磁性二氧化硅复合材料制备及其对磺酰脲类除草剂的吸附研究  

Preparation of magnetic silica composites and adsorption studies on sulfonylurea herbicides

作　　者：张颖 叶宇航 司文帅[2] ZHANG Ying;YE Yu-hang;SI Wen-shuai(Shanghai University of Medicine&Health Sciences,Shanghai 201318,China;Institute for Agro-Food Standards and Testing Technology,Shanghai Academy of Agricultural Sciences,Shanghai 201403,China)

机构地区：[1]上海健康医学院药学院,上海201318 [2]上海市农业科学院质量标准与检测技术研究所,上海201403

出　　处：《化学研究与应用》2025年第2期482-487,共6页Chemical Research and Application

摘　　要：采用共沉淀法制备四氧化三铁(Fe_(3)O_(4)),溶胶凝胶法制得SiO_(2)溶胶,利用二者间的静电作用制备了磁性二氧化硅复合材料(Fe_(3)O_(4)@SiO_(2))。借助XRD、SEM、VSM、FTIR等方法对Fe_(3)O_(4)@SiO_(2)进行表征,结果表明,所得材料的粒径为20 nm左右,BET比表面积约为59 m^(2)/g,平均孔径9.8 nm,具有超顺磁性(39.7 emu/g)。将该复合材料用作磁固相萃取(magnetic solid-phase extraction,MSPE)的吸附剂,与液相色谱-质谱(LC-MS)联用检测水样中的磺酰脲类除草剂。对于不同添加水平的所有分析物,测定的回收率在78.7%~102.9%之间,平行测定6次,检测的RSD值在1.6%~6.7%之间。结果表明,这是一种制备价格低廉、方便高效、绿色环保的复合材料,可实现对农药快速吸附、回收率高、重复性好,对环境水样中磺酰脲类农药的快速筛选具有潜在的价值。Magnetic silica composites(Fe_(3)O_(4)@SiO_(2))were prepared by a two-step method which used electrostatic gravitational effects between Fe_(3)O_(4) and SiO_(2)sol.The Fe_(3)O_(4)@SiO_(2) was characterized with the help of XRD,SEM,VSM,FTIR,etc.The results showed that the material had a particle size of about 20 nm,a BET specific surface area of about 59 m^(2)/g,and an average pore size of 9.8 nm,and had a saturated magnetic intensity of 39.7 emu/g.The material was used as an adsorbent for magnetic solid-phase extraction(MSPE)and coupled with liquid chromatography-mass spectrometry(LC-MS)to detect sulfonylurea herbicides(SUs)in water samples.The method recoveries were 78.7.0%-102.9%,with the relative standard deviations below 6.7%for all the analytes with different spiked levels.The results showed that the Fe_(3)O_(4)(@SiO_(2)) is an inexpensive,convenient,efficient and green composite material which can realize rapid adsorption of pesticides,high recovery and good reproducibility.The material had a great potentially valuable for the rapid screening of sulfonylurea pesticides in environmental water samples.

关 键 词：磁性二氧化硅复合材料 制备 表征 吸附 磺酰脲 

分 类 号：O614.4[理学—无机化学]