J Sep Sci. 2014 Jan;37(1-2):99-105. doi: 10.1002/jssc.201301005.
In this paper, an effective graphene-based SPE clean-up procedure coupled with GC-MS was developed for the determination of organophosphorus pesticide residues in apple juices. The apple juice samples were diluted with water and could be loaded onto the cartridge directly. Several parameters affecting the extraction efficiency were investigated, including the type of elution, washing solution, and sample pH. Under the optimized conditions, excellent limits of quantitation for the target analytes were found to be 0.15-1.18 ng/mL, and the average recoveries of the analytes at two spiked levels for real-sample analysis ranged from 69.8 to 106.2% with RSDs less than 7.3%. Furthermore, the graphene-based cartridges exhibited superior reusability for juice sample analysis. The proposed method is sensitive, simple, and cost saving, and provides a detection platform for the monitoring of pesticide residues.
本文提出了一种基于石墨烯的固相萃取净化方法,并结合气相色谱-质谱联用技术,用于测定苹果汁中的有机磷农药残留。将苹果汁样品用水稀释后可直接加载到小柱上。考察了影响萃取效率的几个参数,包括洗脱液的类型、洗涤液和样品 pH 值。在优化条件下,目标分析物的定量限为 0.15-1.18ng/mL,实际样品分析中两个加标水平的分析物平均回收率为 69.8-106.2%,相对标准偏差小于 7.3%。此外,基于石墨烯的小柱在果汁样品分析中表现出优异的可重复使用性。该方法灵敏、简单、经济,为农药残留监测提供了一个检测平台。