动态微波辅助萃取法快速萃取苹果中8种氨基甲酸酯类农药

Rapid extraction of carbamate pesticides from apple on dynamic microwave-assisted extraction

目的建立一种绿色的动态微波辅助快速萃取法结合高效液相色谱-串联质谱法测定苹果中8种氨基甲酸酯类农药的方法。方法以水为萃取溶剂,利用动态微波辅助萃取法对苹果中氨基甲酸酯类农药进行快速萃取;通过两步固相萃取法对所获得的萃取物进行净化和富集;采用高效液相色谱.串联质谱法对目标化合物进行测定。结果实验中对影响动态微波辅助萃取和固相萃取效率的实验条件进行了优化,最优的实验条件为:萃取剂为纯水;微波萃取功率为600 W;微波萃取时间为10 min;萃取剂流速为1.0 mL/min;固相萃取洗脱剂为2 mL的乙醇。8种氨基甲酸酯类农药在8.0~800 ng/g范围内成线性关系,相关系数为0.994~0.999;检出限为1.1~4.2 ng/g;方法的加标(8.0 ng/g)回收率为71%~90%。结论该方法可以用于苹果中氨基甲酸酯类农药的快速检测。

Objective A green and fast sample pretreatment method was proposed for determination of 8 carbamate pesticides from apple. Methods The 8 carbamate pesticides in apple samples were extracted by dynamic microwave-assisted extraction with water as extraction solvent. The extract obtained was purified by two steps SPE. Finally, the extract was injected into the LC-MS/MS system for analysis. The parameters which could affect the extraction efficiency were optimized. Results The optimized extraction conditions were observed at water as extraction solvent; 600 W of microwave forward power; extraction time, 10 min;extraction solvent flow-rate, 1.0 mL/min; 2 mL ethanol as the elution solvent of SPE. The linearity ranges of the proposed method from 8.0 to 800 ng/g were obtained and the correlation coefficient were 0.994~0.999. The limits of detection for the eight carbamate pesticides were in the range of 1.1~4.2 ng/g. The recoveries of the eight carbamate pesticides for the spiked samples (8.0 ng/g) were in the range of 71%~90%. Conclusion This method could be applied to rapid detection of carbamate pesticides from apple.