Enantioselective determination of selfotel in human urine by high-performance liquid chromatography on a chiral stationary phase after derivatization with 9-fluorenylmethyl chloroformate |
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| Institution: | 1. Ciba-Geigy Corporation, Pharmaceuticals Division, 556 Morris Avenue, Summit, NJ 07901, USA;2. Ciba-Geigy S.A., Division Farmaceutica, C. de la Marina 206, 08013 Barcelona, Spain;3. Perkin-Elmer Corporation, 761 Main Avenue, Norwalk, CT 06859, USA;1. Unipampa Federal University, Uruguaiana, Rio Grande do Sul, Brazil;2. Division of Allergy and Clinical Immunology, Federal University of São Paulo, São Paulo, Brazil;3. Department of Pediatrics, Federal University of Paraná, Curitiba, Paraná, Brazil;4. Dr Avelino L. Castelán Pediatric Hospital, Chaco, Argentina;5. Hospital Universitario Metropolitano, Barranquilla, Colombia;6. Hospital Universitario General Calixto García, Havana, Cuba;7. Centro de Asma y Alergia, Tegucigalpa, Honduras;8. Centro Médico San Angel, Xalapa, Mexico;9. Clínica de Alergia y Asma, Asuncion, Paraguay;10. Centro de Medicina Avanzada Dr. Abel González, Santo Domingo, Dominican Republic;11. Hospital Pediatrico Pereira Rossell, Montevideo, Uruguay;12. Clínica Regional del Este, Córdoba, Argentina;13. Centro Nacional de Biopreparados, Havana, Cuba;14. Centro de Pesquisa: Consultorios del médico de familia, Havana, Cuba;15. Hospital Universitario Infantil Sur, Santiago de Cuba, Cuba;p. Allergy Service of the Hospital ISSSTE, Veracruz, Mexico;q. Universidad Nacional Del Este, Asuncion, Paraguay;r. ABC Foundation School of Medicine, Santo André, Brazil;1. Sisli Etfal Education and Research Hospital, Department of Pediatric Immunology and Allergy, Istanbul, Turkey;2. Bakırkoy Dr. Sadi Konuk Education and Research Hospital, Department of Pediatric Immunology and Allergy, Istanbul, Turkey;3. Division of Immunology and Allergy, Department of Chest Diseases, School of Medicine, Hacettepe University, Ankara, Turkey;4. International Hospital, Yesilkoy, Istanbul, Turkey;1. Department of Bioengineering, College of Life Science, Dalian Minzu University, Dalian 116600, Liaoning, China;2. Key Laboratory of Biotechnology and Bioresources Utilization (Dalian Minzu University), Ministry of Education, China;3. School of Life Science and Biotechnology, Dalian University of Technology, No 2 Linggong Road, Dalian 116024, Liaoning, China;4. Department of Agricultural Biotechnology, College of Agriculture and Life Sciences, Seoul National University, Gwanak-gu, Seoul 08826, Republic of Korea;5. Division of Biotechnology, College of Life Sciences and Biotechnology, Korea University, Seoul 02841, Republic of Korea;6. Institute of Life Science and Natural Resources, Korea University, Seoul 02841, Republic of Korea |
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| Abstract: | An analytical method for the enantioselective determination of selfotel in human urine has been developed and validated. The method is based on high-performance liquid chromatography and utilizes CGS 20005 (a selfotel analog) as the internal standard. Urine samples were derivatized in situ with o-phthalic dicarboxaldehyde–3-mercaptopropionic acid and 9-fluorenylmethyl chloroformate (FMOC). Chromatographic separations of the FMOC derivatives of selfotel enantiomers and the internal standard were achieved using a column switching system consisting of an Inertsil ODS-2 column (75×4.6 mm I.D., 5 μm) and a Chiralcel OD-R column (250×4.6 mm I.D., 10 μm). The composition of the mobile phase was acetonitrile–0.1 M phosphate buffer, pH 2.50 (35:65) for the Inertsil ODS-2 column and acetonitrile–0.1 M phosphate buffer, pH 2.00 (35:65) for the Chiralcel OD-R column. The analytes were monitored using fluorescence detection at an excitation wavelength of 262 nm and an emission wavelength of 314 nm. The limit of quantification (LOQ) for this method is 0.25 μg/ml for each selfotel enantiomer. The method was successfully utilized to determine preliminary selfotel stereospecific pharmacokinetics. |
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