Otimização de método CG-EM/SIM para determinação de HPAs

Abstract

Polycyclic aromatic hydrocarbons (PAHs) comprise a large class of organic compounds, characterized by containing two or more fused aromatic rings in their structure. The study of this class of compounds is necessary because they are found in different environments and associated with the degradation of human health, attributed to a toxic potential, which can lead to mutagenesis and/or carcinogenesis of different cells. The present project was dedicated to the optimization and validation of a chromatographic method for the determination of 16 PAHs in atmospheric particulate matter. Chromatographic conditions were optimized such as: temperature and volume of injection, carrier gas flow rates, temperature programming of the chromatographic oven and detection mode (SIM and SCAN). The optimization was performed through experimental planning with the aid of the Statistica® software, based on the BoxBehnken factorial planning model. The conditions optimized for the CG / EM system include: injection temperature (300ºC), injection volume (2.0 µL), split mode injection (1:10), carrier gas flow rates ((2,0 mL min-1), heating ramp (70ºC/1 min, heating at 180ºC at a rate of 10ºC min-1 and isotherm of 5 min, new heating at 40ºC at a rate of 5ºC min-1 and isotherm of 5 min, inally heating at 300ºC at a rate of 20ºC min-1 and isotherm of 3 min) and selective ion detection mode. It has assessed the influence of each chromatographic parameter on the resolution of the peaks of each HPA. Validation on the method was done following the parameters required by ANVISA and INMETRO (CVmédio ˂ 20%), and presented low detection limits (LDnaftaleno=2,8 mg L-1) and quantification (LQnaftaleno =8,4 mg L-1).