Chemometrics in capillary electrophoresis. Part A: Methods for optimization

Sentellas, Sònia; Saurina, Javier

doi:10.1002/jssc.200301514

Cited by 58 publications

(41 citation statements)

References 62 publications

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“…The electrophoretic separation is influenced by experimental variables, such as voltage, temperature, injection time and mode, capillary characteristics, and buffer composition (including pH, presence of organic solvents and modifiers) [28]. Chemometrics was used since the preliminary stages for the establishment of the CE method and the analysis of CE data to extract the maximum amount of significant information.…”

Section: Optimization Of the Separation Stepmentioning

confidence: 99%

Determination of B2 and B6 vitamers in serum by capillary electrophoresis-molecular fluorescence-charge coupled detector

Priego-Capote

Castro

2005

Electrophoresis

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A method for the separation by capillary zone electrophoresis and determination of vitamers of two important water-soluble vitamins, i.e., B2 and B6, is proposed here. The working conditions for optimal separation were obtained by a multivariate methodology in order to succeed in the best resolution in the shortest analysis time. The optimization of the buffer composition together with other variables, such as analysis and injection voltage, temperature of the capillary cassette, and injection time, resulted in a solution of 30 mM KH2PO4 adjusted to pH 8.5 with formic acid. Concerning the detection step, the target analytes were quantified by molecular fluorescence, for which two different detectors, a photomultiplier tube (PMT) and a charge-coupled detector (CCD), were compared in terms of resolution, sensitivity, and precision. A Xe-Hg lamp was used as an irradiation source in the two cases. The best option was the CCD, which provides three-dimensional electropherograms and enables to solve the overlapped peaks. Besides, the sensitivity of the CCD was similar to that of the PMT, due to the treatment data, obtaining limits of detection and quantification from 1.16 to 27.1 ng/g and from 3.83 to 89.4 ng/g, respectively. The method was applied to the serum samples for which a prior liquid-liquid extraction using ethanol in an acid medium was mandatory for eliminating the interferences and concentrating the analytes by a factor of 5. The rapidity of the analysis (13 min for the electrophoretic separation) and the excellent precision (repeatability and within-laboratory reproducibility between 2.86 and 4.11% and 7.03 and 8.45%, respectively, both expressed as relative standard deviation) demonstrated the capability of the proposed method for a clinical routine analysis.

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Section: Optimization Of the Separation Stepmentioning

confidence: 99%

Determination of B2 and B6 vitamers in serum by capillary electrophoresis-molecular fluorescence-charge coupled detector

Priego-Capote

Castro

2005

Electrophoresis

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“…Concluded with a summary of the most important basic principles (golden rules) how to prepare a BGE for a good migration/detection, this work would be particularly useful to facilitate the task of method development by those just beginning to work in the field. Sentellas and Saurina prepared two general reviews on the application of experimental design techniques for optimizing CE separations [6] and chemometric techniques to CE data analysis [7] for various types of analytes including inorganic species. Fritz and his colleagues [8] reviewed recent progress in developing separation systems in which ions migrate under a combined action of ion-exchange (IE) interactions and electrophoretic movement.…”

Section: Reviewsmentioning

confidence: 99%

Capillary electrophoresis of inorganic ions: An update

Timerbaev

2004

Electrophoresis

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This review as a sequel of three earlier similar reports gives a summary of the progress and significant methodological developments, starting from 2002, in the use of capillary electrophoresis (CE) for inorganic ion analysis. As substantiated by the illustrative number of relevant references, improvements in sensitivity achieved both in and outside a CE system, advances in manipulating the separation selectivity, novel hardware configurations, and system performance innovations are continually being reported over the review period. Specifically viewed are the recent advancements in elemental (bio)speciation analysis, which remains one of the most fertile areas of CE research, as well as in three recently booming research topics: contactless conductivity detection, separations on microchips, and transient isotachophoretic preconcentration. A state-of-the-art picture of technique's potentialities within the field of interest presented here demonstrates that CE has become recognized and is growing in acceptance as a reliable alternative to traditional analytical methods such as high-performance liquid chromatography (HPLC).

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“…A general application of chemometric experimental designs for CE optimization methods has also been reviewed [25,26]. Plackett-Burman design is a technique typically used for screening purposes before the precise optimization of parameters using a central composite or Box Benken design to reduce the number of required experiments.…”

Section: Introductionmentioning

confidence: 99%

Use of multivariate analysis for optimization of separation parameters and prediction of migration time, resolution, and resolution per unit time in micellar electrokinetic chromatography

et al. 2006

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The optimization of separation parameters in chromatography for better separation and resolution of analytes continues to be a labor intensive procedure usually performed by a trial and error method. A multivariate analysis in the form of multilinear regression (MLR) is used to optimize separation parameters and predict the migration behavior, resolution, and resolution per unit time of achiral (4-chlorophenol, pentachlorophenol, clonazepam, and diazepam) and chiral (1,1'-binaphthyl 2,2'-dihydrogen phosphate (BNP), and 1,1'-bi-2-naphthol (BOH)) compounds in MEKC. Separations of achiral and chiral analytes were performed using an achiral (poly(sodium N-undecylenic sulfate)) molecular micelle and chiral (poly(sodium N-undecanoyl-L-leucylvalinate) or poly(sodium N-undecanoyl-L-isoleucylvalinate)) molecular micelle, respectively, at various operating temperatures, applied voltages, pH values, and molecular micelle concentrations in the BGE. The separation parameters were subsequently used as input variables for MLR models. The models were validated with independent samples. The root-mean-square percent relative error (RMS%RE) is used as a figure of merit for characterizing the performance of the migration time, resolution, and resolution per unit time models. The RMS%RE obtained for predicted migrated times, resolutions, and resolution per unit time of 4-chlorophenol, pentachlorophenol, clonazepam, diazepam, BNP, and BOH ranged between 8 and 19%. The same experimental procedure was used to optimize the separation parameters of six other chiral analytes of different compound class. The predicted migration times, resolutions, and resolution per unit time of the chiral as well as the achiral analytes compare favorably with the experimental migration times and resolutions, indicating versatility and wide applicability of the technique in MEKC.

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Chemometrics in capillary electrophoresis. Part A: Methods for optimization

Cited by 58 publications

References 62 publications

Determination of B2 and B6 vitamers in serum by capillary electrophoresis-molecular fluorescence-charge coupled detector

Determination of B2 and B6 vitamers in serum by capillary electrophoresis-molecular fluorescence-charge coupled detector

Capillary electrophoresis of inorganic ions: An update

Use of multivariate analysis for optimization of separation parameters and prediction of migration time, resolution, and resolution per unit time in micellar electrokinetic chromatography

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