0000000000114979
AUTHOR
Carlos Mongay-fernández
Chemical initiation for butyl and lauryl acrylate monolithic columns for CEC.
Butyl acrylate (BA)- and lauryl acrylate (LA)-based monolithic stationary phases for CEC were synthesized, using a redox system as initiator of polymerization. BA monoliths were initiated with ammonium peroxodisulfate, whereas LA columns were obtained with lauroyl peroxide as initiator. In both cases, TEMED was used to activate the process. The influence of porogenic solvent composition on both morphological and electrochromatographic properties of the resulting monoliths was investigated. Excellent efficiencies (minimum plate heights of 4.2-6.3 microm for BA columns and 2.6-5.3 microm for LA stationary phases, for a PAHs mixture) were achieved. The capability of separation of both types of…
Lauroyl peroxide as thermal initiator of lauryl methacrylate monolithic columns for CEC
The preparation of lauryl methacrylate (LMA)-based monolithic columns for CEC using lauroyl peroxide (LPO) as thermal initiator of polymerization has been investigated. The influence of initiator amount and composition of porogenic solvent on the physical and electrochromatographic properties of the resulting LMA-based monoliths was evaluated. A comparison with LMA-based columns thermally polymerized with AIBN was performed. At a given porogenic solvent composition, LMA stationary phases initiated with LPO showed higher permeabilities and better efficiency values than those prepared using AIBN as initiator. The optimum polymerization mixture found for LPO initiator provided a minimum plate …
Prediction of the curing time of Spanish hams using peptide profiles established by capillary zone electrophoresis
Abstract A capillary zone electrophoresis procedure for the prediction of curing time of Spanish hams using peptide profiles has been developed. Excellent resolution between the seven peptide peaks was achieved within 30 min analysis time with a BGE containing 60 mM MgSO 4 and 50 mM phosphate at pH 2.5. Using hams with curing times of 6, 8 and 12 months, both linear discriminant analysis (LDA) and multiple linear regression (MLR) models were constructed. In both cases, two different normalisation procedures of the peak areas were compared. Using LDA, all the ham samples corresponding to the three categories were correctly classified. Using MLR, the ham curing time could be predicted with av…
Preparation and evaluation of butyl acrylate-based monolithic columns for CEC using ammonium peroxodisulfate as a chemical initiator.
Acrylate-ester-based monoliths for CEC using peroxodisulfate as a chemical initiator were prepared. The influence of two ternary porogenic solvents on the physical and chromatographic properties of butyl acrylate monolithic stationary phases was investigated. The composition and the ratio of porogenic solvent were adjusted to obtain highly permeable rigid monoliths with adequate column efficiency. Among the prepared butyl acrylate monoliths, those polymerized from a ternary porogenic solvent of acetonitrile/ethanol/water exhibited the most promising performance with a minimum plate height for naphthalene of 10.5 microm and a bed permeability of 7.3 x 10(-14) m(2). A comparison in terms of e…
Improvement of the electrophoretic protein profiles of Leguminosae gums extracts using gamanase and application to the evaluation of carob–guar mixtures
Abstract A quantitative assay for guar gum in carob gum, based on the extraction of proteins in acetonitrile–water (7:3), separation by capillary electrophoresis and multiple linear regression (MLR) using the areas of nine selected peaks as predictors, was improved by performing the extraction in the presence of gamanase. In the absence of the enzyme, peak migration times and areas depended on the guar content, which complicated peak identification and evaluation. Manual correction of the migration times by comparison with standard electropherograms obtained with pure carob and carob–guar mixtures was required; however, when the proteins were extracted under sonication at 60 °C for 30 min i…
CEC column behaviour of butyl and lauryl methacrylate monoliths prepared in non-aqueous media
Polymeric monolithic stationary phases for capillary electrochromatography were prepared using two bulk monomers, butyl methacrylate (BMA) and lauryl methacrylate (LMA), by in situ polymerization in non-aqueous media. The effect of 1,4-butanediol/1-propanol ratio on porous properties was investigated separately for each monomer, keeping the proportion of monomers to pore-forming solvents fixed at 40:60 wt:wt. Also, mixtures of BMA and LMA at different 1,4-butanediol/1-propanol ratios were studied for tailoring the morphological features of the monolithic columns. The chromatographic performance of the different columns was evaluated by means of van Deemter plots of polycyclic aromatic hydro…
Identification of Leguminosae gums and evaluation of carob-guar mixtures by capillary zone electrophoresis of protein extracts.
A procedure for the extraction and capillary zone electrophoresis (CZE) separation of proteins from carob, guar and tara gums in a background electrolyte (BGE) of pH 9 containing 0.1% polyvinyl alcohol is described. The CZE protein profiles exhibit characteristic peaks for each one of the Leguminosae gums, which can be used to construct models capable of identifying samples of carob, guar and tara gums, and predicting the guar content in binary carob-guar mixtures of different geographical origin and harvested in different years. The classification and prediction models are constructed by using linear discriminant analysis (LDA) and multiple linear regression (MLR), respectively. An excelle…
Pointwise resolutive significance of data and applications in experimental design and data treatment
Abstract The concept of the resolutive significance of a point in a data set with regard to a number of addressed parameters is introduced, and two algorithms able to measure it are proposed. The algorithms are validated using simulated experiments. The sum of all the pointwise resolutive significances of a data set is also proposed as a measure of the resolution of the data set. This sum correlates well with the reciprocal of the standard deviation of the fitted parameters, indicating the precision that can be expected for each parameters. Applications in experimental design, and a method for establishing the weights in the least-quarters regression analysis are discussed.
Peroxodisulfate as a chemical initiator for methacrylate-ester monolithic columns for capillary electrochromatography
Organic monolithic stationary phases for CEC were synthesized in situ in fused-silica capillaries. Polymerization mixtures were composed of butyl methacrylate, ethylene dimethacrylate, and [2-(methacryloyloxy)ethyl]trimethyl ammonium chloride in the presence of a porogenic solvent, using ammonium peroxodisulfate as chemical initiator, and N,N,N',N'-tetramethylethylenediamine to activate the reaction. The influence of the amount of initiator, temperature, and composition of porogenic solvent on the physical and chromatographic properties of monolithic stationary phases has been investigated. A minimum plate height of 14.5 microm was obtained at 18 wt% of 1,4-butanediol in the polymerization …
Determination of cationic surfactants by capillary zone electrophoresis and micellar electrokinetic chromatography with deoxycholate micelles in the presence of large organic solvent concentrations.
Mixtures of the cationic surfactants benzalkonium chloride (BKC) and cetylpyridinium chloride (CPC) were quickly resolved and reproducibly and reliably determined by using background electrolytes (BGEs) containing 80 mM borate, pH 8.5, bile salts and large concentrations of an organic solvent. When the bile salt is present, the separation mechanism changes from capillary zone electrophoresis (CZE) to a mixed micellar electrokinetic chromatography (MEKC)-CZE, with predominant MEKC interactions, which lead to an excellent resolution of all the solutes, including the C12-C18 homologues of BKC and CPC. A BGE containing 50 mM sodium deoxycholate and 30% ethanol for an extreme resolution, or 20% …
Preparation and characterization of hexyl methacrylate monolithic columns for CEC
The preparation of hexyl methacrylate (HMA) monolithic columns for CEC separations has been investigated with two initiation systems: (i) ammonium peroxodisulphate and TEMED to activate the polymerization reaction, and (ii) by thermal initiation with AIBN. For both initiators, the influence of composition of porogenic solvent on morphological and chromatographic properties of monoliths was investigated. Two porogenic solvent systems, aqueous and non-aqueous media, were also studied for monolithic beds polymerized with AIBN. Under optimal conditions, low minimum plate heights (9.6 mum for peroxodisulphate, 8.4 and 10.0 mum for AIBN in aqueous and non-aqueous porogenic solvents, respectively)…