摘要:
以菠菜、苹果和大豆为代表性分析物,建立了超高效液相色谱-串联质谱法(U PLC-M S/M S)检测蔬菜、水果及粮谷等植物源性食品中8种二硝基苯胺类除草剂(氟乐灵、二甲戊乐灵、仲丁灵、异乐灵、磺乐灵、氨基乙氟灵、氨磺乐灵和氨基丙氟灵)的残留量.采用电喷雾电离,正离子扫描,多反应监测(M RM)模式检测,并使用外标法定量.结果表明:8种二硝基苯胺类除草剂的测定低限均为10 μg/kg;在添加水平10~200 μg/kg范围内,加标回收率为70.0% ~120%,相对标准偏差为0.56% ~23.0%.该方法灵敏、有效,适用于蔬菜、水果和粮谷等植物源性食品中二硝基苯胺类除草剂多残留的测定.
Abstract:
A method of ultra performance liquid chromatography-tandem mass spectrom-etry(UPLC-MS/MS)was developed for determination of 8 kinds of dinitroaniline herbi-cides(trifluralin,pendimethalin,butralin,isopropalin,dinitramine,nitralin,oryzalin, prodiamine)in spinach,apple and soybean.Afer homogenization,5.0 g sample was soaked with 7 mL water for 1 h.Then 3 g NaCl was added,and the sample was extrac-ted twice by 25 mL hexane saturated acetonitrile solution.After concentration,the extract was put through C18 column and eluted by 5 mL acetonitrile.The eluated was then concentrated and dissolved with 2.0 mL hexane-acetone mixture(2:8,V/V).The preparation was cleaned by Envi-Carb column and eluted with 5.0 mL hexane-acetone. The residue was dissolved by 50% acetonitrile aqueous solution(contain 0.1% formic acid),and determined by UPLC-ESI/MS/MS.Under the optimized chromatographic conditions,8 target compounds were obtained.Confirmation was achieved using electro-spray ionization(ESI)in positive mode with multiple reaction monitoring(MRM),and external standard method was used for quantification.The results show that 8 dinitroa-niline herbicides have good linearity,the linearity is more than 0.99.T he limits of quantification(LOQs)are 10 μg/kg.The mean recoveries are between 70.0% and 120%at the spiked levels of 10-200 μg/kg.The RSD of the method are between 0.56% and 23.0%.T he method is precise,sensitive and accurate,which is suitable for confirma-tion and quantification of dinitroaniline herbicides in vegetables,fruits and grains.