Miniaturisated method for the analysis of polycyclic aromatic hydrocarbons in leaf samples

A new methodology is proposed for monitoring 16 priority polycyclic aromatic hydrocarbons, using tree leaves as passive samplers, by means of a mini-ultrasonic probe coupled with reversed-phase liquid chromatography (RP-LC) and fluorescence (FL) detection. Separation and detection of the 16 PAHs were completed in 19 min, using a 3 μm (particle size) C18 column RP-LC with acetonitrile–water gradient elution. The ultrasonic probe device used was equipped with a 2 mm titanium tip, and sample and solvent amounts used were just 50 mg and 1 mL, respectively. Multivariate optimisation of the variables affecting extraction was conducted by means of full factorial analysis to determine which of the variables were significant. A central composite design was applied to define surface responses and to calculate optimal values for the variables. The accuracy of the method was determined by both analysis of a Certified Reference Material with a similar matrix (IAEA-140 OC, seaweed) and by comparison of the results obtained with those from a previously developed method. The proposed analytical method avoids some of the main problems encountered in the determination of PAH in complex matrices; no clean-up step is necessary, consequently sample preparation time and costs can be significantly reduced. The developed method was applied to determine PAH in leaf samples from medlar and red and white mangrove trees, situated near PAH pollution sources.