稳定同位素氘标记苯脲类除草剂的合成研究

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.

Synthesis of Stable Isotope Deuterium Substituted Phenylurea Hebicides

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.