シアノプロピル結合相を用いる固相抽出とガスクロマトグラフィー/質量分析法による in situ アセチル化後のビスフェノール A の定量

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Before the determination of bisphenol A (BPA) by GC/MS, it is preferable to convert it to a less polar compound to eliminate the adsorption of a polar analyte on the wall of the instrument and to obtain a sharp peak in the chromatogram and a high sensitivity. Although it seems that in situ acetylation producing the acetyl derivative of BPA (BPADA) is simple and rapid, for solidphase extraction (SPE) an undesirably low recovery may result from a possible strong interaction between BPADA and the solid-phase. Thus, the octadecyl-bonded phase (C_18 phase) and the cyanopropyl-bonded phase (CN phase) were compared for the SPE of BPADA at the 0.1 μg ml^-1 level. The former is an apolar phase and the latter has intermediate polarity. The results showed that the CN phase gave more satisfactory results than the C_18 phase for recovery and precision. Furthermore, for trace determination with SPE/GC/MS after in situ acetylation, it was found that the cyanopropyl phase gave a lower blank and a lower detection limit compared with the C_18 phase. Using the cyanopropyl phase and a 500 ml of sample solution, the detection limit was 0.09 ng and the recoveries of 5.0 and 10.0 ng of BPA were 107±6 and 99.6±2.8% (mean ± standard deviation) for four repeated runs, respectively. The present method was applied to the study of a degradation of BPA due to chlorine in tap water.
社団法人日本分析化学会の論文
2002-03-05