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

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

中文关键词:  辣椒  残留  超高效液相色谱-串联质谱法  杀菌剂

英文关键词:pepper  residue  ultra performance liquid chromatography-tandem mass spectrometry  fungicides

中文摘要:

      目的 建立QuEChERS-超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)同时检测辣椒中多菌灵、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, 50 mg C18和20 mg GCB净化, 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。

英文摘要:

      Objective To establish a method for the simultaneous determination of 5 kinds of fungicides (namely, thiophanate methyl, dimethomorph, azoxystrobin and difenoconazole) in pepper by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The samples were 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 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 of method were 0.01 mg/kg. The residual amount of 5 kinds of 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 pepper, market supervision and spot check, etc. The actual samples showed that the application of 5 kinds of fungicides in Guizhou pepper is safe, which does not produce related dietary risks and hazards, and does not affect export trade.