水中双酚类化合物的固相萃取-超高效液相色谱-串联质谱检测法

Determination of bisphenols in water by solid phase extraction and ultra performance liquid chromatography-tandem mass spectrometry

目的建立水中双酚A、双酚B、双酚F三种双酚类化合物固相萃取一超高效液相色谱一串联质谱同时测定方法。方法水样经Cts小柱富集，乙腈洗脱，串联质谱仪检测，利用AcquityBEHC18色谱柱分离，以乙腈-0．1％氨水溶液为流动相梯度洗脱，流量0．3ml／min，以双酚A—d16为内标。结果三种双酚类化合物在1．0-100．0μg／L线性范围内具有良好的线性关系，r≥0．999；该方法的检出限为0．75-1．0ng／L，平均回收率为87．0％-106．9％，RSD为1．61％～3．67％。结论该方法灵敏、准确，适用于水中痕量双酚A、双酚B、双酚F的同时检测。

Objective To establish an analytical method for the determination of three bisphenols in water by ultra performance liquid chromatography-tandem mass spectrometry （UPLC-MS-MS）. Methods The water samples were extracted and condensed with solid-phase extraction using C18 cartridges and eluted by acetonitrile. Separation was carried out with Acquity BEH C18 column and detection were performed by UPLC-MS-MS. The gradient mobile phase was consisted of acetonitrile and 0.1% ammonia water at a flow rate of 0.3 ml/min. Quantification was calculated by an internal standard method with BPA-d16. Results The linear correlation coefficients of three bisphenols in the range of 1.0-100.0 μg/L were all over 0.999.The minimum detectable concentrations were 0.75-1.0 ng/L,and the rates of recovery ranged from 87.0% to 106.9%. RSDs were between 1.61% and 3.67%. Conclusion This method is simple,sensitive, accurate and applicable to the determination of the bisphenols compounds in source water and drinking water.