Determination of toxaphene enantiomers by comprehensive two-dimensional gas chromatography with electron-capture detection

Comprehensive two-dimensional gas chromatography with micro electron-capture detection (GC × GC–μECD) has been evaluated for the enantioseparation of five chiral toxaphenes typically found in real-life samples (Parlar 26, 32, 40, 44 and 50). From the two enantioselective β-cyclodextrin-based columns evaluated as first dimension column, BGB-176SE and BGB-172, the latter provided the best results and was further combined with three non-enantioselective columns in the second dimension: HT-8, BPX-50 and Supelcowax-10. The combination BGB-172 × BPX-50 was finally selected because it provided a complete separation among all enantiomers. A satisfactory repeatability and reproducibility of the retention times in both the first and the second dimension were observed for all target compounds (RSDs below 0.8%, n = 4). Linear responses in the tested range of 10–200 pg/μl and limits of detection in the range of 2–6 pg/μl were obtained. The repeatability and reproducibility at a concentration of 100 pg/μl, evaluated as the RSDs calculated for the enantiomeric fraction (EF), was better than 11% (n = 4) in all instances. The feasibility of the method developed for real-life analyses was illustrated by the determination of the enantiomeric ratios and concentration levels of the test compounds in four commercial fish oil samples. These results were compared to those obtained by heart-cut multidimensional gas chromatography using the same enantioselective column.Financial support was acquired from project 07G/0038/2003 CAM and AGL 2004-02072/ALI-CICYT. L.R.B. thanks CAM for financial support.Peer reviewe