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目的建立生活饮用水中壬基酚(nonylphenol,NP)的同位素稀释超高效液相色谱-串联质谱联用(UHPLC-MS-MS)测定方法。方法 NP浓度高于1μg/L的水样经滤膜过滤或高速离心后直接进行UHPLC-MS-MS分析;NP浓度低于1μg/L的水样经固相萃取小柱富集后进行UHPLC-MS/MS分析。结果当NP浓度高于1μg/L时,在1.0～100.0μg/L线性范围内,所得回归方程为y=0.116 3x+0.037 6,相关系数为0.999 8,检出限为0.15μg/L,定量下限为0.5μg/L;当NP浓度低于1μg/L时,在0.005～1.0μg/L线性范围内,所得回归方程为y=1.119 5x-0.001 6,相关系数为0.999 4,检出限为0.001 5μg/L,定量下限为0.005μg/L。该方法的平均加标回收率为92.5%～102.3%,RSD为0.9%～5.6%。结论该方法具有准确快速,灵敏度和准确度均较高,线性范围宽等优点,适用于生活饮用水中NP的检测。
Objective To establish a method for determination of nonylphenol (NP) in drinking water by isotope dilution ultra performance liquid chromatography-tandem mass spectrometry (UHPLC-MS-MS). Methods UHPLC-MS-MS analysis was performed on the water samples with NP concentration higher than 1μg / L by filtration or high-speed centrifugation. The water samples with NP concentration less than 1μg / L were enriched by solid phase extraction (SPE) MS / MS analysis. Results When the concentration of NP was higher than 1μg / L, the regression equation was y = 0.116 3x + 0.037 6 in the linear range of 1.0-100.0μg / L, the correlation coefficient was 0.999 8, the detection limit was 0.15μg / L, When the NP concentration was lower than 1μg / L, the regression equation was y = 1.119 5x-0.001 6 in the linear range of 0.005-1.0μg / L, the correlation coefficient was 0.999 4, the detection limit was 0.001 5μg / L, the lower limit of quantitation was 0.005μg / L. The average recovery of this method was 92.5% ~ 102.3% with RSD of 0.9% ~ 5.6%. Conclusion The method is accurate, rapid, high sensitivity and accuracy, linear range, etc., suitable for the detection of NP in drinking water.