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Fractional Factorial Design Optimization of the Separation of Pilocarpine and its Degradation Products by Capillary Electrophoresis
Uppsala University, Disciplinary Domain of Medicine and Pharmacy, Faculty of Pharmacy, Department of Medicinal Chemistry, Analytical Pharmaceutical Chemistry.
1997 (English)In: Journal of Chromatography B: Biomedical Sciences and Applications, ISSN 1387-2273, Vol. 697, no 1-2, 207-215 p.Article in journal (Refereed) Published
Abstract [en]

The separation of pilocarpine and its degradation products by micellar electrokinetic capillary chromatography (MECC) has been optimized by using fractional factorial design of the experiments. Critical parameters were identified in a screening design, and an optimization design was used to optimize the separation. The optimal separation method was based on a borate buffer with sodium dodecyl sulfate (SDS). It is concluded that by using fractional factorial design it is possible to improve the separation of pilocarpine, its trans epimer, isopilocarpine and their hydrolysis products, pilocarpic acid and isopilocarpic acid.

Place, publisher, year, edition, pages
1997. Vol. 697, no 1-2, 207-215 p.
National Category
Medical and Health Sciences
Identifiers
URN: urn:nbn:se:uu:diva-89801DOI: 10.1016/S0378-4347(97)00108-4PubMedID: 9342671OAI: oai:DiVA.org:uu-89801DiVA: diva2:161567
Available from: 2002-04-15 Created: 2002-04-15 Last updated: 2013-05-24Bibliographically approved
In thesis
1. Studies of Micellar Electrokinetic Chromatography as an Analytical Technique in Pharmaceutical Analysis - an Industrial Perspective
Open this publication in new window or tab >>Studies of Micellar Electrokinetic Chromatography as an Analytical Technique in Pharmaceutical Analysis - an Industrial Perspective
2002 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

Studies have been performed to evaluate the use of micellar electrokinetic chromatography (MEKC), one mode of capillary electrophoresis (CE), as an analytical technique in industrial pharmaceutical analysis. The potential for using chemometrics for the optimisation of MEKC methods has also been studied as well as the possibilities of coupling MEKC with mass spectrometry (MS).

Two methods were developed, one for the determination of ibuprofen and codeine and another for pilocarpine, together with their degradation products and impurities in both cases. MEKC was found to be the most suitable mode of CE for the methods. Both methods were optimised by means of experimental design. Valuable information was gathered and optimum conditions were defined which resulted in fast systems with baseline-separated peaks. The ibuprofen-codeine method was validated according to the recommended validation procedures of the International Conference of Harmonisation. The validation was performed on a commercially available tablet formulation to verify the suitability of the method, i.e. for quantification of the two main compounds and to determine the degradation products and impurities in area% of each main peak. The following parameters were determined: selectivity, linearity, accuracy, precision, detection limit, quantitation limit, robustness and range. The results confirm that the method is highly suitable for its intended purpose, i.e. as a routine method for assay and impurity determination. The MEKC method for ibuprofen-codeine was coupled to a mass spectrometer in order to evaluate the potential of partial filling (PF)-MEKC-MS for identification of impurities in pharmaceutical substances and products. The so-called partial-filling technique was used to prevent the non-volatile micelles from entering the MS and was shown to fulfil its purpose of providing detection limits of about 10 pg.

The study clearly shows that micellar electrokinetic chromatography is well-suited as an analytical technique in industrial pharmaceutical analysis.

Place, publisher, year, edition, pages
Uppsala: Acta Universitatis Upsaliensis, 2002. 40 p.
Series
Comprehensive Summaries of Uppsala Dissertations from the Faculty of Pharmacy, ISSN 0282-7484 ; 271
Keyword
Pharmaceutical chemistry, Micellar Electrokinetic Chromatography, Pharmaceutical Analysis, Chemometrics, Validation, Mass Spectrometry, Partial-filling technique, Pilocarpine, Ibuprofen, Codeine., Farmaceutisk kemi
National Category
Medicinal Chemistry
Research subject
Analytical Pharmaceutical Chemistry
Identifiers
urn:nbn:se:uu:diva-1970 (URN)91-554-5281-7 (ISBN)
Public defence
2002-05-08, B21, Uppsala, 13:15
Opponent
Available from: 2002-04-15 Created: 2002-04-15Bibliographically approved

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