制备了聚(甲基丙烯酸-乙二醇甲基丙烯酸酯)有机聚合材料用于微固相萃取吸附剂,结合超高效液相色谱-串联三重四级杆质谱,建立了膜保护微固相萃取快速测定水体中E1、E2、E3、EE2和BPA 5种典型雌激素的方法。详细研究了萃取条件和解析条件对萃取效果的影响。在优化实验条件下,E3的检出限为0.2μg/L,线性范围为1~500μg/L,其余4种目标物检出限为0.02μg/L,线性范围为0.1~500μg/L。相对标准偏差均小于7.4%。方法用于实际污水处理厂污水中痕量雌激素的测定,样品加标回收率大于83%。
Poly (methacylic acid-ethylene glycol dimethacrylate) (poly (MAA-EGDMA)) has been applied as a micro-solid phase extraction (μSPE) adsorbent. In combination with ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS-MS), μSPE method was established to determine five estrogens. Some important parameters were intensively optimized. Under the most favorable extraction conditions,the linear ranges and LODs of El, E2, EE2 and BPA are 0. 1-500 μg/L and 0.02 μg/L (except for E3, those of 1-500 μg/L and 0.2 μg/L, respectively). The RSDs of five estrogens were observed less than 7.4%. The method was applied to the determination of real samples from sewage plant,and the recoveries were above 83%.