摘要
采用溶剂热法制备了磁性金属有机骨架吸附剂Fe_3O_4-NH_2@MIL-101,通过电子显微镜、红外光谱、X射线衍射对吸附剂的形貌和组成进行了表征,磁强计对吸附剂的磁强度进行了测定。使用该吸附剂进行磁固相萃取,结合高效液相色谱-紫外检测,对农田灌溉水中4种苯甲酰脲类杀虫剂(氯吡脲、氟幼脲、氟铃脲和虱螨脲)进行分析。实验对吸附和洗脱条件进行了优化,包括吸附剂用量、吸附时间、pH值、离子强度、洗脱溶剂种类以及洗脱时间和体积。在最佳实验条件下,方法能够有效富集灌溉水中的苯甲酰脲类杀虫剂。4种苯甲酰脲类杀虫剂在0. 010～3. 0 mg/L浓度范围内线性关系良好,相关系数(r)均大于0. 999 5,检出限为0. 03～0. 09μg/L,定量下限为0. 10～0. 30μg/L。方法的加标回收率为81. 7%～95. 4%,RSD小于10%。该方法前处理操作简便,萃取用时不超过15 min,可用于农田灌溉水中苯甲酰脲类杀虫剂的检测。
A method of high performance liquid chromatography( HPLC) with magnetic solid-phase extraction( MSPE) was developed for the determination of four benzoylurea pesticides,i. e. forchlorfenuron,penfluron, hexaflumuron and lufenuron in irrigation water. A magnetic metal organic framework sorbent( Fe3O4-NH2@MIL-101) was fabricated via solvothermal method. The composition and morpholgy of the composite were characterized by scanning electron microscopy( SEM),Fourier transform infrared spectroscopy( FT-IR) and X-ray diffraction( XRD) analysis. Meanwhile,the magnetic intensity of the material was detected with a vibrating sample magnetometer. The determination of four analytes was performed by HPLC with the synthesized composite as MSPE adsorbent.The adsorption and elution factors,including adsorbent amount,adsorption time,p H value,elution time and elution volume,were investigated. Under the optimum conditions,the calibration curves for four benzoylurea pesticides showed good linear relationships in the range of 0. 010-3. 0 mg/L with correlation coefficients( r) higher than 0. 999 5. The detection limits and the quantitation limits were in the ranges of 0. 03-0. 09 μg/L and 0. 10-0. 30 μg/L,respectively. The recoveries at three spiked levels ranged from 81. 7% to 95. 4% with RSD less than 10%. With a simple pretreatment process and an extraction time within 15 min,the method could be applied in the analysis on trace residues of benzoylurea pesticides in irrigation water.
作者
贾叶青
念琪循
张磊
冀欠欠
徐厚君
王曼曼
王学生
郝玉兰
JIA Ye-qing;NIAN Qi-xun;ZHANG Lei;JI Qian-qian;XU Hou-jun;WANG Man-man;WANG Xue-sheng;HAO Yu-lan(School of Public Health,North China University of Science and Technology,Tangshan 063210,China)
出处
《分析测试学报》
CAS
CSCD
北大核心
2019年第1期46-51,共6页
Journal of Instrumental Analysis
基金
国家自然科学基金(21305028)
河北省自然科学基金(H2017209232
H2016209018)
河北省教育厅重点项目(ZD2018014)
华北理工大学培育基金项目(JQ201717)
