QuEChERS-超高效液相色谱-串联质谱法同时检测辣椒中5种杀菌剂残留

建立QuEChERS-超高效液相色谱-串联质谱法同时检测鲜食辣椒中多菌灵、甲基硫菌灵、烯酰吗啉、嘧菌酯和苯醚甲环唑5种杀菌剂的分析方法。方法 样品经2.0%乙酸乙腈提取分离, 50 mg C18和20 mg GCB净化, 采用超高效液相色谱-串联质谱法检测, 基质外标法定量。结果 5种杀菌剂在0.01~1.00 mg/L质量浓度范围内, 峰面积与对应的质量浓度间线性关系良好, 相关系数均大于0.989; 5种杀菌剂在0.01、0.1和1.0 mg/kg添加水平下的平均回收率为74%~105%, 相对标准偏差为2.07%~9.61% (n=5), 方法定量限均为 0.01 mg/kg。贵州辣椒中5种杀菌剂的残留量为<0.01-0.092 mg/kg。结论 本方法满足农药残留检测分析要求, 适用于5种农药在鲜食辣椒中的多残留准确定性和定量分析以及市场监督抽查等。实际样品检测显示5种杀菌剂在贵州辣椒上的使用是安全的, 不会产生相关膳食风险与危害, 不影响出口贸易。

Simultaneous determination of 5 kinds of fungicides residues in pepper by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry

A QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method To was established a QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for the simultaneous determination of 5 kinds of fungicides, namely, thiophanate methyl, dimethomorph, azoxystrobin and difenoconazole, in fresh pepper. Methods The samples were separated by extraction extracted with 2.0% acetic acid acetonitrile, purified by 50 mg C18 and 20 mg GCB, and detected by UPLC-MS/MS with matrix external standard method for quantification. Results The linear relationships between the peak areas and the corresponding mass concentrations of the 5 kinds of fungicides were good within the mass concentration range of 0.01?1.00 mg/L, and the correlation coefficients were all greater than 0.989. The average recoveries of the 5 kinds of fungicides at the 0.01, 0.1, and 1.0 mg/kg addition levels were 74%?105%, the relative standard deviations were 2.07%?9.61% (n=5), and the limits of quantification were 0.01 mg/kg. The residual amount of the five fungicides in Guizhou pepper was between <0.01 mg/kg to 0.092 mg/kg. Conclusion This method meets the requirements of pesticide residue detection and analysis, and is suitable for accurate qualitative and quantitative analysis of 5 kinds of pesticides in fresh pepper, market supervision and spot check, etc. The actual samples showed that the application of 5 kinds of fungicides in Guizhou pepper was safe, which did not produce related dietary risks and hazards, and did not affect export trade.