超高效液相色谱-串联质谱法测定生菜中氟吡菌酰胺及其代谢物残留量

Determination of fluopyram and its metabolite residues in Lactuca sativa by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  超高效液相色谱-串联质谱法  氟吡菌酰胺  代谢物  生菜

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  fluopyram  metabolites  Lactuca sativa

中文摘要:

      目的 建立超高效液相色谱-串联质谱法测定生菜中氟吡菌酰胺及其代谢物2-(三氟甲基)苯甲酰胺的方法。方法 采用QuEChERS技术, 用乙腈对生菜样品进行萃取, C18净化剂净化后, 用含0.1%甲酸的乙酸铵溶液-乙腈在BEH C18色谱柱上进行洗脱分离, 质谱检测器测定。结果 氟吡菌酰胺和2-(三氟甲基)苯甲酰胺在1.0~50.0 ng/mL质量浓度范围内, 质量浓度与其质谱响应强度之间呈线性关系, 相关系数不小于0.9996; 检出限为0.25 μg/kg, 定量限为0.10 μg/kg; 回收率平均值在94.6%~97.2%, 相对标准偏差为1.3%~4.5%。结论 所建超高效液相色谱-串联质谱法灵敏度高、精密度好、准确度高、前处理简便, 可为生菜农药残留监测及氟吡菌酰胺农药残留消解动态分析提供技术支撑。

英文摘要:

      Objective To establish a method for the determination of flupyram and its metabolite 2-(trifluoromethyl) benzamide in Lactuca sativa by ultra performance liquid chromatography-tandem mass spectrometry. Methods Using QuEChERS technology, Lactuca sativa samples were extracted with acetonitrile. After purification with C18 purification agent, ammonium acetate solution containing 0.1% formic acid-acetonitrile was eluted and separated on a BEH C18 chromatographic column, and determined by a mass spectrometry detector. Results There was a linear relationship between the mass concentration of flupyram and 2-(trifluoromethyl) benzamide in the range of 1.0 to 50.0 ng/mL and their mass response intensity, with a correlation coefficient not less than 0.9996. The limits of detection were 0.25 μg/kg, and limits of quantification were 0.10 μg/kg; the average recovery rates were 94.6% to 97.2%, and the relative standard deviations were 1.3% to 4.5%. Conclusion The method has a high degree of sensitivity, precision, accuracy, and a simple pre-treatment process, can provide technical support for monitoring lettuce pesticide residues and dynamic analysis of flupyram pesticide residues.