QuEChERS-超高效液相色谱-串联质谱法同时检测大米中5种农药残留

Simultaneous determination of 5 kinds of pesticide residues in rice by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  QuEChERS  超高效液相色谱-串联质谱法  大米  残留  农药

英文关键词:QuEChERS  ultra performance liquid chromatography-tandem mass spectrometry  rice  residues  pesticide

中文摘要:

      目的 明确贵阳市大中型生活超市散售大米中5种农药的残留情况。方法 通过样品前处理方法的筛选, 建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)同时测定大米中仲丁灵、戊唑醇、甲氧虫酰肼、嘧菌酯和茚虫威5种农药残留的分析检测方法。样品经1.0%乙酸乙腈提取分离, PSA净化, 采用UHPLC-MS/MS检测, 外标法定量。结果 5种农药在0.001~0.50 mg/L质量浓度范围内, 峰面积与对应的质量浓度间有良好的线性关系, 相关系数均大于0.99; 5种农药在0.002、0.01、0.1和1.0 mg/kg水平下的平均回收率为88%~111%, 相对标准偏差分别为0.45%~9.33%(n=5), 方法定量限均为0.002 mg/kg。结论 本方法满足农药残留检测分析要求, 适用5种农药在大米中的多残留准确定性和定量分析。

英文摘要:

      Objective To clarify the 5 kinds of pesticide residues in bulk rice sold in large and medium-sized supermarkets of Guiyang city. Methods Through the screening of sample pretreatment methods, a rapid analytical method for the simultaneous determination of 5 kinds of pesticide residues in rice by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was established. The samples were extracted with a mixture of 1.0% acetic acid acetonitrile, purified by dispersive solid phase extraction with primary secondary amine, and detected by UPLC-MS/MS using the external standard method for quantitative analysis. Results In the range of 0.001?0.50 mg/L, there were good linear relationships between the peak area and the corresponding concentration of the 5 kinds pesticides, and the correlation coefficients were all greater than 0.99. The average recoveries of the 5 kinds of pesticides at 0.002, 0.01, 0.1 and 1.0 mg/kg were 88%?111%, with relative standard deviations (RSDs) of 0.45%?9.33% (n=5), respectively. The limits of quantification of the methods were 0.002 mg/kg. Conclusion This method meets the requirements of pesticide residue detection and analysis, and is suitable for the accurate qualitative and quantitative analysis of multiple residues of 5 kinds of pesticides in rice.