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

中文关键词:  QuEChERS  超高效液相色谱-串联质谱  柑橘  吡虫啉  啶虫脒  噻嗪酮

英文关键词:QuEChERS  ultra performance liquid chromatography-tandem mass spectrometry  citrus  imidacloprid  acetamiprid  buprofezin

中文摘要:

      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2~50 μg/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4.00 μg/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。

英文摘要:

      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 2–50 μg/kg, with correlation coefficient over 0.998. The limits of quantification for imidacloprid,?acetamiprid and?buprofezin were 2.00, 0.12 and 4.00 μg/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.