by on-line sample clean-up and trace enrichment, or by improving the analytical separative process. In this paper, the main applications of column-switching techniques to drug analysis in biological samples, are reviewed.
Development and validation of a fast and sensitive chromatographic assay for all-trans-retinol and tocopherols in human serum and plasma using liquid…
2002
A sensitive HPLC assay for all-trans-retinol, alpha-tocopherol, and gamma-tocopherols in human serum and plasma is reported. Sample preparation is performed in one step and involves precipitation of proteins and extraction of lipids with two volumes of an ethanol-chloroform mixture (3:1, v/v) without I.S. addition. After removal of the precipitated protein, 20 microl aliquots of the supernatant (equivalent to 6.7 microl of serum or plasma) were injected into the HPLC system and analyzed using fluorometric detection. RP-HPLC was performed using a C(18) S3 ODS2 column with a methanol-water step gradient (97:3 to 100) at 1.0 ml/min. The quantification limit expressed as nanograms of analyte pe…
Application of solid-phase microextraction combined with derivatization to the enantiomeric determination of amphetamines.
2005
Abstract The utility of combining chiral derivatization and solid-phase microextraction (SPME) for the enantiomeric analysis of primary amphetamines by liquid chromatography has been investigated. Different derivatization/extraction strategies have been evaluated and compared using the chiral reagent o -phthaldialdehyde (OPA)– N -acetyl- l -cysteine (NAC) and fibres with a Carbowax-templated resin coating. Amphetamine, norephedrine and 3,4-methylenedioxyamphetamine (MDA) were used as model compounds. On the basis of the results obtained, a new method is presented based on the derivatization of the analytes in solution followed by SPME of the OPA–NAC derivatives formed. The proposed conditio…
Development of a Rapid Method for the Determination of Phenolic Antioxidants in Dark Chocolate Using Ultra Performance Liquid Chromatography Coupled …
2017
Development of a new comprehensive method based on one-step liquid-liquid extraction (LLE) combined with ultra-high-performance liquid chromatography-Orbitrap high resolution mass spectrometry (UHPLC-Orbitrap-HRMS) for the determination of eight phenolic compounds in dark chocolate is demonstrated. The study focuses on the optimization of sample preparation, chromatographic separation and Orbitrap-HRMS detection parameters to adjust selectivity and sensitivity of the method. The LLE mixture of formic acid-water-acetonitrile (2:58:40, v/v) and hexane at the component ratio of 1:1 (v/v) was applied for sample preparation. The inter-day and intra-day precision expressed from the relative stand…
Evaluation of analytical performance of gas chromatography coupled with atmospheric pressure chemical ionization Fourier transform ion cyclotron reso…
2019
Abstract A new analytical method was established and validated for the analysis of eighteen halogenated flame retardants (HFRs)in food products. Gas chromatography (GC) coupled to Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR-MS) employing atmospheric pressure chemical ionization (APCI) was used for the identification and quantitation of contaminants. Intra-laboratory validation of the method was performed with respect to recovery, repeatability, linear calibration ranges, instrumental and method limits of quantitation (i-LOQ and m-LOQ), and trueness was verified where possible by analysis of reference materials (RMs). The validation results indicated recoveries of ana…
Application of ultra-high pressure liquid chromatography linear ion-trap orbitrap to qualitative and quantitative assessment of pesticide residues
2014
Abstract The analysis of pesticides residues using a last generation high resolution and high mass accuracy hybrid linear ion trap-Orbitrap mass spectrometer (LTQ-Orbitrap-MS) was explored. Pesticides were extracted from fruits, fish, bees and sediments by QuEChERS and from water by solid-phase with Oasis HLB cartridges. Ultra-high pressure liquid chromatography (UHPLC)–LTQ-Orbitrap mass spectrometer acquired full scan MS data for quantification, and data dependent (dd) MS 2 and MS 3 product ion spectra for identification and/or confirmation. The regression coefficients ( r 2 ) for the calibration curves (two order of magnitude up to the lowest calibration level) in the study were ≥0.99. Th…