Search results for "COLUMN"

Usted no, señor Kissinger

2001

El capitalismo, contra el planeta / 2

2007

Determination of barbiturates in urine by micellar liquid chromatography and direct injection of sample.

2000

Abstract A liquid chromatographic procedure for the determination of six barbiturates (barbital, diallyl barbituric acid, phenobarbital, butabarbital, amobarbital and pentobarbital) in urine samples is described. The proposed system uses a Spherisorb octadecyl-silane ODS-2 C 18 analytical column and a guard column of similar characteristics. The UV detector was set at 240 nm. A study to select adequate composition of the micellar mobile phase for the separation of these compounds in urine samples is performed. Maximum resolution was achieved with a 0.07 M sodium dodecylsulphate-0.3% propanol at pH 7.4 eluent. Limits of detection at 240 nm were ranged between 0.13 μg ml −1 for diallyl barbit…

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…

Procedure for automated background correction in flow systems with infrared spectroscopic detection and changing liquid-phase composition

2009

This paper describes a partial least squares (PLS) based automatic procedure to correct for changes in the spectral contribution of the solvent or solvent mixtures from solute spectra recorded in these solvents. The procedure was developed for successful on-line Fourier transform infrared (FT-IR) detection in gradient high-performance liquid chromatography (HPLC) separations. It requires a reference FT-IR data set containing all possible combinations of the expected variation in solvent composition. Furthermore, a spectral region ( A) in these spectra is required where the solvents show absorption but the analytes do not. This is the case for the system ACN:H2O, an often-applied solvent mi…

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.

Optimisation of gradient elution with serially-coupled columns. Part I: single linear gradients.

2014

A mixture of compounds often cannot be resolved with a single chromatographic column, but the analysis can be successful using columns of different nature, serially combined through zero-dead volume junctions. In previous work (JCA 1281 (2013) 94), we developed an isocratic approach that optimised simultaneously the mobile phase composition, stationary phase nature and column length. In this work, we take the challenge of implementing optimal linear gradients for serial columns to decrease the analysis time for compounds covering a wide polarity range. For this purpose, five ACE columns of different selectivity (three C18 columns of different characteristics, a cyano and a phenyl column) we…

H-Point Curve Isolation Method for Coupled Liquid Chromatography and UV−Visible Spectrophotometry

2000

The H-point curve isolation method (HPCIM) for the detection of unknown interferences in chromatography is proposed. The method allows one to estimate the UV-vis spectra of interfering species in a sample as well as to test the purity of the chromatographic peaks. Besides the detection of the unknown interferences in a sample, this method allows one to calculate the concentration of an analyte in the presence of unknown compounds. To illustrate the reliability of the proposed method, samples of diuretics and amphetamines have been analyzed by normal- and reversed-phase high-performance chromatography.

Comparison of the solid-phase extraction efficiency of a bounded and an included cyclodextrin-silica microporous composite for polycyclic aromatic hy…

2016

Solid-phase extraction is one of the most important techniques for sample purification and concentration. A wide variety of solid phases have been used for sample preparation over time. In this work, the efficiency of a new kind of solid-phase extraction adsorbent, which is a microporous material made from modified cyclodextrin bounded to a silica network, is evaluated through an analytical method which combines solid-phase extraction with high-performance liquid chromatography to determine polycyclic aromatic hydrocarbons in water samples. Several parameters that affected the analytes recovery, such as the amount of solid phase, the nature and volume of the eluent or the sample volume and …

Ultra high performance liquid chromatography-time-of-flight high resolution mass spectrometry in the analysis of hexabromocyclododecane diastereomers…

2014

An efficient ultra high performance liquid chromatography (UHPLC)-time-of-flight high resolution mass spectrometry (TOF-HRMS) method was elaborated for the determination of hexabromocyclododecane (HBCD) diastereomers in fish samples and compared against UHPLC-Orbitrap-HRMS and UHPLC-triple quadrupole (QqQ) tandem MS (MS/MS) techniques. The TOF-HRMS analyzer was operated at high resolution (>10000 full width at half maximum (FWHM)) with scanning the m/z range from 600 to 700, to achieve picogram quantitation limits. The effects of various operational parameters on the instrumental response were systematically investigated. Evaluation of the influence of sample clean-up procedure steps on sig…