摘要
利用溶剂热法构建了锰掺杂锆金属有机骨架材料MnDUT-52,将其作为吸附剂用于快速分散固相萃取大豆中除草醚(NIT)、乙氧氟草醚(OXY)和甲羧酸草醚(BIF)3种二苯醚类除草剂(Des)。对MnDUT-52吸附剂的晶体结构、分子基团和表观形貌进行了表征。优化了吸附剂用量、吸附时间、溶液pH、解吸溶剂种类等萃取条件。结果显示,30 mg吸附剂在15 min内即可实现对目标物的完全吸附。在优化的萃取条件下,3种Des在1.0~150μg/kg范围内线性关系良好(R≥0.9993),检出限为0.3~0.4μg/kg,在4,20和100μg/kg 3个加标水平下,回收率为81.7%101.2%,相对标准差(RSD)不超过10%。该方法适用于大豆样品中除草剂的检测分析。
A manganese-doped metal-organic framework composite(MnDUT-52)was fabricated by a facile solvothermal method and used for rapid enrichmentof trace diphenyl ether herbicides(Des),includingnitrofen(NIT),oxyfluorfen(OXY),and bifenox(BIF),in soybean samples.The crystal structure,molecular groups,and apparent morphology of the MnDUT-52 adsorbent were characterized.The main dispersive solid-phase extraction parameters,including the adsorbent amount,adsorption time,solution pH,and desorption solvent,were investigated.The results showed that complete adsorption could be achieved in 15 min with 30 mg of MnDUT-52.Under optimal DSPE conditions,the method showed good linearity in the concentration range of 1.0-150μg/kg with the correlation coefficients(R)≥0.9993.The limits of detection were 0.3-0.4μg/kg,the recoveries of the three Des at three spiked levels of 4,20,and 100μg/kg were 81.7%-101.2%,and the relative standard deviations(RSDs)did not exceed 10%.The method is suitable for the determination of herbicides in soybean samples.
作者
李淼
李佳琪
陈俊杰
董雅柠
陈家怡
闫萌
王茜
王曼曼
郝玉兰
LI Miao;LI Jiaqi;CHEN Junjie;DONG Yanning;CHEN Jiayi;YAN Meng;WANG Qian;WANG Manman;HAO Yulan(School of Public Health,North China University of Science and Technology,Tangshan 063210,China;Beijing Chaoyang District Center for Disease Control and Prevention,Beijing 100027,China)
出处
《分析试验室》
北大核心
2025年第6期821-827,共7页
Chinese Journal of Analysis Laboratory
基金
国家自然科学基金(82073608)
河北省煤矿卫生与安全重点实验室
河北省职业卫生与安全协同创新中心
华北理工大学公共卫生学院高水平科研创新团队建设计划(KYTD202302)资助。
关键词
掺杂金属有机骨架
前处理
分散固相萃取
二苯醚类除草剂
大豆
doped metal-organic framework
pretreatment
dispersive solid phase extraction
diphenyl ether herbicides
soybean sample