目的建立一种应用气相色谱-质谱联用法测定蔬菜、小麦粉、糙米和西瓜中恶霉灵残留量。方法前处理用乙腈提取,提取液使用固相萃取柱(2 g/10 ml)净化,最终提取液用硅烷化试剂(BSTFA)进行衍生化。气相方法以DB-5ms毛细管柱(30 m×0.25 mm,0.25μm)处理,质谱选择离子监测模式(SIM)测定。结果小麦粉和多种蔬菜的恶霉灵在0.010和0.100 mg/kg两个浓度水平的加标回收率范围为63%~101%,不同样品回收率RSD<10%,方法检出限为0.003 mg/kg,定量限为0.005 mg/kg。结论该方法灵敏度高,重现性好,适用于快速检测蔬菜和小麦粉的恶霉灵残留量。 Objective To establish a method for the determination of hymecromone residues in vegetables, wheat flour, brown rice and watermelon by gas chromatography-mass spectrometry. Methods Pretreatment was extracted with acetonitrile. The extracts were purified using a solid phase extraction cartridge (2 g / 10 ml) and the final extract was derivatized with a silylating reagent (BSTFA). The gas phase method was performed on a DB-5ms capillary column (30 m × 0.25 mm, 0.25 μm) with mass spectrometry selected ion monitoring mode (SIM). Results The spiked recoveries ranged from 63% to 101% at the concentrations of 0.010 mg / kg and 0.100 mg / kg for wheat flour and various vegetables. The RSDs of different samples were less than 10%, and the detection limits were 0.003 mg / kg, the limit of quantification is 0.005 mg / kg. Conclusion The method has high sensitivity and good reproducibility and is suitable for rapid detection of hymexazol residues in vegetables and wheat flour.