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Master's Dissertation
DOI
10.11606/D.9.2007.tde-10042007-150259
Document
Author
Full name
Daniela Mendes Louzada de Paula
E-mail
Institute/School/College
Knowledge Area
Date of Defense
Published
São Paulo, 2007
Supervisor
Committee
Moreau, Regina Lúcia de Moraes (President)
Marcourakis, Tânia
Martinis, Bruno Spinosa de
Title in Portuguese
Análise toxicológica de antidepressivos em sangue total por cromatografia em fase gasosa com detector de nitrogênio e fósforo
Keywords in Portuguese
Antidepressivos
Cromatografia gasosa
Extração em fase sólida
Intoxicação
Sangue total
Abstract in Portuguese
Um método cromatográfico foi desenvolvido para determinação dos antidepressivos mais prescritos no Brasil e seus produtos de biotransfomação (amitriptilina, imipramina, clomipramina, desmetilclomipramina, desipramina, nortriptilina, fluoxetina, norfluoxetina e sertralina) em sangue total por cromatografia em fase gasosa com detector de nitrogênio e fósforo. A extração em fase sólida (EFS) com o cartucho abselutTM NEXUS foi empregada de forma inovadora. O procedimento de extração consistiu na diluição de 0,5mL de sangue total em tampão (pH 9,5), aplicação da amostra no cartucho, remoção de interferentes usando tampão (pH 9,5) e eluição dos analitos com diclorometano/ isopropanol (17/3 v/v); a etidocaína foi adotada como padrão interno. Os limites de detecção (LD) e quantificação (LIQ) encontrados foram de 0,1mg/L a 0,4mg/L e de 0,4mg/L a 1,6mg/L, respectivamente. O método foi preciso, específico e linear na faixa de concentração estudada (do LIQ até 12mg/L). A recuperação média de todos os analitos foi 65,5%. O método foi aplicado em amostras de âmbito forense e de emergência clínica.
Title in English
Toxicology analysis of antidepressants in whole blood with gas chromatography and nitrogen-phosphorus detection
Keywords in English
Antidepressants
Gas chromatography
Intoxication
Solid phase extraction
Whole blood
Abstract in English
A gas chromatographic method was developed to determine antidepressants most prescribed in Brazil and their metabolites (amitriptyline, imipramine, clomipramine, desmethylclomipramine, desipramine, nortriptyline, fluoxetine, norfluoxetine, and sertralina) in whole blood, using solid phase extraction and gas chromatography with nitrogen-phosphorus detection. The solid-phase extraction (SPE) with abselutTM NEXUS was applied in an innovative manner. The extraction procedure consists of the dilution of 0.5mL of whole blood in buffer (pH 9.5), application of the sample in the cartridge, washing with buffer (pH 9.5) and elution of the analytes with dichloromethane/isopropanol (17/3, v/v). The limit of detection (LOD) and quantification (LLOQ) were from 0.1mg/L to 0.4mg/L and from 0.4mg/L to 1.6mg/L, respectively. Etidocaine was used as internal standard. The method was precise, specific and linear in the studied concentration (range from LLOQ to 12mg/L). The average recovery of all analytes was 65,5%. Forensic and clinical emergency samples were submitted to the validated method.
 
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DanielaPaula.pdf (1.03 Mbytes)
Publishing Date
2007-05-04
 
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