水果中噻虫嗪农药残留LC/MS/MS测定

Determination of thiamethoxam in fruit by high performance liquid chro-matography-mass spectrometry/mass spectrometry

中文关键词:  水果  噻虫嗪  液相色谱-质谱法

英文关键词:fruit  thiamethoxam  liquid chromatography-mass spectrometry/mass spectrometry

中文摘要:

      目的 建立一种简单、快速、灵敏的水果中噻虫嗪农药残留的液相色谱-串联质谱(liquid chromatography-mass spectrometry/mass spectrometry, LC-MS/MS)分析方法。方法 称取水果样品5 g, 加入乙腈20 mL在超声波振荡条件下提取, 提取液使用20 mg石墨化炭黑(Carb)和 60 mg N-丙基乙二胺(PSA)粉末进行分散固相萃取净化, 经液相色谱质谱联用仪检测, 外标法定量。结果 噻虫嗪农药残留的色谱图分离效果良好, 方法的检出限为0.3 μg/kg, 线性相关系数为0.9999, 噻虫嗪在苹果、梨、桃中的添加水平为0.01、0.05、0.10 mg/kg, 回收试验表明该方法平均回收率为88.9%~100.3% (n=6), 相对标准偏差为1.98%~4.53%。结论 该方法简单、快速、灵敏、净化效果好、回收率高, 适合水果中噻虫嗪农药残留的检测和安全监控。

英文摘要:

      Objective To establish an easy, rapid and sensitive method to determine thiamethoxam pesticide residues in fruit by utilizing liquid chromatography-mass spectrometry/mass spectrometry (LC-MS/MS). Methods Fruit sample 5 g with 20 mL acetonitrile was extracted in the condition of ultrasonic oscillation , then the extract was purified by dispersive solid phase extraction using 20 mg carb and 60 mg PSA as purification sorbent and determined by LC/MS/MS. Results A good separation for thiamethoxam was achieved, with a correlation coefficients about 0.9999. The detection limit of the method was 0.3 μg/kg. The average recoveries of thiamethoxam ranged from 88.9% to 100.3% in the range of 0.01 mg/kg, 0.05 mg/kg and 0.10 mg/kg in apple, pear and peach, and the relative standard deviation (RSD) was between 1.98% and 4.53%, respectively. Conclusion The method is simple, rapid and sensitive, with a good purifying effect and a high recovery rate, which is suitable for the detection and security monitoring of the thiamethoxam in fruit.