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

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.