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超高效液相色谱-串联质谱法测定小麦中吡氟酰草胺残留量

作  者:
刘磊;邵辉;李辉;李娜;李晶;宋淑荣;张玉婷;郭永泽
单  位:
天津农业质量标准与检测技术研究所农业部农产品质量安全风险评估实验室(天津)
关键词:
HPLC-MS/MS;小麦;吡氟酰草胺;残留分析
摘  要:
[目的]建立用于小麦中吡氟酰草胺残留检测的超高效液相色谱-串联质谱方法。[方法]以丙酮和正己烷为溶剂提取小麦样品中的吡氟酰草胺,经弗罗里硅土净化,通过优化色谱分离等条件,建立超高效液相色谱-串联质谱法,结合目标物标准曲线进行定量分析。[结果]方法最低检出限为0.005 mg/kg,添加吡氟酰草胺水平为0.005、0.05、5.0 mg/kg时,平均回收率为88.9%~99.2%,相对标准偏差分别为6.5%、6.2%和3.3%。[结论]经过结果分析和添加回收率试验,所建立的超高效液相色谱-串联质谱方法,可以对小麦中吡氟酰草胺农药残留实现准确定性、精确定量分析,达到农药残留分析测试要求。
译  名:
Determination of Diflufenican Residues in Wheat by UPLC-MS/MS
作  者:
LIU Lei;SHAO Hui;LI Hui;LI Na;LI Jing;SONG Shu-rong;ZHANG Yu-ting;GUO Yong-ze;Tianjin Institute of Agricultural Quality Standard and Testing Technology, Laboratory of Quality & Safety Risk Assessment for Aro-products(Tianjin),Ministry of Agriculture;
关键词:
UPLC-MS/MS;;wheat;;diflufenican;;residue analysis
摘  要:
[Aims] The ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) method was established for the detection of diflufenican residues in wheat. [Methods] The diflufenican residues in the wheat samples were extracted by the mixture of acetone and n-hexane. Then the extract was purified by magnesium trisilicate and detected by UPLC-MS/MS. Quantitative analysis was carried out by the standard curve. [Results] The limit of detection was 0.005 mg/kg. The average recovery rates were in the range of 88.9 and 99.2%, while the RSDs of the method were 6.5, 6.2 and 3.3% under the spike levels of 0.005, 0.5 and 5.0 mg/kg, respectively. [Conclusions] According to the detecting results, the UPLC-MS/MS method can be used to detect diflufenican residues in wheat quantitatively and qualitatively, which can meet the demand of pesticide residue analysis.

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