磁固相萃取与高效液相色谱联用测定水体中防治白蚁农药残留  

Combination Technology of Magnetic Solid-Phase Extraction and High Performance Liquid Chromatography and Its Application in Detection of Termiticides Residues in Aqueous Solutions

作　　者：王为中 崔世海[2] 闫婷婷[2] 倪小璐[2] 孙小涵 娄大雷 

机构地区：[1]徐州市白蚁防治所,江苏徐州221000 [2]江苏省生物功能材料创新中心,江苏省生物材料重点实验室,南京师范大学化学与材料科学学院,江苏南京210023

出　　处：《南京师大学报（自然科学版）》2016年第4期132-138,共7页Journal of Nanjing Normal University(Natural Science Edition)

基　　金：国家自然科学基金(21177061);江苏省第四期“333工程”科研项目(BRA2015062);江苏省自然科学基金(BK20150968)

摘　　要：以FeCl_3为铁源用溶剂热法合成了磁性Fe_3O_4纳米粒子,再以葡萄糖为碳源水热法制备了Fe_3O_4/C纳米复合粒子.通过透射电镜（TEM）、X-射线衍射（XRD）、红外光谱（FT-IR）和差热-热重（TG-DSC）等分析手段对材料进行了表征.将材料应用于水体中防治白蚁药物毒死蜱、溴氰菊酯、联苯菊酯的磁固相萃取考察了材料用量、pH、萃取时间、洗脱溶剂、重复性等条件对萃取效率的影响在优化的实验条件下将该方法应用于实际水样的测定,样品的平均加标回收率在82.9%~106.2%,相对标准偏差为2.1%~9.6%,说明该分析方法准确可靠,Fe_3O_4/C纳米复合粒子与高效液相色谱联用的方法可以测定水体中防治白蚁药物残留.Fe3O4 nanoparticles were prepared by solvothermal method with FeCl3 as the iron resource. Carbon coated Fe304 nanocomposites （Fe3O4/C） were prepared by hydrothermal reaction with the glucose as the carbon resource. The nanoparticles were characterized by transmission electron microscopy （ TEM ） , X-ray diffraction spectra （XRD） , Fourier transforminfrared spectra（ FT-IR） ,and thermogravimetry mass-differential scanning calorimetry spectrometry （ TG-DSC ）. The nanomaterial was then applied in the magnetic solid-phase extraction of termiticides in water such as chlorpyr ifos, deltamethrin and bifenthr in. Various MSPE parameters were optimized including amount of Fe304/C nanoparticles,pH of sample solut ion,adsorption t ime,elut ion solvent and reusabi l ity. Good recoveries（ 82.9% ？1 0 6 .2% ） were achieved with the relative standard deviations range from 2.1% ？9 .6% with the optimal conditions. I t is confirmed that the analysis method is accurate and reliable. The combination of Fe304/C nanocomposites and the high performance l iquid chroma-tography can be used in the determination of termiticides in water.

关 键 词：磁固相萃取 碳包四氧化三铁纳米粒子 拟除虫菊酯 有机磷农药 高效液相色谱 

分 类 号：O657.7[理学—分析化学]