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配合固相萃取预处理技术,采用HPLC-MS/MS内标分析方法检测了污水厂处理流程及其受纳水体污水水样中的雌激素雌酮(E1)、雌二醇(E2)、炔雌醇(EE2)和硫酸雌酮(E1-3-S)浓度,水样中四种目标物均有检出,受纳水体中E1-3-S的当量浓度分别占到E1当量浓度和计算总雌激素浓度的49.4%和19.1%(均折算为E2当量)。本检测方法色谱峰可有效分离,单个混合样的分析周期为12.0 min,线性范围分别为(0.5~100.1)、(0.4~98.8)、(0.1~99.4)和(0.2~100.0)ng/mL,方法检测限分别为0.5、0.4、0.1和0.2 ng/L,测定结果的精密度及加标回收率均良好。
In combination with SPE, HPLC-MS / MS internal standard method was used to test the treatment process and estrogen estrone (E1), estradiol (E2), alkyne Estriol (EE2) and estrone sulfate (E1-3-S) concentration, water samples were detected in four targets, the equivalent concentration of E1-3-S in the receiving water accounted for E1 equivalent concentration and calculated 49.4% and 19.1% of the total estrogen concentration (both converted to E2 equivalents). The chromatographic peak of this test method can be effectively separated. The analysis period of single mixed sample was 12.0 min with the linear range of (0.5-100.1), (0.4-98.8), (0.1-99.4) and (0.2-100.0) ng / mL, The detection limits of the method were 0.5, 0.4, 0.1 and 0.2 ng / L, respectively. The precision of the determination and the recoveries were all good.