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showing 10 items of 6843 documents
Characterization of chromatographic peaks using the linearly modified Gaussian model. Comparison with the bi-Gaussian and the Foley and Dorsey approa…
2017
To characterize column performance in liquid chromatography, several parameters must be obtained from experimental data. These parameters can be computed through the numerical integration of the net signal to calculate the moments after subtraction of the baseline. This requires the establishment of the peak integration limits. The whole process introduces significant uncertainty. For this reason, several alternative procedures have been proposed to measure the area, mean time and variance, based on the assumption that the chromatographic peak can be described with a mathematical function. This allows the calculation of the peak position and variance making use of the values of the experime…
Seafood freshness determination through vapour phase Fourier transform infrared spectroscopy.
2006
Abstract A new vapour-phase manifold has been developed to determine trimethylamine (TMA) in fish and cephalopod samples by Fourier transform infrared (FT-IR) spectroscopy. Samples were treated off-line for 1 h with trichloroacetic acid (TCA), filtered and washed. The obtained extracts were aspirated and alkalinized with NaOH 2.0 M, in an on-line system. TMA was separated from the solution in a gas phase separator and then transported by means of a nitrogen carrier into a home made 10 cm pathlength IR gas cell, where the corresponding FT-IR spectra were acquired by accumulating 30 scans per spectrum with 2 cm−1 nominal resolution. The method was applied to the determination of TMA in natura…
Evaluation of extraction alternatives for Fourier transform infrared spectrometric determination of oil and greases in water
1997
Abstract Liquid-liquid extraction (LLE), solid phase extraction (SPE) and microwave-assisted extraction are evaluated for Fourier transform infrared (FTIR) spectrometric determination of oil and grease in polluted waters. A fast microwave-assisted quantitative procedure is proposed for the total extraction of oil and grease into CCl 4 from water samples, with an irradiation time of 1 min at an exit power of 520 W using closed PTFE vessels. The FTIR quantification of oil and grease is carried out by the measurement of the area under the absorbance spectra in the range between 3058 and 2780 cm −1 , with a baseline established between 3200 and 2700 cm −1 . The analytical features of the propos…
Simultaneous determination of acetylsalicylic acid and caffeine in pharmaceuticals by flow injection with fourier transform infrared detection.
1993
Abstract A fast quality control methodology has been developed for the simultaneous determination of acetylsalicylic acid (ASA) and caffeine in pharmaceuticals by flow injection—Fourier Transform Infrared Spectrometry. The method is based on the solubilization of ASA and caffeine in CH2Cl2 and the use of a flow system to introduce samples and standards in the spectrometer. Two solutions, containing 90 and 110% of the reported concentration of the two active principles in the sample, were employed in order to control the extreme tolerance levels accepted by the International Pharmacopeia for the composition of formulations. A 300 μl volume of each solution was injected in turn, into a carrie…
Effect of storage conditions on furosine formation in milk-cereal based baby foods
2008
[EN] The effect of storage during 9 months at 25, 30 and 37 degrees C on furosine formation in three milk-cereal based baby foods was studied to evaluate development of the Maillard reaction. Furosine was measured by HPLC-UV. Immediately after the manufacturing process, furosine contents were 310-340 mg/100 g protein and at the 9th storage month were 426-603 mg/100 g protein. Storage time and temperature have a significant increase (p < 0.05) of furosine content during storage. Furosine contents were higher in sample containing honey than in those without honey. Interactions (p < 0.05) between storage time and temperature or type of sample were found. A predictive model equation of the evol…
High-performance liquid chromatographic determination of furfural compounds in infant formulas
2002
Furfural contents in adapted and follow-up infant formulas were measured by RP-HPLC. The evolution of furfural compound contents during storage (a year at 20 and 37 °C) was studied. 2-Furylmethylketone and 5-methyl-2-furaldehyde were not detectable in analysed samples. The differences in the furfural compounds at point zero between both infant formulas has to be ascribed to the differences in protein and iron contents. An increase in free 5-hydroxymethyl-2-furfuraldehyde (HMF), 2-furaldehyde (F) and HMF+F contents was observed in all samples, although the differences were not statistically significant. The storage temperature affected the total HMF content and the storage time affected the …
Rayleigh and Brillouin scattering in a lysozyme–water mixture: An unusual behavior around 343K
2011
Abstract This article describes Rayleigh and Brillouin light scattering studies on a lysozyme–water mixture from 293 K to 355 K. The scattering intensities from this system are compared with those from a sodium acetate buffer used to dissolve the lysozyme. It is found that in the vicinity of 343 K the lysozyme–water mixture becomes opalescent, and the intensity of the Brillouin peaks decreases and almost vanishes, to be restored at temperatures above 343 K. Around the same temperature the intensity of the central, unshifted Rayleigh peak, however, increases strongly. No such behavior was observed for the sodium acetate buffer. The analysis of the experimental data indicates an irreversible …
Liquid chromatography-Fourier transform infrared spectrometric determination of cholesterol in animal greases
1997
Abstract Stearic acid, cholesterol and cholesteryl palmitate have been separated in less than 14 min by liquid chromatography on a column (3.9 mm i.d.×150 mm) of Nova-Pack C 18 (5 μm) using chloroform–acetonitrile (45 : 55) as mobile phase pumped at 0.5 ml min −1 ; Fourier transform infrared (FTIR) spectrometry was employed for both, general detection at 2868 or 2855 cm −1 and selective detection at 3285 cm −1 for stearic acid and 3526 cm −1 for cholesterol. In all cases a baseline established at 3900 cm −1 , 9-point smoothing and chromatographic peak height measurements were used. The method has been validated by application to the determination of cholesterol in animal greases and fish oi…
Parabolic-Lorentzian modified Gaussian model for describing and deconvolving chromatographic peaks.
2002
Abstract A new mathematical model for characterising skewed chromatographic peaks, which improves the previously reported polynomially modified Gaussian (PMG) model, is proposed. The model is a Gaussian based equation whose variance is a combined parabolic-Lorentzian function. The parabola accounts for the non-Gaussian shaped peak, whereas the Lorentzian function cancels the variance growth out of the elution region, which gives rise to a problematic baseline increase in the PMG model. The proposed parabolic-Lorentzian modified Gaussian (PLMG) model makes a correct description of peaks showing a wide range of asymmetry with positive and/or negative skewness. The new model is shown to give b…
Peak deconvolution in one-dimensional chromatography using a two-way data approach.
2002
A deconvolution methodology for overlapped chromatographic signals is proposed. Several single-wavelength chromatograms of binary mixtures, obtained in different runs at diverse concentration ratios of the individual components, were simultaneously processed (multi-batch approach), after being arranged as two-way data. The chromatograms were modelled as linear combinations of forced peak profiles according to a polynomially modified Gaussian equation. The fitting was performed with a previously reported hybrid genetic algorithm with local search, leaving all model parameters free. The approach yielded more accurate solutions than those found when each experimental chromatogram was fitted in…