【摘要】 为制备HPLC-MS/MS农药残留分析中使用的苯脲类除草剂同位素内标物,以取代苯胺为原料,与三光气反应制得取代的苯基异氰酸酯,再与二甲胺-D₆盐酸盐亲核加成,合成了9种苯脲类除草剂的氘取代物,分别是敌草隆-D₆、灭草隆-D₆、2,3-敌草隆-D₆、绿麦隆-D₆、甲氧隆-D₆、秀草隆-D₆、非草隆-D₆、伏草隆-D₆和异丙隆-D₆。通过NMR、MS、UV对其进行结构确证,化学纯度均大于98%,同位素丰度大于99.5%,完全满足质谱分析对内标物的要求,可作为HPLC-MS/MS分析的同位素内标物。更多还原

【Abstract】 In order to prepare isotope internal standards of phenylurea hebicides for pesticide residue HPLC-MS/MS analysis,the N,N-dimethyl-deuterated forms of nine ingredients were synthesized form substituted phenylamine in two simple steps via the reaction with triphosgene,and nucleophilic addition with dimethyl-D₆-amine hydrochloride,the deuterium substituted compounds include Diuron-D₆,Monuron-D₆,2,3-Diuron-D₆,Chlorotoluron-D₆,Metoxuron-D₆,Bromuron-D₆,Fenuron-D₆,Fluometuron-D₆ and Isoproturon-D₆. The structures were confirmed by NMR,MS and UV. The purities of all chemicals are more than 98%,meanwhile,all the isotope purities are more than 99. 5%. These deuterium substituted compounds could be used an isotope internal standards by HPLC-MS/MS.更多还原