School of Food Science and Engineering, Shaanxi University of Science & Technology, Xi'an 710021, P. R. China.
Anal Methods. 2022 Nov 24;14(45):4680-4689. doi: 10.1039/d2ay01321e.
Rapid and reliable detection and quantification of pesticide residues in complex matrices by surface enhanced Raman spectroscopy (SERS) remain challenging due to the low level of target molecules and the interference of nontarget components. In this study, SERS was combined with dispersive liquid-liquid microextraction (DLLME) to develop a rapid and reliable method for the detection of organophosphorus pesticides (OPPs). In this method, DLLME was used to extract and enrich two representative OPPs (triazophos and parathion-methyl) from a liquid sample, and a portable Raman spectrometer was used to analyze the separated sediment using homemade gold nanoparticles colloids as enhancing substrates. The results showed that the developed method displayed good sensitivity and stability for the detection and quantification of triazophos and parathion-methyl with ≥ 0.98. The calculated limits of detection (LODs) in the simultaneous detection of triazophos and parathion-methyl were 2.17 × 10 M (0.679 ppb) and 2.28 × 10 M (5.998 ppb), and the calculated limits of quantification (LOQs) were 7.23 × 10 M (2.26 ppb) and 7.62 × 10 M (19.098 ppb), respectively. Furthermore, the developed SERS method was successfully applied to the detection of triazophos and parathion-methyl in apple juice with recoveries between 78.07% and 110.87% and relative standard deviations (RSDs) ≤ 2.06%. Therefore, the developed DLLME facilitated liquid SERS method exhibited good sensitivity and stability for the rapid detection and quantification of OPPs and had the potential to be applied to the rapid detection of OPPs in complex matrices.
表面增强拉曼光谱(SERS)由于目标分子含量低和非目标成分干扰,仍然难以快速可靠地检测和定量复杂基质中的农药残留。在本研究中,SERS 与分散液-液微萃取(DLLME)相结合,开发了一种快速可靠的检测有机磷农药(OPPs)的方法。在该方法中,DLLME 用于从液体样品中提取和富集两种代表性的 OPP(三唑磷和甲基对硫磷),并使用便携式拉曼光谱仪分析分离出的沉淀物,使用自制的金纳米粒子胶体作为增强基底。结果表明,该方法对三唑磷和甲基对硫磷的检测和定量具有良好的灵敏度和稳定性,≥0.98。在同时检测三唑磷和甲基对硫磷时,计算出的检测限(LOD)分别为 2.17×10-6 M(0.679 ppb)和 2.28×10-6 M(5.998 ppb),定量限(LOQ)分别为 7.23×10-6 M(2.26 ppb)和 7.62×10-6 M(19.098 ppb)。此外,该方法成功应用于苹果汁中三唑磷和甲基对硫磷的检测,回收率在 78.07%至 110.87%之间,相对标准偏差(RSD)≤2.06%。因此,开发的 DLLME 辅助液体 SERS 方法对 OPPs 的快速检测和定量具有良好的灵敏度和稳定性,有望应用于复杂基质中 OPPs 的快速检测。