拟除虫菊酯类农药在我国柑橘等果品中的施用量占全球第一,对其残留的快速筛查和监管对于保障我国果品食用安全具有重要意义。该文研究多功能纳米材料(NaYF4∶Yb, Er-Fe3O4@MIP)的制备条件,采用傅里叶变换红外光谱、透射电子显微镜对该材料进行表征,通过对NaYF4∶Yb, Er-Fe3O4@MIP的吸附和选择性实验,验证了其对4种拟除虫菊酯类农药具有较好的选择性和吸附性能,并构建基于该材料的拟除虫菊酯农药类特异性传感体系对柑橘果品菊酯类农残进行快速检测。结果表明,该传感体系在0.02~2.5 mg/L内对拟除虫菊酯类农药(溴氰菊酯、氯氰菊酯、氟氯氰菊酯、氰戊菊酯)具有良好的线性关系,检出限分别为6.17×10-4、6.65×10-4、7.21×10-4、9.61×10-4、6.43×10-4 mg/L。结合柑橘鲜果专属前处理技术进行实际柑橘样品检测,加标回收率为87.9%~105.8%,相对标准偏差为0.53%~6.41%,方法准确、灵敏、稳定,可以用于实际柑橘样品中拟除虫菊酯类农药的检测。
The amount of pyrethroid pesticides used in citrus and other fruits in China ranks first in the world.Rapid screening and supervision of their residues are of great significance to ensure the safety of China’s fruits.This article studied the preparation conditions of multifunctional nanomaterials (NaYF4∶Yb, Er-Fe3O4@MIP), and used Fourier transform infrared spectroscopy and transmission electron microscopy to characterize the material.Through the adsorption and selectivity experiments of NaYF4∶Yb, Er-Fe3O4@MIP, it was verified that NaYF4∶Yb, Er-Fe3O4@MIP had good selectivity and adsorption performance for four kinds of pyrethroid pesticides.Based on the above results, a pyrethroid pesticide-specific sensing system based on this material was constructed to rapidly detect pyrethroid pesticide residues in citrus fruits.Results showed that the sensing system had a good linear relationship with pyrethroid pesticides (deltamethrin, cypermethrin, cyfluthrin, and fenvalerate) in the range of 0.02-2.5 mg/L, and the detection limits were respectively 6.17×10-4, 6.65×10-4, 7.21×10-4, 9.61×10-4, 6.43×10-4 mg/L.Combined with the exclusive pre-treatment technology for fresh citrus fruits, actual citrus samples were tested.The spiked recovery rate was 87.9%-105.8%, and the relative standard deviation was 0.53%-6.41%.The method is accurate, sensitive and stable, and can be used for the detection of pyrethroid pesticides in actual citrus samples.
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