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目的建立一种快速、灵敏、准确测定饮用水中7种痕量酚类化合物的固相萃取-超快速液相色谱-串联质谱分析方法。方法饮用水样经Waters Oasis WAX固相萃取小柱富集与净化,以乙腈和乙酸铵氨水混合溶液为流动相,采用梯度洗脱方式,在Shim-pack XR-ODSⅡ色谱柱(100 mm×2.0 mm,2.2μm)上进行分离,以电喷雾离子源(ESI)多反应监测(MRM)模式下检测,同位素内标法定量。结果 7种酚类化合物在0.1μg/L~100.0μg/L均呈现良好的线性关系(r≥0.999 7),方法的定量限为0.03μg/L~0.50μg/L。当加标水平为0.5μg/L、10.0μg/L和80.0μg/L时,7种酚类化合物的加标回收率为88.6%~103.3%,相对标准偏差(RSD)为0.8%~7.1%。结论本方法可用于饮用水中酚类化合物残留的快速确证与分析。
OBJECTIVE To establish a rapid, sensitive and accurate method for the determination of seven trace phenolic compounds in drinking water by SPE-LC-MS / MS. Methods Drinking water sample was enriched and purified by Waters Oasis WAX SPE cartridge. The mobile phase consisted of acetonitrile and ammonium acetate aqueous solution with gradient elution on a Shim-pack XR-ODS II column (100 mm × 2.0 mm, 2.2μm). The electrospray ionization source (ESI) multi-reaction monitoring (MRM) mode was used for detection. The content was determined by isotope internal standard method. Results The seven phenolic compounds showed a good linearity (r ≥ 0.997) in the range of 0.1μg / L ~ 100.0μg / L. The limit of quantification was 0.03μg / L ~ 0.50μg / L. The spiked recoveries of seven phenolic compounds ranged from 88.6% to 103.3% with relative standard deviations (RSDs) from 0.8% to 7.1% at spiking levels of 0.5 μg / L, 10.0 μg / L and 80.0 μg / . Conclusion This method can be used for rapid confirmation and analysis of phenolic compounds in drinking water.