Search results for "Analyte"
showing 10 items of 303 documents
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…
Validation of a confirmatory method for the determination of macrolides in liver and kidney animal tissues in accordance with the European Union regu…
2006
Abstract This study proposes a simple multiresidue liquid chromatography–diode array detector (LC–DAD) method capable of determining seven macrolide antibiotics in samples of liver and kidney animals at concentrations lower than those allowed by current legislation. Samples were prepared by homogenizing the tissue with EDTA–McIlvaine's buffer and extracted with an Oasis HLB cartridge. The consumption of organic solvent during extraction was minimum. The analytes were detected by LC–DAD and also by liquid chromatography–mass spectrometry with electrospray ionization (LC–(ESI)MS). The method was specific, stable and robust enough for the required purposes. The DAD method was validated in acco…
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.
Comparison of Three Techniques for Lipid Removal from Seal Blubber: Gel Permeation, Acid Treatment, and Dialysis with Semipermeable Membrane
2000
Abstract Harbor seal blubber samples were analyzed for PCDD/Fs and PCBs by splitting the initial extract into three aliquots and applying three different techniques for lipid removal (the first step of sample cleanup methodology for GC-HRMS analysis): gel permeation chromatography (GPC), sulfuric acid treatment, and dialysis through semipermeable membrane. Correlation coefficients of analyte concentrations obtained from three sets of replicate samples ranged from 0.965 to 0.994. In addition, a number of seal blubber samples were processed without pre-extraction using only the dialysis technique. The analyte concentrations in these samples correlated well with the analyte concentrations obta…