超高效液相色谱-串联质谱法测定甜菜中甜菜安和甜菜宁的残留量

Residue Determination of Desmedipham and Phenmedipham in Sugar Beet Using Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

建立了同时测定甜菜安和甜菜宁在甜菜中残留量的分析方法。样品用乙腈和水混合振荡提取,盐析后取有机相浓缩,浓缩液经PSA分散固相萃取净化,超高效液相色谱-串联质谱测定。测定结果,甜菜安在甜菜中的平均回收率为91.1%~95.6%,相对标准偏差为2.4%~7.6%;甜菜宁在甜菜中的平均回收率为93.4%~95.8%,相对标准偏差为5.0%~9.8%。甜菜安及甜菜宁在甜菜中的定量限(LOQ)均为0.02 mg/kg;甜菜安的检出限(LOD)为1.5×10^-3 mg/kg,甜菜宁的检出限为2.6×10^-4 mg/kg。田间试验表明:甜菜苗期施药,收获期甜菜中的甜菜安及甜菜宁残留量均低于0.02 mg/kg。

A method for simultaneously determined the residue of desmedipham and phenmedipham in sugar beet was developed.The sample was extracted with mixture of acetonitrile and water,and the organic phase was concentrated after salting out.The concentrated liquid was purified by PSA(dispersion solid-phase extraction)and then determined by UPLC-MS/MS.The results indicated that the average recoveries of desmedipham in sugar beet were 91.1%-95.6%,and their relative standard deviations were 2.4%-7.6%.The average recoveries of phenmedipham in sugar beet were 93.4%-95.8%,and their relative standard deviations were 5.0%-9.8%.The limits of quantitation(LOQ)of desmedipham and phenmedipham in sugar beet were both 0.02 mg/kg.The LOD of desmedipham and phenmedipham was 1.5×10^-3 mg/kg and 2.6×10^-4 mg/kg,respectively.The field experiments indicated that the residues of desmedipham and phenmedipham were lower than 0.02 mg/kg at the harvest when the herbicide product was used in seeding stage of sugar beet.