QuEChERS法结合SERS快速检测柑橘中农药残留

The QuEChERS Method Combined with SERS Was Used to Rapidly Determine Pesticide Residues in Citrus

摘要:

QuEChERS用于农产品中农药残留SERS检测能有效提高其检测精度。该文基于柑橘中啶虫脒SERS检测的QuEChERS优化结果，将其应用于柑橘中其他农药残留SERS快速分析，以探索该方法对柑橘中农药残留SERS快速检测方法的通用性。以啶虫脒为研究对象，研究纳米竹炭（NBC）和四氧化三铁纳米粒子（Fe3O4MNPs）净化剂对柑橘中啶虫脒SERS检测的基质影响，结果表明12.5 mg NBC和10 mg Fe3O4MNPs净化效果最好。在0.1 ~ 40 mg/L范围内，基于626 cm-1特征峰强度建立柑橘中啶虫脒农药残留SERS分析方程y = 65.011x + 103.25（R2 = 0.9953），平均回收率为97％~106％，相对标准偏差（RSD）为1.03％~4.04％，最低检测限约为0.1 mg/L。该方法用于柑橘中有机磷杀虫剂（毒死蜱、丙溴磷）、新烟碱类杀虫剂（吡虫啉、啶虫脒）和昆虫生长调节剂类杀虫剂（噻嗪酮）等SERS快速分析，其平均回收率在87.60％~106％之间，相对标准偏差（RSD）为1.03％~7.71％，表明所研究的QuEChERS能适用于柑橘中不同农药残留SERS快速检测分析，该方法在20 min内可完成样品检测，为柑橘中农药残留快速检测方法开发奠定基础。

Abstract:

The application of QuEChERS in SERS detection of pesticide residues in agricultural products can effectively improve the detection accuracy. In this paper, based on the QuEChERS optimization results for SERS detection of acetamiprid in citrus, it was applied to the SERS analysis of other pesticide residues in citrus to explore the universality of this method for SERS detection of pesticide residues in citrus.The influence of Nano-bamboo charcoal (NBC) and Ferric oxide nanoparticles (Fe3O4MNPs) purification agent on the SERS of acetamiprid in citrus was studied. The results showed that 12.5mg NBC and 10mg Fe3O4 had the best purification effect. In the range of 0.1 ~ 40 mg/L, based on the characteristic peak intensity of 626 cm-1, the SERS analysis equation y = 65.011x + 103.25 (R2 = 0.9953) was established with an average recovery of 97% ~ 106%. The relative standard deviation (RSD) was 1.03% to 4.04%, and the lowest detection concentration was about 0.1 mg/L.The method was applied for the SERS analysis of organophosphorus insecticides (chlorpyrifos and profenofos), neonicotinoid insecticides (imidacloprid and acetamiprid) and insect growth regulator insecticides (buprofezin) in citrus, and the average recovery rate was between 87.60% and 106%, and the relative standard deviation (RSD) ranged from 1.03% to 7.71%, indicating that QuEChERS could be used for the rapid detection and analysis of SERS of different pesticide residues in citrus. The detection time of a single sample in this method was completed within 20 min, which laid a foundation for the development of rapid detection methods for pesticide residues in citrus.