磁性聚多巴胺磁固相萃取气相色谱-质谱分析尿中三苯  

Fe_3O_4@PDA magnetic solid phase extraction combined with GC-MS for analysis of BTX in urine

作　　者：张楚欣 沙亚南 郑倩 叶青 ZHANG Chu-xin;SHA YA-Nan;ZHENG Qian;YE Qing(School of chemistry and Environmental Science,Shangrao Normal University,Shangrao 334001,China)

机构地区：[1]上饶师范学院化学与环境科学学院,江西省高等学校应用有机化学重点实验室,江西上饶334001

出　　处：《化学研究与应用》2018年第8期1358-1361,共4页Chemical Research and Application

基　　金：江西省科技厅工业支撑计划项目(20151BBE50022)资助;2017上饶师范学院大学生创新创业训练计划项目(2017-CX-14)资助。

摘　　要：合成了磁性聚多巴胺纳米材料,以其为固相萃取材料、结合气相色谱-质谱方法建立了检测尿中苯、甲苯和二甲苯的新方法。优化了萃取条件,实验结果表明:当使用磁性聚多巴胺10mg,旋涡震荡吸附10min,乙酸乙酯作为洗脱剂,用0.6m L乙酸乙酯超声洗脱10min时效率最高。在优化的实验条件下,方法的线性范围在0.15~750μg·L-1之间,相关系数大于0.997,RSD在3.9%~5.2%之间,检出限为0.010-0.025μg·L-1。将方法应用于尿中苯、甲苯和二甲苯的分析,回收率在93.6%~102%之间,富集倍数为66.7。The polydopamine coated magnetic Fe 3O 4 microspheres(Fe 3O 4@PDA)were synthesized and applied as an effective adsorbent for the preconcentration of Benzene,toluene and xylene(BTX)in urine samples prior to GC-MS.The extraction conditions were optimized.The experimental results showed it achieved maximum efficiency when adsorption time for 10 mins with 10 mg magnetic polydopamine and supersonic elution for 10mins with 0.6mL ethyl acetate.Under optimum conditions,the linear relationship was obtained in the range of 0.15-750μg·L^-1 and the correlation coefficients were greater than 0.997.The relative standard deviations were between 3.9~5.2%and the detection limits were between 0.010~0.025μg·L^-1.This method has been applied for the determination of BTX in urine samples with satisfactory results.The recoveries fell in the range from 93.6~102%and concentration factor is 66.7.

关 键 词：磁性聚多巴胺 磁固相萃取 苯、甲苯和二甲苯 气相色谱-质谱 尿 

分 类 号：O657.7[理学—分析化学]