固相萃取-液相色谱-串联质谱法测定水源水中的壬基酚、辛酚和双酚A

Determination of nonylphenol,octylphenol bisphenol A in raw water by liquid chromatography tandem mass spectrometry with solid phase extraction

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 ： A method for the determination of nonylphenol, octylphenol and bisphenol A in source wa- ter by solid -phase extraction coupled with liuid chromatography tandem Mass Spectrometry （LC -MS/MS）was de- veloped. Methods： The targets in sources of drinking water were concentrated on Waters Osasis HLB solid - phase column and eluted with methylene chloride , evaporated under nitrogen gas to near dryness and then reconstituted in methanol aqueous solution. The extract components were separated completely on a Waters Xbridge C 18 column with methanol - 0.1% NH4OH gradient elution and simultaneously quantified under the multiple reaction monitoring （MRM） mode. Results： The average recoveries of spiked water sample ranged from 74% - 106% and their relative standard deviation varied between 4.8 % and 13.5 %. The limits of detection （LODs） for nonylphenol, octylphenol and bisphenol A were between 0. 0016 μg/L-0. 0030μg/L. The method was applied to analyze raw water from West River access to South Sea in Zhuhai - Macao region, where concentrations for phenol environmental estrogens ranged from 0.05 μg/L to 0.72 μg/L. Conclusion： The method was selective, sensitive, accurate, completely suitable for determination of trace environmental estrogens in sources of drinking water.