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采用化学键合法制备了磁性石墨烯纳米粒子,将磁性石墨烯纳米粒子与乙烯基三乙氧基硅烷结合,再与离子液体发生聚合反应,得到磁性石墨烯聚离子液体(Fe_3O_4@SiO_2@G@PIL)纳米复合材料,用SEM对其进行形态表征。将复合材料作为分散固相萃取(QuEChERS)的吸附剂,结合GC-MS/MS分析技术,建立了蔬菜中30种保鲜剂残留的检测方法。考察了不同类型吸附剂的净化效果,复合材料的最佳用量,净化时间等实验条件。30种保鲜剂在5~500μg/L的范围内线性关系良好,相关系数为0.9972~0.9997,检测限(LOD)为0.02~0.42μg/L。加标回收率为75.1%~111.9%,RSD为0.1%~6.7%。方法适用于蔬菜中多种保鲜剂残留的快速检测。
The magnetic graphene nanoparticles were prepared by chemical bonding method. The magnetic graphene nanoparticles were combined with vinyltriethoxysilane and then polymerized with ionic liquid to obtain magnetic graphene polyionic liquid (Fe 3 O 4 @SiO 2 @G @ PIL ) Nanocomposites were characterized by SEM. The composites were used as sorbent for dispersive solid phase extraction (QuEChERS) and GC-MS / MS analysis was used to establish the detection method for 30 kinds of preservatives in vegetables. The effects of different types of adsorbents on the purification efficiency, the optimum dosage of composite materials, purification time and other experimental conditions were investigated. The results showed that there was a good linearity in the range of 5 ~ 500μg / L with the correlation coefficient of 0.9972 ~ 0.9997 and the limit of detection (LOD) of 0.02 ~ 0.42μg / L. The spiked recoveries ranged from 75.1% to 111.9% with RSD from 0.1% to 6.7%. The method is suitable for the rapid detection of a variety of preservative residues in vegetables.