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目的:建立水中壬基酚、辛基酚和双酚A的酚类环境雌激素的高效液相色谱-串联质谱测定方法。方法:水样中目标组分采用OASIS固相萃取柱富集,二氯甲烷洗脱,吹氮浓缩至近干并置换溶剂为甲醇水溶液。Waters Xbridge C18质谱柱分离,以甲醇-0.1%氨水为流动相,梯度洗脱后在LC/MS/MS多反应监测模式下进行定性定量分析。结果:水样平均加标回收率74%～106%,相对标准偏差4.8%～13.5%,壬基酚、辛基酚和双酚A的方法检出限为0.0016μg/L～0.0030μg/L。应用建立的方法对珠澳地区西江水源水中酚类环境雌激素进行连续动态监测分析,浓度范围为0.05μg/L～0.72μg/L。结论:本法具有非常高的选择性、灵敏度和准确度,完全能满足水中痕量酚类环境雌激素的高灵敏分析。
Objective: To establish a method for the determination of phenolic environmental estrogens in nonylphenol, octylphenol and bisphenol A in water by high performance liquid chromatography-tandem mass spectrometry. Methods: The target components in water samples were enriched by OASIS solid phase extraction column, eluted with dichloromethane, concentrated to near dry nitrogen by nitrogen and replaced with methanol. Waters Xbridge C18 column with methanol-0.1% aqueous ammonia as the mobile phase, gradient elution and qualitative and quantitative analysis in LC / MS / MS multiple reaction monitoring mode. Results: The average recoveries were 74% -106% with relative standard deviations of 4.8% ~ 13.5%. The detection limits of nonylphenol, octylphenol and bisphenol A were 0.0016μg / L ~ 0.0030μg / L . The established method was used to continuously monitor the phenolic environmental estrogens in the water of Xijiang River in Zhuhai and Macao regions in the range of 0.05μg / L ~ 0.72μg / L. Conclusion: This method has a very high selectivity, sensitivity and accuracy, fully meet the high sensitivity of trace phenols in the water of estrogen.