【摘要】 环境雌激素（EEs）在畜禽和水产养殖业中存在被非法滥用的现象，对环境和生物样品中EEs的定量检测是实现其应用监管的基础。由于环境和生物样品中EEs的残留量常为痕量或超痕量，并且共存组分复杂，因此以富集目标化合物和净化基质为目标的样品前处理方法就显得尤为重要。基于苯并噻吩（BT）的极性共轭芳环可能对EEs产生良好的吸引作用，以其作为聚合单体与对二氯苄（DCX）合成超交联聚合物BT-DCX，建立该聚合物作为吸附剂的固相萃取（SPE）、高效液相色谱（HPLC）分离和紫外（UV）检测的EEs测定方法。BT-DCX对甲醇溶液中三种EEs(17β-E2、EE2和DES)的饱和吸附容量分别为5.34 mg/g、2.17 mg/g和3.11 mg/g；在最佳萃取条件下，对50 mL0.08 mg/L 17β-E2、EE2和DES的萃取回收率分别为87.6%、96.2%和92.2%。10次重复使用，EEs回收率没有明显变化，表现出良好的重复使用性能。建立的SPE-HPLC-UV分析方法的线性范围为2.0～1 000.0μg/L，检出限在0.4～0.7μg/L之间，日内和日间相对标准偏差在6.1%以下。方法成功用于湖水、鱼肉、鸡粪等复杂基体样品中EEs的检测，样品加标回收率在74%～114%之间。方法灵敏、稳定，样品测定结果令人满意。更多还原

【Abstract】 There are cases of illegal abuse of environmental estrogens(EEs) in the livestock, poultry and aquaculture industries. Quantitative detection of EEs in environmental and biological samples is the basis for supervising their application. Since the residual amount of EEs in environmental and biological samples is often trace or ultra-trace, and the coexisting components are complex, sample pretreatment methods aimed at enriching target compounds and purifying the matrix are particularly important. Based on the fact that the polar conjugated aromatic ring of benzothiophene(BT) may exert a strong affinity for EEs, BT was used as a monomer to synthesize the hypercross-linked polymer BT-DCX with α, α’-dichloro-p-xylene(DCX). A method for the determination of EEs was established by solid-phase extraction(SPE), high-performance liquid chromatography(HPLC) separation and ultraviolet(UV) detection using this polymer as the adsorbent. The saturated adsorption capacities of BT-DCX for three EEs(17β-E2, EE2 and DES) in methanol solution are 5.34 mg/g, 2.17 mg/g and 3.11 mg/g, respectively. Under the optimal extraction conditions, the extraction recoveries of 17β-E2, EE2 and DES from 50 mL of 0.08 mg/L solution were 87.6%, 96.2% and 92.2%, respectively. After 10 repeated uses, the recovery rates of EEs showed no significant change, indicating good reusability. The established SPE-HPLC-UV analytical method has a linear range of 2.0-1 000.0 μg/L, a detection limit ranging from 0.4 μg/L to 0.7 μg/L, and intra-day and inter-day relative standard deviations(RSDs) of less than 6.1%.This method has been successfully applied to the detection of EEs in complex matrix samples such as lake water, fish meat and chicken manure, with spiked recoveries ranging from 74% to 114%. The method is sensitive, stable, and the sample determination results are satisfactory.更多还原