氧化石墨烯-Cu金属有机框架固相萃取-电感耦合等离子体质谱法测定环境水中痕量铅  

Graphene-oxide/copper-based metal-organic framework-based solid-phase extraction combined with inductively coupled plasma-mass spectrometry for determination of trace amount of lead in environmental water samples

作　　者：张敏会[1] 李静 贺云凤 冯晓青[1] 杨鹏飞[1] 王露[1] ZHANG Min-hui;LI Jing;HE Yun-feng;FENC Xiao-qing;YANG Peng-fei;WANG Lu(Huai'an Municipal Center for Disease Control and Prevention,Huai'an,Jiangsu 223001,China)

机构地区：[1]淮安市疾病预防控制中心,江苏淮安223001

出　　处：《江苏预防医学》2023年第5期528-531,535,共5页Jiangsu Journal of Preventive Medicine

基　　金：淮安市自然科学研究计划(HAB202222);淮安市突发公共卫生事件应急检测重点实验室(HAP201906)。

摘　　要：目的制备1种吸附环境水样中重金属元素铅的氧化石墨烯-金属有机框架材料(GO/Cu-MOFs),并采用电感耦合等离子体质谱法(ICP-MS)进行定量检测。方法对萃取环境水样中铅元素的条件进行优化,再用ICP-MS测定。结果成功制备Cu-MOFs和GO/Cu-MOFs,两者红外图谱相似度很高。以GO/Cu-MOFs作为固相萃取材料,在最优化的实验条件下(样品100 mL,溶液pH=6,吸附剂用量25 mg,萃取时间15 min,洗脱剂1.0 mL 0.1 mol/L EDTA)萃取后,进行ICP-MS分析,铅元素在0.05~50.0μg/L质量浓度范围内线性良好,相关系数为0.9996,检出限为0.01μg/L,定量限为0.03μg/L,主要共存离子对检测均无显著影响。对铅质量浓度为5.00μg/L标准样品进行检测,方法回收率为90.0%~100.4%,相对标准偏差(RSD)为0.8%~3.1%。结论建立的氧化石墨烯-Cu金属有机框架固相萃取-电感耦合等离子体质谱法适合测定环境水中痕量铅。Objective To develop a type of graphene-oxide/copper-based metal-organic framework composites materials(CO/Cu-MOFs)that absorbed the heavy mental lead in environmental water samples;to develop a solid-phase extraction combined with in-ductively coupled plasma-mass spectrometry(SPE-ICP-MS)assay based on CO/Cu-MOFs for determination of lead in environmental water samples.Methods The conditions for extraction of lead in environmental water samples were optimized,and the level of lead was quantified using the CIP-MS assay.Results The Cu-MOFs and CO/Cu-MOFs were successful prepared,and these two materials shared highly similar infrared spectrum.The CO/Cu-MOFs were selected as SPE materials,and ICP-MS was performed following extrac-tion under the optimal exaction conditions(100 mL sample,solution pH value of 6,adsorbent usage of 25 mg,extraction duration of 15 min,elution buffer:0.1 mol/L EDTA 1.0 mL).Lead showed a high linear relationship at mass concentrations of 0.05 to 50.0μg/L(r=0.9996),with a 0.01μg/L limit of detection and 0.03μg/L limit of quantification,and the major coexisting ions posed no remarka-ble impact on the detection.If the SPE-ICP-MS assay was employed for detection of the standard sample containing a lead concentration of 5.00μg/L.The assay showed a recovery rate of 90.0%to 100.4%and relative standard deviations of 0.8%to 3.1%.Conclusions An SPE-ICP-MS assay based on GO/Cu-MOFs has been successfully developed for determination of trace amount of lead in environ-mental water samples,which is feasible for detection of trace lead in environmental water samples.

关 键 词：氧化石墨烯 金属有机框架 氧化石墨烯-Cu金属有机框架 电感耦合等离子体质谱法 铅 

分 类 号：R113[医药卫生—公共卫生与预防医学]