固相抽出-液体クロマトグラフ-質量分析計による水道水中フェノール類の検査法の開発とその妥当性評価

摘要

In order to develop a simple and rapid analytical method for phenols (phenol and chlorophenols) in drinking water, solid phase extraction and liquid chromatography mass spectrometry (SPE-LC/MS) method was examined. We established the LC condition with excellent peak separation of 15 phenols and developed the method by which pretreatment time was shortened to less than half. To evaluate the accuracy and precision of developed analytical method, two set points validation test was conducted to determine the recovery of phenols from tap water with nine organizations. Satisfactory results were obtained about accuracy (recovery) in two set points. Reproducibility (RSD%) of nine organizations in two set points was less than 20% (except one organization, 22.1% (2-chlorophenol) and the value of precision between laboratories was less than 30% (3.55%-13.9%) in two set points. Because excellent results were obtained about accuracy (recovery), repeatability, and precision between laboratories by validation test, we concluded that this analytical method can be adopted to a standard analytical method for phenols in drinking water in Japan.%水道水中フニノール類の標準検査法を迅速•簡便化するため、固相抽出-液体クロマトグラフ-質量分析法を検討した。その結果、全15化合物のピーク分離が良好なLC条件を確立し、また、固相カラムの乾燥時間の短縮化や溶出溶媒量の少量化等により、前処理時間を現行法の1/2以下に大幅に短縮できる方法を開発した。開発した検査法について、多施設共同試験による妥当性評価試験を実施した。水道水を用いて添加回収試験を行い、妥当性評価ガイドラインの性能パラメータが目標を満たすか評価した結果、真度(回収率)、併行精度及び室間精度から外挿して評価した室内精度も目標を満たしたことから、本検査法は妥当であると判断した。