磁性固相萃取-气相色谱质谱联用检测桔汁中的农药残留

Determination of pesticide residues in orange juice by MSPE-GC/MS

建立了磁性固相萃取-气相色谱质谱联用(MSPE-GC/MS)检测桔汁中3种农药(2-苯基苯酚、二苯胺、胡椒基丁醚)的分析方法。首先采用化学共沉淀法合成了磁性羟基化多壁碳纳米管(Fe3O4@MWSNTs-OH)。在同等条件下,萃取效果优于磁性多壁碳纳米管和磁性氮参杂碳纳米管。优化了磁性固相萃取过程,考察了磁性吸附剂用量,萃取时间,洗脱溶剂种类和体积等参数对萃取效率的影响,在最优条件下,3种农药在0.01~10mg·L^-1浓度范围内,线性关系良好,相关系数在0.9973~0.9987之间,检测限为0.167~0.333μg·L^-1(S/N=3)。实际样品的加标回收率为85.1%~101.0%,相对标准偏差为1.9%~5.5%。结果表明,建立的方法操作简便,且重复性较好,适用于果汁中农药残留的检测。

Hydroxylated multi-walled carbon nanotubes magnetic nanoparticles(Fe3O4@MWSNTsOH)was successfully synthesized and exploited as sorbent for extraction of three pesticides(2-phenylphenol,diphenylamine,piperonyl butoxide).The linear relationship was in the range of 0.01-10 mg·L^-1,the correlation coefficients ranged from 0.9973 to 0.9987,the LODs were in the range of 0.167-0.333μg·L^-1(S/N=3).The standard recoveries ranged from 85.1%to 101.0%,the variation coefficients were in the range of 1.9%-5.5%.This method is simple and suitable for trace analysis of the three pesticides.With convenient magnetic separation,the synthesized magnetic adsorbent can be recycled more than four times.