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

E ser miktardaki kalıcı organik kirleticilerin su örneklerinde özütlemesi önemli bir konudur. Bu nedenle bu çalışmada, yeni nesil katı-faz özütleme adsorbenti olarak p HEMAPA monolitik kolon geliştirilmiş, aynı zamanda, p HEMAPA katı-faz özütleme adsorbenti yüksek performanslı sıvı kromatografisi ile birleştirilerek p HEMAPA-HPLC on-line modda benzo a piren’in tayini gerçekleştirilmiştir. Enjeksiyon hacmi, akış hızı, ve örnek hacmi gibi HPLC parametreleri incelendikten sonra, ayırma işlemlerinde BaP derişimi, hareketli faz ve tekrar kullanılabilirlik çalışmaları gerçekleştirilmiştir. Bu yöntemin avantajları düşük tayin sınırı 0.05–1.0 ng/mL , kısa özütleme zamanı, düşük organik çözücü tüketimi ve tüm analiz boyunca çalışma ve otomasyonun kolay olmasıdır. Deneysel sonuçlar, optimum koşullar altında p HEMAPA-HPLC ile BaP özütlemesi, ayırımın ve analitik tayinin tek adıma gerçekleştiğini kanıtlamıştır. On kez ardı ardına tekrarlanan adsorpsiyon-desorpsiyon işlemi sonucunda adsorpsiyon kapasitelerinde önemli bir kayıp olmadan tekrar kullanılabilirlik %99.7 olarak bulunmuştur. Yöntem tayin sınırı MDL , standart sapma ve geri kazanım sırasıyla 0.007 ng/mL, %0.26, and %97, olarak hesaplanmıştır. HPLC ile birleştirilen p HEMAPA monolitik kolonun eser seviyedeki BaP’ın rutin analizi için mükemmel bir alternatif olduğu kanıtlanmıştır

Anahtar Kelimeler:

Monolitik kolon, yüksek performanslı sıvı kromatografisi, katı-faz özütleme, benzo a piren

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

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.

Keywords:

monolithic column HPLC, High performance liquid chromatography, solid-phase extraction, benzo[a]pyrene,

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