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Separation of Pharmaceuticals by Capillary Electrophoresis using Partial Filling and Multiple-injections
Uppsala University, Disciplinary Domain of Medicine and Pharmacy, Faculty of Pharmacy, Department of Medicinal Chemistry, Analytical Pharmaceutical Chemistry.
2008 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

Different multiple-injection methodologies and the partial filling technique (PFT) have been utilized for separation of pharmaceuticals by capillary elec-trophoresis.

In multiple-injection capillary zone electrophoresis (MICZE), the samples and all standards, used for construction of the calibration curve, are analyzed within a single run. Four different modes of MICZE have been described by means of equations, which were experimentally verified. The developed equations facilitate the transfer from conventional single-injection CZE to one or more of these MICZE-modes, depending on the selectivity between the analyte and the injection marker. The applicability of two of these modes was then demonstrated by quantification of buserelin and salbutamol, re-spectively in commercially available pharmaceutical products. The content of buserelin in an injection solution was determined to 0.94 mg/ml, which only deviated slightly from the declared concentration (1 mg/ml). An alter-native mode of MICZE, offering a higher number of sequential sample injec-tions, was then utilized for single-run determination of salbutamol in 15 tab-lets, with a labelled content of 8 mg. The average content of the tablets was determined to 7.8 mg, with an intra-tablet variation of 3 % or less.

Moreover, UV- and mass-spectrometric detection of enantiomeric amines, resolved by non-aqueous capillary electrophoresis (NACE), was demon-strated. Separation of enantiomeric amines was achieved using the chiral selector (-)-2,3:4,6-di-O-isopropylidene-2-keto-L-gulonic acid, (-)-DIKGA. Introduction of the non-volatile (-)-DIKGA into the mass-spectrometer was avoided by using the PFT, where the capillary is only partially filled with electrolyte containing the chiral selector.

Place, publisher, year, edition, pages
Uppsala: Acta Universitatis Upsaliensis , 2008. , p. 60
Series
Digital Comprehensive Summaries of Uppsala Dissertations from the Faculty of Pharmacy, ISSN 1651-6192 ; 75
Keywords [en]
Capillary Coating, Chiral Separation, Enantiomers, Mass-spectrometric Detection, Method Validation, Multiple-injection Capillary Zone Electrophoresis, Non-aqueous Capillary Electrophoresis, Organic Solvents, Pharmaceutical Analysis, Quantitative Analysis
Identifiers
URN: urn:nbn:se:uu:diva-8841ISBN: 978-91-554-7211-5 (print)OAI: oai:DiVA.org:uu-8841DiVA, id: diva2:172111
Public defence
2008-06-05, B41, BMC, Husargatan 3, Uppsala, 13:15
Opponent
Supervisors
Available from: 2008-05-14 Created: 2008-05-14 Last updated: 2011-01-28Bibliographically approved
List of papers
1. Principles for different modes of multiple-injection CZE
Open this publication in new window or tab >>Principles for different modes of multiple-injection CZE
2008 (English)In: Electrophoresis, ISSN 0173-0835, E-ISSN 1522-2683, Vol. 29, no 19, p. 3952-3958Article in journal (Refereed) Published
Abstract [en]

This paper introduces four different modes of multiple-injection CZE (MICZE). The validity of these MICZE models was evaluated by the experimental data. Prior to the application of MICZE, the electrophoretic conditions are developed in the single-injection mode by adjusting different experimental parameters such as pH, type and concentration of buffer additives and temperature. Based on the migration time difference (tmig) between the analyte and the internal standard or injection marker, one or more MICZE modes can be employed. The injection marker is added to the sample to compensate for injection-volume fluctuations. The inter-plug distance is regulated by applying an electrical field over the capillary for a short period of time between each injection. After the final injection, the separation is completed by electrophoresis for a time period corresponding to that in the single-injection mode

Place, publisher, year, edition, pages
Wiley, 2008
Keywords
Moxonidine, Multiple-injection, Oxprenolol, Phenylpropanolamine, Salbutamol
National Category
Medicinal Chemistry
Research subject
Analytical Pharmaceutical Chemistry
Identifiers
urn:nbn:se:uu:diva-86740 (URN)10.1002/elps.200800398 (DOI)000261049400002 ()
Note
Conference Information: 7th Asia-Pacific International Symposium on Microscale Separations and Analysis Singapore, SINGAPORE, DEC 17-19, 2007 Available from: 2008-12-01 Created: 2008-12-01 Last updated: 2018-01-13Bibliographically approved
2. Quantification of Buserelin in a Pharmaceutical Product by Multiple-injection CZE
Open this publication in new window or tab >>Quantification of Buserelin in a Pharmaceutical Product by Multiple-injection CZE
2007 (English)In: Electrophoresis, ISSN 0173-0835, E-ISSN 1522-2683, Vol. 28, no 10, p. 1548-1556Article in journal (Refereed) Published
Abstract [en]

An efficient and rapid separation method based on reversed-polarity multiple-injection CZE (MICZE), has been developed for the quantification of buserelin in a pharmaceutical product. The determinations were performed by serially injecting five standard solutions of buserelin (50-300 μug/mL) and one reference analyte into a Polybrene-coated capillary. All the samples contained goserelin, an analog peptide to buserelin, as internal standard (IS). Immediately after pressure injection, the applied sample plugs were subjected to electrophoresis for 2 min at -25 kV. Consequently, each sample plug became isolated from its neighboring plugs by the BGE, composed of 100 mM phosphate-triethanolamine buffer at pH 3.0 containing 10% v/v ACN. During separation the individual sample components migrated at similar velocities and as distinct zones through the capillary giving 24 peaks, 12 from the analyte and the IS and 12 from the sample matrix. The buserelin content of the pharmaceutical product was determined to be 0.94 ± 0.05 mg/mL, which is only a slight deviation from the declared concentration (1 mg/mL).

Keywords
Buserelin, Multiple injection, Peptides, Polybrene, Quantitative analysis
National Category
Pharmaceutical Sciences
Identifiers
urn:nbn:se:uu:diva-97251 (URN)10.1002/elps.200600636 (DOI)000246923300012 ()17447243 (PubMedID)
Available from: 2008-05-14 Created: 2008-05-14 Last updated: 2018-01-13Bibliographically approved
3. Determination of Salbutamol in Tablets by Multiple-injection Capillary Zone Electrophoresis
Open this publication in new window or tab >>Determination of Salbutamol in Tablets by Multiple-injection Capillary Zone Electrophoresis
Manuscript (Other academic)
Identifiers
urn:nbn:se:uu:diva-97252 (URN)
Available from: 2008-05-14 Created: 2008-05-14 Last updated: 2010-01-13Bibliographically approved
4. Development of a Chiral non-Aqueous Capillary Electrophoretic System using the Partial Filling Technique with UV and Mass Spectrometric Detection
Open this publication in new window or tab >>Development of a Chiral non-Aqueous Capillary Electrophoretic System using the Partial Filling Technique with UV and Mass Spectrometric Detection
Show others...
2003 In: Journal of Chromatography A, ISSN 0021-9673, Vol. 986, no 1, p. 143-152Article in journal (Refereed) Published
Identifiers
urn:nbn:se:uu:diva-97253 (URN)
Available from: 2008-05-14 Created: 2008-05-14Bibliographically approved

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