生物炭材料分散固相萃取环境水中有机氯农药  

Biochar Materials Dispersed Solid Phase Extraction of Organochlorine Pesticides In Environmental Water

作　　者：李睿 曹月阳 刘郁枫 赵汗青[1,2] 赵文婷 LI Rui;CAO Yue-yang;LIU Yu-feng;ZHAO Han-qing;ZHAO Wen-ting(College of Bioscience and Resources Environment,Beijing University of Agriculture,Beijing 102206,China;Key Laboratory of Urban Agriculture In North China,Ministry of Agriculture Rural Affairs,Beijing 102206,China)

机构地区：[1]北京农学院生物与资源环境学院,北京102206 [2]农业农村部华北都市农业重点实验室,北京102206

出　　处：《化学试剂》2023年第8期116-121,共6页Chemical Reagents

基　　金：2022年度市属高校优秀青年人才培育计划项目(BPHR202203098);北京市教育工会支持项目(北京高校青年教师创新教研工作室);2023农业农村部华北都市农业重点实验室开放课题项目;北京农学院学位与研究生教育改革与发展项目(5056516024/002)。

摘　　要：以头发为原材料制备生物炭作为分散固相萃取方法的吸附剂,结合气相色谱,建立了一种新的样品前处理方法,用于检测环境水体中8种有机氯农药(OCPs)的残留量。头发生物炭通过低温裂解法,在300℃恒温条件下,经过3 h烧制而成,研磨成大小均匀的颗粒,可作为吸附剂。将其与包含目标分析物的水溶液超声混合。离心分离后,再用正己烷将生物炭中的目标分析物充分洗脱,洗脱溶剂过膜,进气相色谱检测分析。对超声时间、洗脱溶剂、加炭量、pH值以及盐含量等影响萃取效率的因素进行优化。选择最优参数,建立最优分散固相萃取方法。研究结果表明:该方法LODs为1.3~8.8μg/L,LOQs为4.4~29.4μg/L,相对标准偏差为4.2%~6.4%,在2~100μg/L的添加浓度范围内呈现良好的线性关系,相关系数范围为0.9913~0.9951。该方法操作简单、萃取效率高、重现性好,且废弃物得到了重复利用,可应用于环境水体中的8种OCPs农药残留的检测。Using hair as raw material to prepare biochar as a sorbent for dispersive solid phase extraction method,a new sample pretreatment method was established to detect 8 organochlorine pesticide residues in environmental water bodies combined with gas chromatography.The hair biochar was through the low temperature pyrolysis method,under the condition of 300℃temperature,kept 3 h,and ground to a uniform size,it could be used as a sorbent for dispersive solid-phase extraction.The biochar was mixed with sample solution by ultrasonic,which contained the target analyte.After centrifugal separation,n-hexane was used to elution target analyte in biochar adequately.It was recycled for filtration and analyzed in gas chromatography.Ultrasonic time,elution solvent,carbon content,pH value,salt content and other factors affecting extraction efficiency were optimized.The optimal dispersive solid phase extraction method was established by selecting the optimal parameters.The limits of detection were 1.3~8.8μg/L,and the limits of quantitation were 4.4~29.4μg/L.The relative standard deviations were 4.2%~6.4%,and the correlation coefficients ranged from 0.9913 to 0.9951 in the range of 2~100μg/L.The method had the advantages of simple operation,high efficiency and good reproducibility,and wastes were reused.The method can be applied to detect 8 organochlorine pesticides residues in environmental water.

关 键 词：生物炭 分散固相萃取 有机氯农药 气相色谱 环境水 

分 类 号：O65[理学—分析化学]