Solid-phase extraction of nitro-PAH from aquatic samples and its separation by reverse-phase capillary liquid chromatography

Journal of the Brazilian Chemical Society

Marcelo Toledo¹  Fernando M. Lanças¹  Emanuel Carrilho¹ 

[1] ,Universidade de São Paulo Instituto de Química de São Carlos São Carlos SP ,Brazil

关键词: nitrated aromatic hydrocarbons;    capillary liquid chromatography;    carcinogenic compounds;    method development;    SPE;   

DOI  :  10.1590/S0103-50532007000500019

来源: SciELO

【 摘 要 】

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.

【 授权许可】

CC BY   
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