以Na4EDTA为络合剂,以五氟苄基溴为衍生试剂,采用快速溶剂萃取仪萃取,同时实现土壤酸性除草剂的络合萃取在线衍生,并以气相色谱-质谱(NCI源)进行检测。对络合条件、衍生条件、萃取条件、离子源选择进行了优化。方法的回收率为75%～95%、相对标准偏差为6.7%～13%、检测限2.8～8.4μg/Kg。 Na4EDTA was used as the complexing agent and pentafluorobenzyl bromide was used as the derivatization reagent. The extract was extracted by fast solvent extraction. At the same time, the complexation extraction of acid soil herbicide was carried out on-line and detected by gas chromatography-mass spectrometry (NCI source). Complex conditions, derivatization conditions, extraction conditions, ion source selection were optimized. The recovery of the method was 75% ~ 95%, the relative standard deviation was 6.7% ~ 13%, and the detection limit was 2.8 ~ 8.4μg / Kg.