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 fast,sensitive,and accurate method for simultaneous determination of 7 trace phenolic compounds in drinking water by ultra- fast liquid chromatography- tandem mass spectrometry( UFLC- MS / MS). Methods Drinking water samples were firstly enriched and purified by Waters Oasis WAX solid- phase extraction cartridges,and then UFLC separation was performed on a Shim- pack XR- ODS II( 100 mm × 2. 0 mm,2. 2 μm) with a linear gradient elution program of acetonitrile and with water containing ammonium acetate and ammonium hydroxide as elution solvent. And they were detected by an electrospray ion source( ESI) in the multiple reaction monitoring( MRM) mode,and quantified by internal standard method. Results Calibration curves were linear within the range of 0. 1 μg / L- 100. 0 μg / L( r≥0. 999 7). The limits of quantification( LOQs) were among 0. 03 μg / L- 0. 50 μg / L. Recoveries were among 88. 6%- 103. 3% at the three spiked concentrations of 0. 5 μg / L,10. 0 μg / L,and 80. 0 μg / L. The relative standard deviations( RSDs) were among 0. 8%- 7. 1%. Conclusion The developed method can be applied for the rapid confirmation and determination of phenolic compounds residues in drinking water.