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Peak purity determination with principal component analysis of high-performance liquid chromatography-diode array detection data
Stockholm University, Faculty of Science, Department of Analytical Chemistry.
Stockholm University, Faculty of Science, Department of Analytical Chemistry.
2004 (English)In: Journal of Chromatography A, ISSN 0021-9673, E-ISSN 1873-3778, Vol. 1029, no 1-2, 13-20 p.Article in journal (Refereed) Published
Abstract [en]

A method is proposed for the determination of chromatographic peak purity by means of principal component analysis (PCA) of high-performance liquid chromatography with diode array detection (HPLC–DAD) data. The method is exemplified with analysis of binary mixtures of lidocaine and prilocaine with different levels of separation. Lidocaine and prilocaine have very similar spectra and the chromatograms used had substantial peak overlap. The samples analysed contained a constant amount of lidocaine and a minor amount of prilocaine (0.02–2 conc.%) and hence the focus was on determining the purity of the lidocaine peak in the presence of much smaller levels of prilocaine. The peak purity determination was made by examination of relative observation residuals, scores and loadings from the PCA decomposition of DAD data over a chromatographic peak. As a reference method, the functions for peak purity analysis in the chromatographic data system used (Chromeleon) were applied. The PCA method showed good results at the same level as the detection limit of baseline-separated prilocaine, outperforming the methods in Chromeleon by a factor of ten. There is a discussion of the interpretation of the result, with some comparisons with evolving factor analysis (EFA). The main advantage of the PCA method for determination of peak purity over methods like EFA lies in its simplicity, short time of calculation and ease of use.

Place, publisher, year, edition, pages
2004. Vol. 1029, no 1-2, 13-20 p.
Keyword [en]
Principal component analysis, Peak purity determination, Relative observation residuals, Scores, Loadings
Identifiers
URN: urn:nbn:se:su:diva-22777DOI: 10.1016/j.chroma.2003.12.052OAI: oai:DiVA.org:su-22777DiVA: diva2:189422
Note
Part of urn:nbn:se:su:diva-110Available from: 2004-04-22 Created: 2004-04-22 Last updated: 2010-08-03Bibliographically approved
In thesis
1. Multivariate spectroscopic methods for the analysis of solutions
Open this publication in new window or tab >>Multivariate spectroscopic methods for the analysis of solutions
2004 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

In this thesis some multivariate spectroscopic methods for the analysis of solutions are proposed. Spectroscopy and multivariate data analysis form a powerful combination for obtaining both quantitative and qualitative information and it is shown how spectroscopic techniques in combination with chemometric data evaluation can be used to obtain rapid, simple and efficient analytical methods. These spectroscopic methods consisting of spectroscopic analysis, a high level of automation and chemometric data evaluation can lead to analytical methods with a high analytical capacity, and for these methods, the term high-capacity analysis (HCA) is suggested. It is further shown how chemometric evaluation of the multivariate data in chromatographic analyses decreases the need for baseline separation.

The thesis is based on six papers and the chemometric tools used are experimental design, principal component analysis (PCA), soft independent modelling of class analogy (SIMCA), partial least squares regression (PLS) and parallel factor analysis (PARAFAC). The analytical techniques utilised are scanning ultraviolet-visible (UV-Vis) spectroscopy, diode array detection (DAD) used in non-column chromatographic diode array UV spectroscopy, high-performance liquid chromatography with diode array detection (HPLC-DAD) and fluorescence spectroscopy. The methods proposed are exemplified in the analysis of pharmaceutical solutions and serum proteins.

In Paper I a method is proposed for the determination of the content and identity of the active compound in pharmaceutical solutions by means of UV-Vis spectroscopy, orthogonal signal correction and multivariate calibration with PLS and SIMCA classification. Paper II proposes a new method for the rapid determination of pharmaceutical solutions by the use of non-column chromatographic diode array UV spectroscopy, i.e. a conventional HPLC-DAD system without any chromatographic column connected. In Paper III an investigation is made of the ability of a control sample, of known content and identity to diagnose and correct errors in multivariate predictions something that together with use of multivariate residuals can make it possible to use the same calibration model over time. In Paper IV a method is proposed for simultaneous determination of serum proteins with fluorescence spectroscopy and multivariate calibration. Paper V proposes a method for the determination of chromatographic peak purity by means of PCA of HPLC-DAD data. In Paper VI PARAFAC is applied for the decomposition of DAD data of some partially separated peaks into the pure chromatographic, spectral and concentration profiles.

Place, publisher, year, edition, pages
Stockholm: Institutionen för analytisk kemi, 2004. 73 p.
Keyword
Chemometrics, UV-Vis spectroscopy, Multivariate calibration, Lidocaine, Identity, Content, PLS, SIMCA, Non-column, Diode array UV spectroscopy, DAD, Control sample, High Capacity Analysis (HCA), Fluorescence spectroscopy, Albumin, Immunoglobulin G, HPLC-DAD, Prilocaine, Peak purity determination, PCA, PARAFAC, Partial separation, Curve resolution
National Category
Analytical Chemistry
Identifiers
urn:nbn:se:su:diva-110 (URN)91-7265-789-8 (ISBN)
Public defence
2004-05-14, Magnélisalen, Kemiska övningslaboratoriet, Svante Arrhenius väg 12 A, Stockholm, 13:15
Opponent
Supervisors
Available from: 2004-04-22 Created: 2004-04-22Bibliographically approved

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