超高效液相色谱-串联质谱法同时测定柑橘中的吡虫啉、啶虫脒和噻嗪酮残留量

Simultaneous determination of imidacloprid,acetamiprid and buprofezin residues in citrus by ultra performance liquid chromatography-tandem mass spectrometry

目的建立超高效液相色谱-串联质谱同时检测柑橘中吡虫啉、啶虫脒和噻嗪酮残留的分析方法。方法样品经酸化乙腈溶液提取后加入盐析剂分层,然后在提取液中加入无水硫酸镁、十八烷基键合硅胶吸附剂(C18)和N-丙基乙二胺吸附剂(PSA)填料进行基于QuEChERS法净化,采用高效液相色谱-串联质谱法进行检测。选用电喷雾离子源正离子(electrospray ionization,ESI+)以及多反应监测(multi-reaction monitoring,MRM)模式。结果吡虫啉、啶虫脒和噻嗪酮在2~50μg/kg范围内具有较好的线性关系,相关系数均优于0.998。吡虫啉、啶虫脒和噻嗪酮方法定量限分别为2.00、0.12和4.00μg/kg,添加水平的回收率为69.5%~118.3%,相对标准偏差(relative standard deviations,RSD)为1.8%~10.7%(n=8)。结论本方法速度快、灵敏度高、准确性好,可用于柑橘样品中吡虫啉、啶虫脒和噻嗪酮残留量的定性和定量检测。

Objective To establish a method for simultaneous determination of the residues of imidacloprid,acetamiprid and buprofezin in citrus by ultra performance liquid chromatography-tandem mass spectrometric.Methods The samples were extracted with acidified acetonitrile solution and layered with salting out agent.Then the samples were purified with MgSO4,octadecyl bonded silica gel adsorbent(C18)and n-propyl ethylenediamine adsorbent(PSA)based on QuEChERS method and finally detected by ultra performance liquid chromatography-tandem mass spectrometric,using positive electrospray ionization(ESI+)mode and MRM.Results The linear relationship among imidacloprid,acetamiprid and buprofezin was good in the concentration range of 2–50μg/kg,with correlation coefficient over 0.998.The limits of quantification for imidacloprid,acetamiprid and buprofezin were 2.00,0.12 and 4.00μg/kg,respectively.The recovery was 69.5%–118.3%and the relative standard deviation(RSD)was 1.8%–10.7%(n=8).Conclusion The method is rapid,sensitive and accurate,and can be applied for the qualitative and quantitative analysis of imidacloprid,acetamiprid and buprofezin in citrus.