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应用QuEChERS前处理方法结合表面增强拉曼光谱(Surface-Enhanced Raman Spectroscopy)检测技术建立了豆类蔬菜(Legume Vegetables)中马拉硫磷(Malathion)残留的快速检测方法。样品以0.1%乙酸乙腈提取,N-丙基乙二胺(PSA)、C18净化剂配合石墨化炭黑(PestiCarb)净化,净化液经表面增强拉曼光谱测定后外标法定量。实验表明:加入表面增强剂后,拉曼光谱图在760cm-1处出现明显的马拉硫磷拉曼特征峰;其特征峰强度与马拉硫磷质量浓度在0.1~8.0μg/mL范围有良好的线性关系;在0.5、1.0、2.0 mg/kg添加水平下,4种豆类蔬菜的平均添加回收率在79.3%~102.1%之间,相对标准偏差(RSD)2.3%~7.8%,定量下限(LOQ)0.2 mg/kg。方法操作简便、高效、环保,符合国家规定的残留限量的检测要求,可用于豆类蔬菜中马拉硫磷残留量的快速测定。
The rapid detection of Malathion residues in Legume Vegetables was established by using QuEChERS pretreatment combined with Surface-Enhanced Raman Spectroscopy. Samples were extracted with 0.1% acetic acid in acetonitrile, purified with PSA, C18 and PestiCarb, and purified by surface-enhanced Raman spectroscopy. The experimental results show that Raman spectroscopy shows obvious Raman-Raman peak at 760cm-1 after adding the surface-enhanced agent, and its characteristic peak intensity and the concentration of malathion in the range of 0.1-8.0μg / mL The average recoveries of four kinds of legume vegetables ranged from 79.3% to 102.1% with relative standard deviations (RSDs) of 2.3% -7.8% at the dosages of 0.5, 1.0 and 2.0 mg / kg, Lower limit (LOQ) 0.2 mg / kg. The method is simple, efficient and environmentally friendly, and meets the testing requirements of residue limits prescribed by the state. It can be used for the rapid determination of malathion residues in legume vegetables.