基于Fe金属-有机骨架的磁性多孔碳材料的制备及其萃取水中孔雀石绿的应用研究  

Preparation of magnetic porous carbon material based on Fe metal-organic framework and its application in the extraction of malachite green in water

作　　者：陈祥明[1,2] 张聪 王丹红[1] 李捷[1] 谢白璐 石祥程 林妍[1] 张昌盛[1] 杨燕萍[1] 叶芳贵[4] 

机构地区：[1]福建出入境检验检疫局,福州350001 [2]福建省检验检疫技术研究重点实验室,福州350001 [3]福建省食品药品质量检验研究院,福州350001 [4]广西师范大学,桂林541004

出　　处：《食品安全质量检测学报》2016年第9期3629-3635,共7页Journal of Food Safety and Quality

基　　金：国家质量监督检验检疫总局项目(2015IK029;2014Ik097);福建省科技厅项目(2016J01087);福建出入境检验检疫局项目(FK2014-JS002)~~

摘　　要：目的制备一种新型磁性多孔碳材料-γ-Fe2O3/C,并建立一种简单可靠的富集水中孔雀石绿的方法。方法先利用水热法合成MOF-MIL-53（Fe）,再以其为模板通过微波辅助高温离子热法合成γ-Fe2O3/C,利用XRD、FT-IR、SEM、TEM等手段对γ-Fe2O3/C进行表征,并将其作为MSPE吸附剂富集环境水样中的孔雀石绿,同时对吸附剂用量、洗脱剂种类、萃取时间以及洗脱次数等影响磁固相萃取效率的因素进行优化。结果孔雀石绿在50-5000μg/L的浓度范围内线性关系良好,相关系数大于0.9995,方法检出限为11.07μg/L,添加低、中、高3个浓度水平下的回收率范围为84.0%-102.0%,相对标准偏差小于5%（n=5）。结论本研究制备的纳米材料可适用于日常环境水样中的孔雀石绿的检测。Objective To prepare a new type of magnetic porous carbon material（γ-Fe2O3/C） and establish a simple and reliable method for rapid enrichment of malachite green in water sample.Methods Firstly,（MOF）-MIL-53（Fe） was synthesized by hydrothermal method,and then it was used as template for synthesis ofγ-Fe2O3/C by high temperature ionothermal method assisted with microwave.γ-Fe2O3/C composites were characterized by means of XRD,FT-IR,SEM and TEM,and used as absorbents for concentrating malachite green from water sample.Meanwhile,the factors relevant to the microextraction efficiency such as the amount of adsorbent,the type of eluting agent,extraction time and eluent time and so on were optimized.Results The malachite green had a good linear relationship in the range of 50-5000 μg/L with correlation coefficient larger than 0.9995.The limit of detection was 11.7 μg/L.The recoveries spiked at low,medium,and high levels were in the range of84.0%-102.0%with RSDs less than 5%（n=5）.Conclusion The magnetic nanostructured porous carbon material can be used for enrichment and detection of malachite green in water sample.

关 键 词：金属-有机骨架 磁固相萃取 磁性碳材料 孔雀石绿 

分 类 号：TS254.7[轻工技术与工程—水产品加工及贮藏工程] O658.2[轻工技术与工程—食品科学与工程]