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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: To establish a method for the determination of 8 carbamates pesticides in apples by using the rapid dynamic microwave assisted extraction and high performance liquid chromatography-tandem mass spectrometry. Methods Water was used as the extraction solvent, and the dynamic microwave-assisted extraction method was used to extract the carbamate pesticides in apple rapidly. The two extracts were purified and enriched by two-step solid-phase extraction. The HPLC was used. The target compound was determined by tandem mass spectrometry. Results The experimental conditions influencing the efficiency of dynamic microwave assisted extraction and solid-phase extraction were optimized in this experiment. The optimal experimental conditions were as follows: extraction solvent was pure water, microwave extraction power was 600 W, microwave extraction time was 10 min, The flow rate was 1.0 mL / min and the solid-phase extraction eluent was 2 mL of ethanol. The linear relationships were obtained for the eight carbamates in the range of 8.0-800 ng / g with a correlation coefficient of 0.994-0.999. The detection limits were 1.1-4.2 ng / g. The spiked (8.0 ng / g) recoveries For 71% ~ 90%. Conclusion The method can be applied to the rapid detection of carbamates pesticides in apples.