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基于金属有机骨架材料分散固相萃取-高效液相色谱法检测环境水体中两种磺胺类药物 被引量:7

Determination of Two Sulfonamides in Environmental Water Based on Dispersivesolid-Phase Extraction with MIL-101(Cr) Metal-Organic Framework
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摘要 比较了3种金属有机骨架材料(MIL-101(Cr)、MIL-101(Cr)-SO3H和MIL-101(Cr)-NH2)在不同pH的环境水体中对两种磺胺类药物(磺胺对甲氧嘧啶和磺胺氯哒嗪)的吸附性能,从而选择出最佳吸附剂及pH条件。研究发现pH为9时MIL-101(Cr)吸附性能最佳,进而对影响吸附及解析效率的主要因素,如吸附剂使用量、吸附时间和解析溶剂及其用量、解析时间等进行优化。优化后的最佳实验条件为:每10.0 mL样品溶液(pH=9)中加入6.0 mg的MIL-101(Cr)吸附剂,吸附4.0 min,离心去掉上清液,然后用1.5 mL的甲酸-甲醇溶液解析-10.0 min后离心。结果表明:2种磺胺类药物在5.0~8000μg/L范围内线性良好且相关系数均大于0.9990,方法检出限以信噪比(S/N=3)计磺胺对甲氧嘧啶和磺胺氯哒嗪分别为0.08μg/L、0.05μg/L,3种浓度加标回收率为71.2%~91.9%,相对标准偏差为3.1%~8.5%。 Three metal-organic frameworks(MIL-101(Cr),MIL-101(Cr)-SO3H,MIL-101(Cr)-NH2)were used as adsorbents,and the adsorption properties of sulfadiazine and sulfadiazine were compared in environment water under different pH conditions by solid phase dispersion extraction.With MIL-101(Cr)as the best adsorbent,the main factors affecting the efficiency of adsorption and desorption,such as the amount of adsorbent used,adsorption time,type and amount of desorption solvent,and desorption time were investigated.The optimized extraction conditions were as follows:10.0 mL of sample solution(pH=9.0)was extracted with 6.0 mg of MIL-101(Cr)adsorbent for 4.0 min,the supernatant was removed by centrifugation,and the sample was resolved with 1.5 mL of 2%(volume fraction)formic acid-methanol solution for 10.0 min.The results show that the linear range of two sulfonamides are 5.0~8000μg/L,and r>0.9990.The detection limits of the method are 0.05μg/L to 0.08μg/L.The recoveries of the three spiked concentrations are from 71.2% to 91.9%.The relative standard deviations(RSDs)are in the range of 3.1%~8.5%.
作者 张鸣珊 李腾崖 雷宇 吴艳 何书海 ZHANG Ming-Shan;LI Teng-Ya;LEI Yu;WU Yan;HE Shu-Hai(Hainan Ecological Environment Monitoring Center,Haikou 571126,China)
出处 《应用化学》 CAS CSCD 北大核心 2021年第2期236-244,共9页 Chinese Journal of Applied Chemistry
关键词 金属有机骨架材料 分散固相萃取 磺胺类药物 环境水体 Metal-organic frameworks Dispersive solid-phase extraction Sulfonamides Environmental water
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