DANIEL ROMERO MUñOZ
Projetos de Pesquisa
Unidades Organizacionais
Departamento de MedicinaLegal, Ética Médica e Medicina Social e do Trabalho, Faculdade de Medicina - Docente
LIM/40 - Laboratório de Imunohematologia e Hematologia Forense, Hospital das Clínicas, Faculdade de Medicina
LIM/40 - Laboratório de Imunohematologia e Hematologia Forense, Hospital das Clínicas, Faculdade de Medicina
2 resultados
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- Determination of antidepressants in whole blood using hollow-fiber liquid-phase microextraction and gas chromatography-mass spectrometry(2014) SANTOS, Marcelo Filonzi dos; FERRI, Caio Caleiras; SEULIN, Saskia Carolina; LEYTON, Vilma; PASQUALUCCI, Carlos Augusto Goncalves; MUNOZ, Daniel Romero; YONAMINE, MauricioA hollow-fiber liquid-phase microextraction (HF-LPME), used in three-phase mode, and combined with gas chromatography-mass spectrometry (GC-MS), was developed to quantify antidepressants and their major metabolites (amitriptyline, nortriptyline, imipramine, desipramine, clomipramine, desmethylclomipramine, fluoxetine, and norfluoxetine) in whole blood samples, using their deuterated analogs as internal standards. The HF-LPME system comprised a disposable 8-cm polypropylene porous hollow fiber, 4.0 ml of sample solution (0.5 ml of blood added to 3.5 ml of 0.1 M NaOH: donor phase), dodecane (organic phase), and 0.1 M formic acid (acceptor phase) for extraction. After stirring the system, the acceptor phase was evaporated under a nitrogen stream and resuspended in 30 mu l of methanol. Derivatization was not required. A 2.0-mu l aliquot of this solution was injected into a GC-MS system. The method was validated after the optimization of several parameters that may influence the extraction efficiency. The limits of quantification for all antidepressants were below the therapeutic levels (20.0 ng/ml). The average intraday and interday precisions were within 9.7 and 9.8 %, respectively, for all analytes. The calibration curves were linear in the concentration range of 20-1,200 ng/ml. The developed method was applied to seven actual postmortem samples. Tricyclic antidepressants were detected in all of the analyzed cases. To our knowledge, this is the first demonstration of usefulness of HF-LPME for analysis of antidepressants in postmortem forensic cases.
- Hollow fiber-liquid phase microextraction of barbiturates in liver samples(2013) MENCK, Rafael Almeida; OLIVEIRA, Carolina Dizioli Rodrigues de; LIMA, Diogenes Saulo de; GOES, Ligia Endo; LEYTON, Vilma; PASQUALUCCI, Carlos Augusto; MUNOZ, Daniel Romero; YONAMINE, MauricioBarbiturates, especially phenobarbital, are involved in intoxication cases in Brazil and other countries. Liver tissue can be a useful alternate specimen when blood is not available (decomposition, severe fire, and exsanguination cases). Because the liver is a very complex matrix, it is essential is to eliminate potential interfering substances in this specimen before instrumental analysis of target compounds. In recent years, novel strategies for sample preparation have gained acceptance in the field of analytical toxicology. The objective of this work was to develop a gas chromatography-mass spectrometry (GC-MS) method using hollow fiber-liquid phase microextraction (HF-LPME) for determination of barbiturates (phenobarbital, secobarbital, pentobarbital, and butalbital) in liver samples. An aliquot of homogenized and acidified liver in aqueous solution (equivalent to 50 mg tissue) was submitted to extraction by the use of a 9-cm hollow fiber. The fiber was filled with eucalyptus oil in its pores and its lumen was filled with a NaOH solution (pH 13; acceptor phase). After extraction in an ultrasonic bath for 5 min, the acceptor phase was withdrawn and derivatized in the injector port of the GC-MS with trimethylanilinium hydroxide for flash methylation. A totally ""green chemistry"" approach of the sample extraction was obtained, because relatively large amounts of organic solvent generally used for extraction could be substituted by an essential oil used as a supported liquid membrane for HF-LPME. This method was validated and successfully applied to liver samples collected from five deceased persons with previous history of exposure to barbiturates. Phenobarbital concentrations in the liver found in these actual cases ranged from 1.3 to 16.7 mu g/g.