Methodological optimization for determination of benzo(a)pyrene in cachaças by HPLC with fluorescence detection and evaluation of its occurrence / Otimização de metodologia para determinação de benzo(a)pireno em cachaças por CLAE com detecção de fluorescência e avaliação de sua ocorrência

ABSTRACT

The objectives of the present study were to compare, to adapt and to validate analytical methodology for identification, and quantification of benzo(a)pyrene (BaP) in cachaça samples by HPLC-DFl and confirmation by GC/MS; also, to evaluate the BaP levels in cachaças commercialized in São Paulos market, and to verify which stages of one production of still cachaça could contribute for BaP contamination. Three distinct methods for BaP extraction were studied solid phase extraction (SFE), liquid-liquid extraction with cyclohexane (LLE-CHX) and liquid-liquid extraction with N,N dimethyllformamideand cyclohexane (LLE-DMF/CHX). SFE extraction used a C18 cartridge in silica base (500mg, 6 mL) and cyclohexane, while the LLE consisted on sample partition in appropriate solvent and purification by column chromatography on silica gel. The extracts obtained from all extractions were evaporated to dryness, reconstituted in acetonitrile and analyzed by HPLC-DFl. Chromatography separation was carried out on a column C18 (25 cm; 0.45 m; 4.6 mm) using acetonitrile/water (7030) as mobile phase at a flow rate of 1mL/min. The response of fluorescence detector was linear for BaP standard solutions ranging from 0.05 to 30 ppb (R2=0.9995). The detection and quantification limits were 0.03 ppb and 0.1 ppb for all methods. Recoveries values at 3 concentration levels (0.1, 1.0, 3.0 ppb) (n=3) ranged

RESUMO

iptesenta resumo em inglês.