QuEChERS-UPLC-MS/MS法快速筛查稻米和稻茎中42种农药残留

建立了QuEChERS前处理技术结合超高效液相色谱-串联质谱 (UPLC-MS/MS) 同时检测稻米和稻茎中42种农药残留的分析方法。样品经乙腈涡旋提取、QuEChERS净化管净化，C₁₈超高效液相色谱柱分离后，在电喷雾正离子 (ESI+) 模式下，通过多反应监测正离子模式进行检测，采用基质匹配标准曲线峰面积外标法进行定量分析。结果表明:在0.01~0.2 mg/L范围内，42种农药的质量浓度与对应的峰面积间线性关系良好，R2 > 0.99，检出限为0.001~0.002 mg/kg。在0.01、0.02、0.05、0.1和0.2 mg/kg 5个添加水平下，42种农药在稻米和稻茎中的平均回收率均为70%~117%，相对标准偏差 (RSD) 稻米为1.5%~15%和稻茎为0.9%~15%。该方法具有操作简单、快速、灵敏度高、准确度高等优点，适用于稻米和稻茎中多种类农药残留的快速筛查分析。

Rapid screening of 42 pesticides in rice and rice stems by QuEChERS-UPLC-MS/MS

A method for the analysis of 42 pesticide residues in rice and rice stems was developed using ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) combined with QuEChERS pretreatment technology. The sample was extracted with acetonitrile vortex extraction, purified by QuEChERS purification tube and separated by C₁₈ ultra-high performance liquid chromatography column. 42 analytes were measured under multiple reaction monitoring (MRM) using the electrospray positive ionization mode (ESI⁺). Quantification determination was performed by peak area external standard methods using matrix-matched calibration, which were linear in the range of 0.01-0.2 mg/L with good linear relationships. The determination coefficients (R²) were all above 0.99. The limits of detection (LOD) were lower than 0.002 mg/kg. The average recoveries of 42 pesticides in rice and rice stems all ranged from 70%-117%, and the relative standard deviations were in the range of 1.5%-15% in rice, and 0.9%-15% in rice stems, at the spiked levels of 0.01, 0.02, 0.05, 0.1 and 0.2 mg/kg. This method is simple, rapid, sensitivite, accuracy, which can be used in the simple and rapid screening of pesticide multi-residues in rice and rice stems.