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New SPE loading material for affinity‐based separation of cyclodextrins from drug:CD complexes in order to overcome Beer's law deviations
Authors:Stavroula Rozou  Panayiotis Raftopoulos  Sophia Hatziantoniou  Ekaterini Antoniadou‐Vyza
Affiliation:1. R&D Department, ELPEN Pharmaceutical Company, Attica, Greece;2. Department of Pharmaceutical Chemistry, School of Pharmacy, University of Athens, Panepistimiopolis Zografou, Athens, Greece. Fax: +30‐210‐7274747/+30‐210‐3625332;3. Department of Pharmaceutical Technology, University of Athens, Panepistimiopolis Zografou, Athens, Greece
Abstract:Molecular inclusion of guest molecules within CDs is known to alter guest molecule spectrophotometric absorptivity, making their determination, based on spectrophotometric data, inaccurate. Therefore specific analytical methods capable of quantifying the drugs as free molecules must be developed and validated. SPE was selected to simplify sample and avoid more time‐consuming alternatives. A new solid phase was synthesized and characterized by infrared spectrometry, differential scanning calorimetry and elemental analysis. The competitive complexation of adamantane groups immobilized on the silica substrate facilitates drug:CD complex dissociation and elimination of CD from samples. The drug molecules, now free from CD, can be easily analysed by an already available HPLC method. This new SPE loading material was employed in the determination of ketoprofen in its CD complex as a representative example of the utility of this novel material. The calculated analytical errors were reduced from a maximum of 20.79% (without SPE) to a minimum of 3.99%.
Keywords:Cyclodextrin complexes  Ketoprofen  Sample pretreatment  SPE  Stationary phase
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