QuEChERS-高效液相色谱-串联质谱法 测定苹果中丁醚脲及其代谢物残留量

Determination of diafenthiuron and its metabolites residue in apple by QuEChERS- high performance liquid chromatography-tandem mass spectrometry

中文关键词:  丁醚脲及其代谢物  QuEChERS  高效液相色谱-串联质谱法

英文关键词:diafenthiuron and its metabolites  QuEChERS  high performance liquid chromatography- tandem mass spectrometry

中文摘要:

      目的 建立基于QuEChERS-高效液相色谱-串联质谱测定苹果中的丁醚脲及其代谢物丁醚脲-脲和丁醚脲-甲酰胺残留量的方法。方法 样品经乙腈提取后用PSA作为固相分散萃取剂净化除杂, 以0.1%甲酸乙腈溶液和0.1%甲酸水溶液(含10 mmol/L甲酸铵)为流动相进行梯度洗脱, 高效液相色谱-串联质谱法正离子多反应监测模式(MRM)测定。结果 丁醚脲及其代谢物在5~100 μg/L的范围内有良好的线性, 相关系数(R2)>0.999。定量限5 μg/kg为以空白苹果为基质, 在5、10、50 μg/kg三个水平的加标回收率范围在78.3%~103.1%之间, 精密度在2.1%~8.2%之间。结论 该方法前处理快速简单, 可用于对进出口的苹果中丁醚脲及其代谢物的检测。

英文摘要:

      Objective To establish a method to detect the diafenthiuron and its metabolites residue in apple by QuEChERS-high performance liquid chromatography-tandem mass spectrometry. Methods The samples were extracted with acetonitrile and cleaned up by PSA. The separation was carried out with a gradient elution using 0.1% formic acid acetonitrile solution and 0.1% formic acid solution (10 mmol/L ammonium formate) as mobile phases. The analysis of diafenthiuron and its metabolites was performed under electrospray positive ionization MRM mode. Results A good linearity (R2>0.999) was achieved for the target compounds in the range of 5~100 μg/L. The limit of quantification was 5 μg/kg. The recoveries at the three spiked levels (5, 10, and 20 μg/kg) in the blank matrix were ranged from 78.3% to103.1%, with the relative standard deviations varied from 2.1% to 8.2%. Conclusion The method is accurate and efficient, and can be applied to the determination of diafenthiuron and its metabolites residue in apple for import and export.