QuEChERS-UPLC-MS/MS测定大米中氯虫苯甲酰胺和五氟磺草胺的残留

目的：建立一种新的QuEChERS-超高效液相色谱—串联质谱（UPLC-MS/MS）检测大米中氯虫苯甲酰胺和五氟磺草胺的残留方法。方法：样品经0.2%甲酸—乙腈提取后，N-丙基乙二胺（PSA）和石墨化碳黑（GCB）填料净化，以0.2%甲酸水—乙腈为流动相梯度洗脱，经C₁₈色谱柱分离，采用UPLC-MS/MS测定。结果：氯虫苯甲酰胺和五氟磺草胺的定量限（LOQ）均为0.004 mg/kg，方法检出限（LOD）均为0.001 mg/kg。两种待测农药在0.002~0.5 mg/L质量浓度范围内呈良好的线性关系，其相关系数均在0.993以上。在0.05，0.1，0.5 mg/kg添加水平下，两种待测农药的平均回收率为86%~110%；相对标准偏差（RSD）为1.5%~6.1%。结论：该方法高效简便、稳定性好、灵敏度高，适用于大米中氯虫苯甲酰胺和五氟磺草胺的检测。

Determination of chlorantraniliprole and penoxsulam residues in rice by QuEChERS-UPLC-MS/MS

Objective: To establish a new QuEChERS-ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for the detection of chlorantraniliprole and penoxsulam residues in rice. Methods: After the sample was extracted with 0.2% formic acid-acetonitrile, purified with N-propylethylenediamine (PSA) and graphitized carbon black (GCB) packing, 0.2% formic acid water and acetonitrile were used as mobile phases for gradient elution, and then subjected to C₁₈ chromatography. UPLC-MS/MS was used to column separation and determination. Results: The limits of quantification (LOQ) of chlorantraniliprole and penoxsulam were both 0.004 mg/kg, and the method detection limits (LOD) were both 0.001 mg/kg. Chlorantraniliprole and penoxsulam had a good linear relationship in the range of 0.002~0.5 mg/L, and their coefficient was greater than 0.993. At the addition levels of 0.05, 0.1, and 0.5 mg/kg, the average recovery rates of chlorantraniliprole and penoxsulam were 86% to 110% with the relative standard deviations (RSD) of 1.5% to 6.1%. Conclusion: This method is efficient and simple, has good stability and high sensitivity, and is suitable for the detection of chlorantraniliprole and penoxsulam in rice.