In order to fulfill the rapid,high throughput and high sensitive analysis of paraquat and diquat in complex biological samples,a convenient matrix assisted laser desorption ionization fourier transform ion cyclotron resonance mass spectrometric(MALDI-FTICR-MS) was developed for rapid detection of paraquat and diquat in seven vegetable samples,including benincasa hispida,cucumber,pakchoi,greengrocery,garlic chives,celery and lactuca sativa.In this study,the impacts of low concentrations of 2,5-dihydroxybenzoic acid(2,5-DHB) and α-cyano-4-hydroxycinnamic acid(CHCA) on the ionization response strength of paraquat and diquat were we compared.Simultaneously,the analytical results of different concentrations of CHCA mixed separately with pure standard solution and sample matrix standard solution in equal proportion were investigated.Ultimately,the extraction conditions for seven vegetable samples were optimized.The vegetable samples were extracted with acetonitrile solution containing 1% formic acid after homogenization by liquid-liquid extraction.After mixed with 2 g/L CHCA,the extracted solution was injected immediately.Results showed that different concentrations of CHCA as MALDI matrix had a noticeable influence on the ionization efficiency of paraquat and diquat in blank solvent and sample matrix.The response of pure standard solution was similar to that of the standard solution prepared with sample substrate as the concentration of CHCA was 2 g/L,which was more suitable for the establishment of detection method.There were good linear relationships for paraquat and diquat in seven vegetable samples in the mass concentration range of 2-200 μg/L,with their correlation coefficients(r) of 0.997 2-0.999 6.The limits of detections(LODs) and limits of quantitations(LOQs) of the method for paraquat were in the ranges of 1.0-1.5 μg/kg and 3.0-4.5 μg/kg,while the LODs and LOQs for diquat were 5.0-7.5 μg/kg and 15-23 μg/kg,respectively.The recoveries for paraquat at spiked levels ranged from 73.0% to 109%,with the relative standard deviations(RSDs) of 1.0%-8.2%,while the recoveries for diquat ranged from 81.7% to 117%,with the RSDs of 1.0%-7.0%.The analysis results were obtained by this method within 30 minutes.With the merits of rapidness,high sensitivity,reliability,stability,low solvent consumption and simple operation,this method could be used for the rapid and high throughput detection of paraquat and diquat in vegetables.