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| Abstract |
We developed a new analytical method for accurately determining concentrations of polychlorinated dibenzo-p-dioxins (PCDDs), polychlorinated dibenzofurans (PCDFs) and non-ortho-coplanar polychlorinate...d biphenyls (Co-PCBs) at a blood volume of 5g. The method consists of three major steps, the extraction of lipid from human blood by an accelerate solvent extractor (ASE) system, a clean-up procedure at a scale one-fourth that of the conventional method, and a sensitive determination method by a high-resolution gas chromatography/high-esolution mass spectrometry (HRGC/HRMS) equipped with a solvent cut large volume (SCLV) injection system as a large volume injection technique. By the improvement of the pretreatment method, the operation time and consumption of the solvent could be drastically reduced, and the sensitivity of the GCMS with the SCLV injection system was increased to 10 times the level of the classical method. From the results of the PCDDs, PCDFs and Co-PCBs concentrations measured by the developed method and the conventional method using the same blood sample, it was confirmed that the measurement became possible at a blood volume of 5g. The developed method is more effective than the conventional method for treating many samples within a short period of time with high reproducibility.
5gの血液量でダイオキシン類分析を可能にする測定系および血液試料の前処理法を検討した. すなわち, 高速溶媒抽出装置による血液試料からの脂質の抽出法, 従来法の1/4スケールでのカラムクリーンアップ法および大量溶媒注入装置(SCLVinjectionsystem)を装備したHRGC/ HRMSを用いて高感度測定の一連の分析方法について検討し, 超高感度迅速分析法を確立した. 大量溶媒注入装置の装備によりHRGC/HRMSの相対感度は10倍程度向上した. 同一の血液を用いて行った従来法との比較検討結果から, 5gの血液量でもダイオキシン類濃度が十分測定可能であることを確認された. さらに, 従来法に比べ血 液試料の前処理段階で費やす時間を大幅に短縮することができた. 本法は5g程度の少量の血液量でダイオキシン類を測定できるだけでなく, 多数のサンプルを効率よく, かつ迅速に処理するのに効果的な方法である.show more
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