基质固相分散萃取-超高效液相色谱串联质谱法检测大米中27种农药残留量

Determination of 27 kinds of pesticides residues in rice by matrix solid phase dispersion extraction coupled with ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  基质固相分散萃取  超高效液相色谱-串联质谱法  大米  农药残留

英文关键词:matrix solid phase dispersion  ultra performance liquid chromatography-tandem mass spectrometry  rice  pesticide residue

中文摘要:

      目的 建立基质固相分散萃取-超高效液相色谱-串联质谱法(matrix solid phase dispersive extraction-ultra performance liquid chromatography-tandem mass spectrometry, MSPD-UPLC-MS/MS)检测大米中27种农药残留的分析方法。方法 以中性氧化铝为吸附剂, C18为固相萃取净化剂, 以甲醇-二氯甲烷(2:1, V:V)为洗脱溶剂, 提取液经UPLC-MS/MS分析。结果 27种化合物线性关系良好, 相关系数均大于0.999, 方法检出限为0.2～4.0 μg/kg, 定量限为0.4～10.0 μg/kg; 加标回收率为76.7%～113.3%, 相对标准偏差为1.7%～13.7%。结论 该方法灵敏、准确, 适合于大米样品中27种农药残留的定性和定量检测。

英文摘要:

      Objective To establish a method for determination of 27 pesticide residues in rice by the matrix solid phase dispersion-ultra performance liquid chromatography-tandem mass spectrometry (MSPD-UPLC-MS/MS). Methods Using neutral aluminua as dispersing sorbent, C18 as further cleanup sorbents, methanol /dichloromethane(2:1, V:V) as elution solvent, the extracting solution were analyzed by UPLC-MS/MS. Results The results showed that 27 pesticides residues had good linearity with their correlation coefficients (r2) higher than 0.999. The limits of detection were 0.2–4.0 μg/kg, and the limits of quantitation were 0.4–10.0 μg/kg. The standard recoveries were 76.7%–113.3% and the relative standard deviations were 1.7%–13.7%. Conclusion This method is sensitive, accurate and suitable for the qualitative and quantitative detection of 27 kinds of pesticide residues in rice samples.