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Development of a liquid chromatography Q Exactive high resolution mass spectrometry method by the Box-Behnken design for the investigation of sibutramine urinary metabolites.
de Souza Anselmo, Carina; Matias, Bernardo Fonseca; Sardela, Vinicius Figueiredo; Ribeiro, Ana Ferreira; da Costa Nunes, Isabelle Karine; de Sousa, Valéria Pereira; Pereira, Henrique Marcelo Gualberto.
Afiliación
  • de Souza Anselmo C; Federal University of Rio de Janeiro, Institute of Chemistry, LBCD - LADETEC, Rio de Janeiro, Brazil; Federal University of Rio de Janeiro, Faculty of Pharmacy, Department of Drugs and Pharmaceutics, Rio de Janeiro, Brazil. Electronic address: carinaanselmo@iq.ufrj.br.
  • Matias BF; Federal University of Rio de Janeiro, Institute of Chemistry, LBCD - LADETEC, Rio de Janeiro, Brazil.
  • Sardela VF; Federal University of Rio de Janeiro, Institute of Chemistry, LBCD - LADETEC, Rio de Janeiro, Brazil.
  • Ribeiro AF; Federal Institute of Rio de Janeiro, Rio de Janeiro, Brazil.
  • da Costa Nunes IK; Federal University of Rio de Janeiro, Institute of Chemistry, LBCD - LADETEC, Rio de Janeiro, Brazil.
  • de Sousa VP; Federal University of Rio de Janeiro, Faculty of Pharmacy, Department of Drugs and Pharmaceutics, Rio de Janeiro, Brazil.
  • Pereira HMG; Federal University of Rio de Janeiro, Institute of Chemistry, LBCD - LADETEC, Rio de Janeiro, Brazil.
J Chromatogr B Analyt Technol Biomed Life Sci ; 1125: 121726, 2019 Sep 01.
Article en En | MEDLINE | ID: mdl-31362180
Sibutramine is cited by the World Anti-Doping Agency as a stimulant. According to the literature, sibutramine is extensively metabolized into N-desmethyl-sibutramine (M1), N-bisdesmethyl-sibutramine (M2) and monohydroxy derivatives of M1 and M2. Therefore, it is important to verify new sibutramine metabolites through current analytical methodologies, such as liquid chromatography coupled to high resolution mass spectrometry (LC-HRMS). Furthermore, the development of a comprehensive approach to investigate sibutramine metabolism can increase the detection window for stimulant misuse and enable advancements in pharmacological studies. This work aimed to develop and evaluate the performance of an LC-HRMS method applying Design of Experiments (DoE) for sibutramine metabolite analysis in human urine. After optimizing the method by DoE, the final chromatographic conditions were based on reversed-phase chromatography using a C18 column with a ramp time of 25 min, a flow rate of 0.17 mL min-1 and a temperature of 50 °C. Mobile phase A consisted of water with 0.1% formic acid and 5 mM ammonium formate, and mobile phase B consisted of methanol with 0.1% formic acid; the initial gradient percent was 15% B, and the injection volume was 5 µL. In addition to the hydroxylated metabolites previously described in human urine, dihydroxy derivatives of M1 and M2 were observed for the first time. These dihydroxy derivative metabolites can be applied as new targets for doping control.
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Texto completo: 1 Colección: 01-internacional Base de datos: MEDLINE Asunto principal: Espectrometría de Masas / Cromatografía Líquida de Alta Presión / Ciclobutanos Tipo de estudio: Evaluation_studies Límite: Humans Idioma: En Revista: J Chromatogr B Analyt Technol Biomed Life Sci Asunto de la revista: ENGENHARIA BIOMEDICA Año: 2019 Tipo del documento: Article Pais de publicación: Países Bajos
Texto completo
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Texto completo: 1 Colección: 01-internacional Base de datos: MEDLINE Asunto principal: Espectrometría de Masas / Cromatografía Líquida de Alta Presión / Ciclobutanos Tipo de estudio: Evaluation_studies Límite: Humans Idioma: En Revista: J Chromatogr B Analyt Technol Biomed Life Sci Asunto de la revista: ENGENHARIA BIOMEDICA Año: 2019 Tipo del documento: Article Pais de publicación: Países Bajos