Change search
CiteExportLink to record
Permanent link

Direct link
Cite
Citation style
  • apa
  • ieee
  • modern-language-association-8th-edition
  • vancouver
  • Other style
More styles
Language
  • de-DE
  • en-GB
  • en-US
  • fi-FI
  • nn-NO
  • nn-NB
  • sv-SE
  • Other locale
More languages
Output format
  • html
  • text
  • asciidoc
  • rtf
Rapid determination of lidocaine solutions with non-column chromatographic diode array UV spectroscopy and multivariate calibration
Stockholm University, Faculty of Science, Department of Analytical Chemistry.
Stockholm University, Faculty of Science, Department of Analytical Chemistry.
2003 (English)In: Journal of Pharmaceutical and Biomedical Analysis, ISSN 0731-7085, E-ISSN 1873-264X, Vol. 30, no 5, 1575-1586 p.Article in journal (Refereed) Published
Abstract [en]

A new method for the rapid determination of pharmaceutical solutions is proposed. A conventional HPLC system with a Diode Array Detector (DAD) was used with no chromatographic column connected. As eluent, purified water (Milli Q) was used. The pump and autosampler of the HPLC system were mainly utilised as an automatic and convenient way of introducing the sample into the DAD. The method was tested on the local anaesthetic compound lidocaine. The UV spectrum (245–290 nm) from the samples analysed in the detector was used for multivariate calibration for the determination of lidocaine solutions. The content was determined with PLS regression. The effect on the predictive ability of three factors: flow, data-collection rate and rise time as well as two ways of exporting a representative UV spectrum from the DAD file collected was investigated by means of an experimental design comprising 11 experiments. For each experiment, 14 solutions containing a known content of lidocaine were analysed (0.02–0.2 mg ml−1). From these 14 samples two calibration sets and two test sets were made and as the response in the experimental design the Root Mean Square Error of Prediction (RMSEP) values from the predictions of the two test sets were used. When the factor setting giving the lowest RMSEP was found, this setting was used when analysing a new calibration set of 12 lidocaine samples (0.1–0.2 mg ml−1). This calibration model was validated by two external test sets, A and B, analysed on separate occasions for the evaluation of repeatability (test set A) and determination over time (test set B). For comparison, the reference method, liquid chromatography, was also used for analysis of the ten samples in test set B. This comparison of the two methods was done twice on different occasions. The results show that in respect of accuracy, precision and repeatability the new method is comparable to the reference method. The main advantages compared with liquid chromatography are the much shorter time of analysis (<30 s) as well as the automatic and simple analytical procedure and the low consumption of organic solvents.

Place, publisher, year, edition, pages
2003. Vol. 30, no 5, 1575-1586 p.
Keyword [en]
Non-column, Diode array UV spectroscopy, Multivariate calibration, Lidocaine, PLS
Identifiers
URN: urn:nbn:se:su:diva-22774DOI: 10.1016/S0731-7085(02)00548-4OAI: oai:DiVA.org:su-22774DiVA: diva2:189419
Note
Part of urn:nbn:se:su:diva-110Available from: 2004-04-22 Created: 2004-04-22 Last updated: 2017-12-13Bibliographically 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

Open Access in DiVA

No full text

Other links

Publisher's full text

Search in DiVA

By author/editor
Jacobsson, Sven P.
By organisation
Department of Analytical Chemistry
In the same journal
Journal of Pharmaceutical and Biomedical Analysis

Search outside of DiVA

GoogleGoogle Scholar

doi
urn-nbn

Altmetric score

doi
urn-nbn
Total: 118 hits
CiteExportLink to record
Permanent link

Direct link
Cite
Citation style
  • apa
  • ieee
  • modern-language-association-8th-edition
  • vancouver
  • Other style
More styles
Language
  • de-DE
  • en-GB
  • en-US
  • fi-FI
  • nn-NO
  • nn-NB
  • sv-SE
  • Other locale
More languages
Output format
  • html
  • text
  • asciidoc
  • rtf