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目的建立气相色谱法检测水果中氟虫腈农药残留的方法。方法样品提取液分别经N-丙基乙二胺净化柱、弗洛里硅土柱、QuEChERS净化管提取净化后,采用外标法进行定量检测。结果方法在0.01～0.2μg/mL浓度范围内,线性良好。在3个添加水平下,经QuEChERS柱提取净化后的回收率为89.0%～104.0%,较其他2种净化柱净化的回收率高。相对标准偏差为2.58%～4.08%(n=6),氟虫腈的最低检出限为0.001 mg/kg,定量限为0.003 mg/kg。结论该方法准确、简单、重现性好,能够用于水果中氟虫腈残留量的检测。
Objective To establish a method for the determination of fipronil pesticide residues in fruits by gas chromatography. Methods The sample extracts were purified by N-propyl ethylenediamine purification column, Florisil column and QuEChERS purification tube, respectively, and then quantified by external standard method. Results The method was linear in the range of 0.01 ~ 0.2μg / mL. At the three addition levels, the recovery after purification by QuEChERS column was 89.0% ~ 104.0%, which was higher than that of the other two purification columns. The relative standard deviations were 2.58% ~ 4.08% (n = 6). The detection limit of fipronil was 0.001 mg / kg and the limit of quantification was 0.003 mg / kg. Conclusion The method is accurate, simple and reproducible. It can be used for the determination of fipronil in fruits.