QuEChERS-超高效液相色谱-串联质谱法快速检测果蔬中35种甲氧基丙烯酸酯类和三唑类杀菌剂的残留量

Simultaneous determination 35 kinds of Strobilurin Fungicides and Triazole Fungicide in fruit and vegetable by QuEChERS-UPLC-MS/MS

中文关键词:  甲氧基丙烯酸酯类杀菌剂  三唑类杀菌剂  残留  QuEChERS  超高效液相色谱-串联质谱  果蔬

英文关键词:strobilurin fungicides  triazole fungicides  residues  QuEChERS  ultra performance liquid chromatography-tandem mass spectrometry  fruit and vegetable

中文摘要:

      目的 建立一种测定水果蔬菜中甲氧基丙烯酸酯类和三唑类35种杀菌剂残留量的超高压液相色谱-串联质谱检测方法。方法 样品用乙腈提取和QuEChERS方法净化, 采用C18柱子以0.2%甲酸溶液-乙腈作为流动相进行梯度洗脱, 质谱(ESI+)电喷雾正离子模式电离，采用多离子检测模式(MRM)对35种杀菌剂的定量离子和定性离子进行监测。结果 本方法中35种杀菌剂在1.0~50 μg/L的浓度范围内线性关系良好, 相关系数r2为 0.9990~0.9998；在0.005、0.050、0.100 mg/kg添加水平的回收率为61.8%~123%, 方法定量限为1.0~1.5 μg/kg。 结论 该方法快速、环境友好、准确、灵敏, 适合水果蔬菜甲氧基丙烯酸酯类和三唑类杀菌剂残留的检测。

英文摘要:

      ABSTRACT: Objective To establish a fast method for simultaneously determination of 35novel amide fungicides in fruits and vegetables by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS-MS). Methods The fungicides residues were extracted from the samples by acetonitrile and cleaned-up with QuEChERS, the separation was performed on C18 column with the gradient elution of acetonitrile(A) and 0.2% formic acid solution(B) by UPLC-MS-MS. Using LC–MS/MS (ESI+) with multiple reactions monitoring (MRM), identification of the major components of the 35 kinds of fungicides residues was performed based upon the intensities of fragments. Results The method showed a good linearity over the range of 1.0-50 μg/L with correlation coefficients r2 of 0.9990-0.9998. The recoveries were ranged from 61.8%~123% for the 35 kinds of fungicides residues with 2 spiked levels of 0.005, 0.050 and0.100 mg/kg, and the limits of quantitation (LOQ) for the 35 kinds of fungicides were 1.0-1.5 μg/kg. Conclusion The method is fast, environmental friendly with high sensitivity and good reproducibility which is suitable for the determination of the contents of 35 kinds of strobilurin fungicides and triazole fungicides residues in fruit and vegeta-ble.