Volume 45 - Issue 2 - 143 - 151

Preparation of Hydrophobic Monolithic Columns for On-line Solid-phase Extraction Coupled with HPLC for the Determination of Trace Level Benzo[a]pyrene

Eser Miktardaki Benzo(a)piren Tayininde HPLC ile Birleştirilmiş On-line Katı-faz Özütlemesi için Hidrofobik Monolitik Kolonların Hazırlanması

Extraction of trace level persistent organic pollutants is an important issue in water samples. So in this work, p(HEMAPA) monolithic columns were developed as a novel kind of solid-phase extraction adsorbents, as well as p(HEMAPA) solid-phase extraction (SPE) adsorbent was coupled with high-performance liquid chromatography (HPLC) (p(HEMAPA-HPLC) for the determination of benzo[a]pyrene (BaP) on-line mode. After p(HEMAPA-HPLC) para- meters including the injection volume, flow rate, and the sample volume had been optimized in detail, BaP separation procedures on the p(HEMAPA-HPLC) containing mobile phase, different amounts of BaP, and reusability were perfor- med. Advantages of this procedure are low quantitation limits (0.05–1.0 ng/mL), short extraction time, low consump- tion of organic solvents, and ease of automation and operation of the whole analysis. The experimental results indi- cated that p(HEMAPA-HPLC) allowed for one-step BaPs extraction, clean-up and analytical determination under the optimal conditions. The reusability of BaPs from water samples was 99.7% with a negligible capacity decrease after ten adsorption–desorption cycles. The method detection limit (MDL), relative standard deviation (RSD) and recovery were obtained as 0.007 ng/mL, 0.26%, and 97.0%, respectively. It was concluded that p(HEMAPA) monolithic column coupled with HPLC was an excellent alternative for the routine analysis of BaPs at trace level. 

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