【摘要】 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0.03～0.3μg/L,定量限(LOQ,S/N=10)为0.1～1.0μg/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。更多还原

【Abstract】 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. Tetraaza[2]arene[2]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.更多还原