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Title: Hollow-fiber liquid-phase microextraction and gas chromatography-mass spectrometry of barbiturates in whole blood samples
Authors: ALMEIDA, Rafael Menck deLIMA, Diogenes Saulo deSEULIN, Saskia CarolinaLEYTON, VilmaPASQUALUCCI, Carlos AugustoMUNOZ, Daniel RomeroOSSELTON, Michael DavidYONAMINE, Mauricio
Citation: JOURNAL OF SEPARATION SCIENCE, v.35, n.23, p.3361-3368, 2012
Abstract: Here, we present a method for measuring barbiturates (butalbital, secobarbital, pentobarbital, and phenobarbital) in whole blood samples. To accomplish these measurements, analytes were extracted by means of hollow-fiber liquid-phase microextraction in the three-phase mode. Hollow-fiber pores were filled with decanol, and a solution of sodium hydroxide (pH 13) was introduced into the lumen of the fiber (acceptor phase). The fiber was submersed in the acidified blood sample, and the system was subjected to an ultrasonic bath. After a 5 min extraction, the acceptor phase was withdrawn from the fiber and dried under a nitrogen stream. The residue was reconstituted with ethyl acetate and trimethylanilinium hydroxide. An aliquot of 1.0 mu L of this solution was injected into the gas chromatograph/mass spectrometer, with the derivatization reaction occurring in the hot injector port (flash methylation). The method proved to be simple and rapid, and only a small amount of organic solvent (decanol) was needed for extraction. The detection limit was 0.5 mu g/mL for all the analyzed barbiturates. The calibration curves were linear over the specified range (1.0 to 10.0 mu g/mL). This method was successfully applied to postmortem samples (heart blood and femoral blood) collected from three deceased persons previously exposed to barbiturates.
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Artigos e Materiais de Revistas Científicas - FM/MLS
Departamento de Medicina Legal, Ética Médica e Medicina Social e do Trabalho - FM/MLS

Artigos e Materiais de Revistas Científicas - FM/MPT
Departamento de Patologia - FM/MPT

Artigos e Materiais de Revistas Científicas - LIM/22
LIM/22 - Laboratório de Patolologia Cardiovascular

Artigos e Materiais de Revistas Científicas - LIM/40
LIM/40 - Laboratório de Imunohematologia e Hematologia Forense

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