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Separation of Pharm...
Separation of Pharmaceuticals by Capillary Electrophoresis using Partial Filling and Multiple-injections
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- Lodén, Henrik, 1972- (författare)
- Uppsala universitet,Avdelningen för analytisk farmaceutisk kemi
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Pettersson, Curt (preses)
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Arvidsson, Torbjörn (preses)
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Amini, Ahmad (preses)
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- Stefansson, Morgan, Docent (opponent)
- AstraZeneca R&D, Mölndal
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(creator_code:org_t)
- ISBN 9789155472115
- Uppsala : Acta Universitatis Upsaliensis, 2008
- Engelska 60 s.
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Serie: Digital Comprehensive Summaries of Uppsala Dissertations from the Faculty of Pharmacy, 1651-6192 ; 75
- Relaterad länk:
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https://uu.diva-port... (primary) (Raw object)
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https://uu.diva-port...
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https://urn.kb.se/re...
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Abstract
Ämnesord
Stäng
- 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.
Nyckelord
- 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
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