Search results for "analytical"
showing 10 items of 9586 documents
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…
Automated Photo-Induced Fluorescence Determination of Flumetsulam
2009
The present article deals with a new procedure for determination of the herbicide flumetsulam. The fluorimetric procedure is performed on the basis of photo-increased fluorimetric emission of the pesticide solution and by means of a multicommutation continuous-flow assembly. The alkaline solution containing the analyte is irradiated online and then directly forced through the fluorimeter flow cell. The analysis of different samples is completely automated, as the analyte separation was performed online by including a separation cartridge in the manifold. When dealing with solid samples (such as soil samples), the automation was completed by adding to the manifold the corresponding device fo…
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, …
Adsorbent phases with nanomaterials for in-tube solid-phase microextraction coupled on-line to liquid nanochromatography
2015
Following the present trends in miniaturization, a methodology that combines on-line In-Tube Solid-Phase Microextraction (IT-SPME) with Liquid Nanochromatography (nano-LC) and UV-vis diode array detection (DAD) was developed. This coupling was achieved by using two interconnected valves (i.e. conventional and micro-automatic valves) in the system of injection. As for IT-SPME, different materials, containing in some cases nanostructures or nanoparticles and in other cases polymeric adsorbent phases immobilized on capillary columns, were tested in order to improve extraction efficiencies of organic compounds; diclofenac was selected as the target analyte. Additionally, the transfer time of th…
In-tube solid phase microextraction coupled to miniaturized liquid chromatography for both, noble metal nanoparticle assessment and sensitive plasmon…
2021
Abstract Colorimetric localized surface plasmon resonance (LSPR) as analytical response is applied for a wide number of chemical sensors and biosensors. However, the dependence of different factors, such as size distribution of nanoparticles (NPs), shape, dielectric environment, inter-particle distance and matrix, among others, can provide non-reliable results by UV–vis spectrometry in complex matrices if NP assessment is not carried out, particularly at low levels of analyte concentrations. Miniaturized liquid chromatography, capillary (CapLC) and nano (NanoLC), coupled on line with in-tube solid phase microextraction (IT-SPME) is proposed for the first time for both, controlling suitabili…
Evaluation and elimination of the blank bias error using the H-point standard additions method (HPSAM) in the simultaneous spectrophotometric determi…
1997
Abstract The aim of this report is to demonstrate the usefulness of the HPSAM in all instances where the determination of two analytes requires the use of an absorbent reagent, particularly when it does not present a constant analytical signal because of its consumption. This problem can be treated as a ternary mixture by the HPSAM method and then, the fundamentals of the method for resolving these kind of mixtures can be applied. The method can calculate the concentration of one species from spectral data at two wavelengths where the two other species present the same absorbance relationship. These wavelength pairs are easily found, and can be selected to give the most precise results. The…
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…
Control of matrix interferences by multiple linear regression models in the determination of arsenic and lead concentrations in fly ashes by inductiv…
2010
A multiple linear regression technique was used to evaluate and correct the matrix interferences in the determination of As and Pb concentrations in fly ashes by inductively coupled plasma optical emission spectrometry. The direct determination of As and Pb in SRM 1633b by ICP-OES failed to obtain the certified concentrations, except in a couple of cases. However, it proved possible to use the multiple linear regression (MLR) technique to correct the determined concentrations to a satisfactory level. This method of correction is based on the multiple regression line obtained from the analysis of 19 synthetic mixtures of matrix and analyte elements (Al, As, Ca, Fe, Pb, and Si) at five concen…
Identification and determination of synthetic cannabinoids in herbal products by dry film attenuated total reflectance-infrared spectroscopy.
2017
A new procedure has been developed for the identification and quantitative determination of synthetic cannabinoids in illicit herbal preparations. The methodology is based on the use of attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR) measurement of sample extracts with 2-propanol drying 5µL of the extracts onto the ATR crystal. The qualitative identification was carried out on the 2-propanol extract after identification of the herbal matrix, followed by its subtraction and using a cut-off criterion of 75%. Quantitative determination was made by univariate calibration using the absorbance of the band located at 1520cm-1 of the spectrum. Four different cannabin…
In-tube solid-phase microextraction-capillary liquid chromatography as a solution for the screening analysis of organophosphorus pesticides in untrea…
2006
This paper describes a method for the selective screening of organophosphorus pesticides in water. In-tube solid-phase microextraction (SPME) in an open capillary column coupled to capillary liquid chromatography (LC) with UV detection has been used to effect preconcentration, separation and detection of the analytes in the same assembly. For in-tube SPME two capillary columns of the same length and different internal diameters and coating thicknesses have been tested and compared, a 30 cm x 0.25 mm I.D., 0.25 micro m thickness coating column, and a 30 cm x 0.1 mm I.D., 0.1 micro m of coating thickness column. In both columns the coating was 95% dimethylpolysiloxane (PDMS)-5% diphenylpolysi…