Abstract
In this work, an analytical methodology to extract 1-nitronaphthalene, 2-nitrofluorene, 9-nitroanthracene, 3-nitrofluoranthene, and 1-nitropyrene aquatic samples is proposed. Capillary liquid chromatography with on-column UV detection (µLC-UV) was employed to separate and quantitate all five nitrated polycyclic aromatic hydrocarbons (nitro-PAH) extracted from water samples. Two different extraction techniques were tested and compared: liquid-liquid extraction (LLE) and solid phase extraction (SPE) with two different sorbents, octadecylsilica (C18) and styrene divinylbenzene (XAD-2) particles. The elution of analytes was tested with both acetonitrile and methylene chloride. The best recovery results were obtained for SPE-C18 extraction with the methylene chloride with values ranging from 76 to 97% with RSD values smaller than 4%. The chromatographic conditions for analysis was carried out using a 250 × 0.3 mm i.d. packed capillary column with 5 µm C18 particles. The elution was isocratic with 65% acetonitrile in water (v/v) as mobile phase with a flow rate of 7 µL min-1. The detection limits due to on-column UV detection (ranging ~3-30 mmol L-1) are limiting for environmental applications, however, they are suited for toxicological studies.
Highlights
Nitrated polycyclic aromatic hydrocarbons are compounds of broad environmental importance
Since this pump is provided with just one piston, it does not allow either on-line solvent composition nor gradient elution, the optimization of the separation of all 5 nitro-PAH had to conducted in isocratic mode with fine adjustment of the eluent composition
The values of limit of detection (LOD) found for the μLCUV system were between 0.8 and 5.8 mg L-1, depending on the response factor of each analyte
Summary
Nitrated polycyclic aromatic hydrocarbons (nitroHPA) are compounds of broad environmental importance. Vol 18, No 5, 2007 in order to determine its carcinogenic and mutagenic potential Among these studies, the Ames Salmonella test has evidenced that nitro-PAH generally are more mutagenic than its correspondent PAH.[6] is important to assess the presence and the effects of nitroPAH in tropical countries since there is a high incidence of sunlight. The concentration range for each nitro-PAH varied to their sensitivity at each selected wavelength, they were all between 2 and 80 mg L-1 For both liquid-liquid and solid-phase extraction schemes, 100 mL of ultra pure water were spiked with 75 μg of each nitro-PAH (0.75 mg L-1). The pHs of the water samples were lowered to ~ 2 with HCl 2 mol L-1 to suppress microbiologic activity and were filtrated in 0.45-μm pore filter prior to analysis
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