玉米须衍生磁性多孔碳的制备及其对海水中孔雀石绿的萃取  

Preparation of Magnetic Porous Biochar Derived from Corn Silk and Its Extraction of Malachite Green in Seawater

作　　者：陈柏森 王希越[1] 祝波[1] 连丽丽[1] 娄大伟[1] CHEN Bai-sen;WANG Xi-yue;ZHU Bo;LIAN Li-li;LOU Da-wei(Department of Analytical Chemistry,Jilin Institute of Chemical Technology,Jilin 132022,China)

机构地区：[1]吉林化工学院分析化学系,吉林吉林132022

出　　处：《分析测试学报》2020年第8期993-999,共7页Journal of Instrumental Analysis

基　　金：国家自然科学基金青年基金(21605056);吉林省自然科学基金(20180101292JC);吉林省科技发展计划项目(20190303116SF);吉林省产业技术研究与开发项目(2020C028-1);吉林省教育厅“十三五”科学技术项目(JJKH20200238KJ)。

摘　　要：以可再生农业废弃物玉米须为碳前驱体,三氯化铁为铁源,通过溶剂热碳化法制备了表面负载Fe3O4纳米粒子的磁性水热碳材料(MHC),再以氢氧化钾(KOH)为化学活化剂,通过高温热解法成功制备了生物质衍生磁性多孔碳(AMC)。该磁性纳米复合材料具有多孔结构,可为目标分析物提供大量的吸附位点,而均匀地分散在碳基质表面的铁氧化物(Fe3O4及Fe2O3)纳米粒子有助于吸附剂及负载分析物从水溶液中快速分离。AMC对孔雀石绿(MG)具有显著的吸附性能,最大吸附量可达312.5 mg/g。采用磁性固相萃取(MSPE)结合超高效液相色谱(UPLC)建立了水中MG的分析方法。优化了影响AMC萃取性能的关键因素,在100 mL pH 7.0的样品溶液中,使用6 mg AMC萃取20 min,以甲醇-乙醇(9∶1,体积比)作为洗脱液,可获得最佳萃取结果。该方法对0.05~5μg/L范围内的MG呈现良好的线性(r=0.999 6),其检出限为0.01μg/L,定量下限为0.03μg/L。使用AMC萃取加标海水样品中的MG,其回收率为104%~106%,RSD为1.7%~3.4%。该方法可用于养殖海水中MG的灵敏检测。A magnetic hydrothermal carbon material(MHC) coated with Fe3O4 nanopaticles was firstly prepared by solvothermal method,using renewable agricultural waste corn silk as the carbon precursor,ferric chloride(FeCl3·6 H2O) as the source of iron.Then,a biomass-derived activated magnetic porous carbon(AMC) was successfully fabricated via pyrolysis treatment of MHC using KOH as activating reagent.This magnetic nanocomposite,with a well-developed porous structure,provided a large number of activated sites for the target absorption.Besides,the iron oxide(Fe3O4 and Fe2O3) homogeneously distributed on the surface of the carbon matrix.AMC exhibited a remarkable adsorption performance toward malachite green(MG),and the maximum adsorption capacity reached up to 312.5 mg/g obtained from the Langmuir isotherm.Combined with ultra-high performance liquid chromatography(UPLC),AMC was served as a magnetic solid-phase extraction(MSPE) adsorbent to detect MG in water.The important parameters influencing the extraction performance of the adsorbent were investigated and optimized.The best extraction results were obtained when 6 mg AMC was applied to extract MG in 100 mL sample solution(pH 7.0) for 20 min,using a mixture of methanol-acetic acid(9 ∶1,by volume) as eluent.Results showed that there was a good linear relationship for MG in the concentration range of 0.05-5 μg/L,with correlation coefficient(r) of 0.999 6.The limit of detection(LOD) was 0.01 μg/L,and the limit of quantitation(LOQ) was 0.03 μg/L.The spiked recoveries for MG in the seawater samples ranged from 104% to 106%,with RSDs of 1.7%-3.4%.The developed method was suitable for the detection of MG in aquacultural seawater.

关 键 词：多孔碳 磁分离 孔雀石绿(MG) 磁性固相萃取(MSPE) 超高效液相色谱(UPLC) 

分 类 号：O657.72[理学—分析化学] F767.4[理学—化学]