PYE컬럼 HPLC와 GC-ECD를 이용한 연안환경 시료의 PBDEs의 분석

Abstract

Measurement of toxicologically relevant Polychlorinated biphenyl (PCB) congeners such as non-ortho (IUPAC#) 77, 81, 126 and 169 and mono-ortho 105, 114, 118, 123, 156, 157, 189 and di-ortho 170, 180 and Polybrominated diphenyl ethers (PBDEs) such as 47, 66, 85, 99, 100, 138, 153, 154 in environmental samples become almost mandatory in several countries now. However, most of the available methods involve expensive instrumentations such as HRGC-HRMS or ECNI-LRMS, apart from expensive extraction and clean-up (large volume of solvents) steps. A method has been devised combining the analytical separation power of PYE [2-(1-pyrenyl)ethyldimethysilylated silica] column HPLC and high-resolution gas chromatographic techniques including micro- electron capture detection (ECD) and two dimensional gas chromatograpy-ECD techniques to determine these eco-toxic substances at parts-per-trillion (ppt) levels. This combination resolves co-elution of congeners that occur in disproportationate ratios (eg. CB-110 and -77) and allows accurate congener-specific determination of target compounds. This method is cost effective as it involves only hexane, that in small quanties (10ml) and GC-ECD. The elution and analysis time are optimized to involve less human hours. This method is effectively utilized in the analysis of co-planar CBs and PBDEs from archived solvent extracts of samples previously analysed for pesticides and PCBs. Structure based separation of contaminant classes improves GC-ECD determination with extreme low volume micro-concentration at ppt levels.