四氮杂杯[2]芳烃[2]三嗪键合硅胶固相萃取-高效液相色谱法测定河水中硝基苯酚和己烯雌酚

基于四氮杂杯2]芳烃2]三嗪键合硅胶吸附剂（NC-Si），构建了固相萃取-高效液相色谱法同时测定河水中3种硝基苯酚和己烯雌酚的新方法。考察并获得了固相萃取和液相色谱分离的优化条件：将样品溶液pH调至5，以5 mL/min上样，经自制固相萃取柱净化，2 mL氨水-甲醇（2：98，v/v）洗脱；在C8柱上以甲醇-0.1%磷酸溶液为流动相进行梯度洗脱。4种目标分析物的检出限（LOD，S/N=3）为0.03~0.3 μg/L，定量限（LOQ，S/N=10）为0.1~1.0 μg/L；加标回收率为75.5%~104.2%，相对标准偏差（RSD，n=5）小于6.3%。该方法准确、可靠，可用于河水中硝基苯酚及己烯雌酚的灵敏检测。

Solid phase extraction and high performance liquid chromatography with tetraaza[2]arene[2]triazine-bonded silica gel adsorbent for determination of nitrophenols and diethylstilbestrol in river water

A novel method based on solid phase extraction (SPE)-high performance liquid chromatography (HPLC) was developed for the simultaneous determination of nitrophenols and diethylstilbestrol in river water. Tetraaza2]arene2]triazine-bonded silica gel, a homemade SPE adsorbent, was used to enrich the nitrophenols and diethylstilbestrol, and the optimal SPE and HPLC conditions were established. The sample solution was adjusted to pH 5, purified with a lab-made solid phase extraction column, and then eluted with 2 mL ammonia-methanol (2:98, v/v). The enriched sample was separated on a C8 column with methanol and 0.1% phosphoric acid solution as mobile phases in a gradient elution. Under the optimized conditions, the limits of detection (LOD, S/N=3) for the four target analytes were 0.03-0.3 μg/L, and the limits of quantification (LOQ, S/N=10) were 0.1-1.0 μg/L. The recoveries were 75.5%-104.2%, and the relative standard deviations (RSD, n=5) were less than 6.3%. The proposed method is accurate and reliable, and it has been successfully used for determining nitrophenols and diethylstilbestrol in river water.