SPE-UPLC-MS法同时检测乳制品中11种三嗪类除草剂的残留

优化固相萃取(SPE)条件,采用SPE前处理,结合超高效液相色谱-质谱联用法(UPLC-MS)检测乳制品中11种常用三嗪类除草剂,即西码津、莠去津、西草净、阿特拉津、仲丁通、扑灭通、莠灭净、扑灭津、特丁津、扑草净、特丁净的残留量.分析方法为:经过Varian Plexa SPE柱处理的乳制品,用Waters BEH C...

Multiresidue Determination of 11 Triazine Herbicides in Milk By SPE-UPLC-MS

The contents of simazine,atraton,simetryn,atrazine,secbumeton,prometon,ametryn,propazine,terbuthylazine,prometryn and terbutryn in milk were determined by ultra performance liquid chromatography-mass spectrum（UPLC-MS） after the pre-treatment with optimized SPE.The analytical conditions were as follows：triazine herbicides,which were extracted from milk samples with Varian Plexa SPE column,were chromatographed with a Waters BEH C18 column（2.1×100 mm,1.7 μm） eluted with water and acetonitrile in gradient mode,and detected with Waters Q-Tof Premier MS in positive full-scan mode from m/z 50 to 600.Then all triazine ions were extracted from total ion chromatograms（TIC）,and quantitated with external standard method.The results showed that a satisfactory linear relationship was presented between the detecting signal and concentrations of triazine over the range of 1.0～200.0 ng/mL.The regression coefficient was greater than 0.99.The detection range of 11 triazine herbicides in milk was 1.0～40.0 ng/g with the recovery of 84.30%～106.99%,RSD of 0.04%～5.01% and detection limit of 0.02～0.08 ng/g.This method was significant for monitoring triazine herbicide residues in milk products accurately and efficiently.