论文部分内容阅读
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 m L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0.3μg/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。
Objective To establish a simple, rapid and sensitive liquid chromatography-mass spectrometry (LC-MS / MS) method for the determination of thiamethoxam pesticides residues in fruits. Methods Weigh 5 g of fruit samples and extract them by adding 20 mL of acetonitrile under ultrasonic agitation. The extract was dispersed solid phase using 20 mg of graphitized carbon black (Carb) and 60 mg of N-propyl ethylenediamine (PSA) powder Extraction purification, liquid chromatography mass spectrometry detection, external standard quantitative. Results Thiamethoxam pesticide residue chromatogram separation was good, the detection limit was 0.3μg / kg, the linear correlation coefficient was 0.9999, thiamethoxam in apple, pear, peach in the levels of 0.01,0.05,0.10 mg / kg, the recovery test showed that the average recovery of the method was 88.9% ~ 100.3% (n = 6), the relative standard deviation of 1.98% ~ 4.53%. Conclusion The method is simple, rapid and sensitive, and has a good purification effect and high recovery rate. It is suitable for the detection and safety monitoring of thiacloprid pesticide residues in fruits.