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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-D_6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-D_6、灭草隆-D_6、2,3-敌草隆-D_6、绿麦隆-D_6、甲氧隆-D_6、秀草隆-D_6、非草隆-D_6、伏草隆-D_6和异丙隆-D_6。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。
In order to prepare the internal standard of phenylurea herbicide isotope used in the analysis of pesticide residues in HPLC-MS / MS, the substituted phenyl isocyanate was prepared by reacting substituted aniline with triphosgene and reacted with dimethylamine-D_6 hydrochloride Salt nucleophilic addition, deuterium substitutes of nine kinds of phenylurea herbicides were synthesized, namely diuron-D_6, vancomycin-D_6,2,3-diuron-D_6, Methoxynil-D_6, Xuron-D_6, Fusarium-D_6, Fusulin-D_6 and Isoproturon-D_6. Its structure was confirmed by NMR, MS and UV. The chemical purity was more than 98% and the abundance of isotope was more than 99.5%. It fully satisfied the requirements of mass spectrometry for internal standard and could be used as isotope internal standard for HPLC-MS / MS .