Biomedical subjects

Jorge R Vega

Publications and source records attributed to Jorge R Vega.

4 recordsLinked to original sources

PubMed2006

Estimation of band broadening in size-exclusion chromatography. I. A method based on analyzing narrow standards with a molar mass-sensitive detector.

A method is proposed for estimating the (asymmetrical and non-uniform) band broadening function (BBF) in size-exclusion chromatography (SEC). The following data are required: the molar mass calibration and the concentration- and molar mass chromatograms of a set of narrow standards. In the narrow range of each standard, the BBF is uniform but skewed. Each uniform BBF is estimated through a nonlinear optimization procedure that compares one (of the two) measured chromatograms with its theoretical prediction based on the other chromatogram. The method is validated with numerical examples that simulate the analyses of narrow standards exhibiting log-normal and Poisson weight chain length distributions. The BBF can be assumed of arbitrary shape, or represented by an exponentially-modified Gaussian (EMG). From the uniform BBF estimate, the true polydispersity of the standard can be determined. The global non-uniform BBF is obtained by interpolation between a set of uniform BBFs covering a wide range of elution volumes.

Algorithms↗

PubMed2005

Alternative approaches for the estimation of the band broadening parameters in single-detection size exclusion chromatography.

New approaches for the determination of the extent of symmetric and asymmetric band broadening (BB) in size exclusion chromatography (SEC) are presented. For this purpose raw data was simulated by starting with either a theoretical Poisson number chain length distribution (NCLD), or a log-normal weight chain length distribution (WCLD). Each distribution was first converted to a BB-free mass chromatogram, as typically obtained from a standard differential refractive index detector. Then, the broadened (or "measured") chromatograms were simulated by convoluting the BB-free chromatograms with a BB function, which was assumed to follow symmetrical (Gauss) as well as unsymmetrical (exponentially modified Gauss) function. A broad range of BB parameters (standard deviation, sigma(BB), and exponential decay, tau(BB)) was used for the simulations. The approaches are based on the determination of the points of inflection belonging to the peak of the broadened chromatogram, and closed as well as empirically derived equations connecting the peak width, its variance, and the parameters sigma(BB) and tau(BB). The developed methods are applicable for Poisson distributions well above a peak chain length of 100.

Chromatography, Gel↗

PubMed2005

Contamination by larger particles of two almost-uniform latices: analysis by combined dynamic light scattering and turbidimetry.

Multiangle dynamic light scattering (MDLS) and turbidimetry (T) were applied (both individually and combined) for determining the contamination by larger particles of two almost-uniform polystyrene (PS) latices. Latex 1 was synthesized in our laboratories, and it contained a main population diameter of 340 nm together with a small fraction of larger particles. This latex was used as the base material for producing an immunoassay kit. Latex 2 was obtained by a simple blend of two uniform PS standards. The proposed data treatment calculates the diameter and number fraction of the large particles contamination assuming that the PSDs are bimodal. The calculation involves minimizing the errors between the measurements and their theoretical predictions. When analyzed by combined MDLS-T, the contamination of Latex 1 involved number fraction 0.6% and particle diameter 865 nm. The T average diameter is a function of the measurement wavelength, and the highest deviations of this average to an increasing contamination by large particles were always observed at the higher wavelengths. The DLS average diameter is a function of the measurement angle, but in this case it is impossible to determine a priori the angle of observation that provides the largest deviation of this average diameter to an increasing contamination.

Journal Article↗

PubMed2003

Latex particle size distribution by dynamic light scattering: novel data processing for multiangle measurements.

Multiangle dynamic light scattering (DLS) provides a better estimate of particle size distributions (PSD) than single-angle DLS. However, multiangle data treatment requires appropriate weighting of each autocorrelation measurement prior to calculation of the PSD. The weighting coefficients may be directly obtained from (i). the autocorrelation baselines or (ii). independent measurement of the average light intensity by elastic light scattering. However, the propagation of errors associated with such procedures may intolerably corrupt the PSD estimate. In this work, an alternative recursive least-squares calculation is proposed that estimates the weighting coefficients on the basis of the complete autocorrelation measurement. The method was validated through a numerical example that simulates the analysis of a polystyrene latex with a bimodal PSD and with "measurements" taken at 10 detection angles. The ill-conditioned nature of the problem determines that the "true" PSD cannot be recovered, even in the absence of errors. A sensitivity analysis was carried out to determine the effect of errors in the weighting coefficients on the PSD recoveries.

Journal Article↗