高比活度碳-14标记毒氟磷的合成与分析

以14C]碳酸钡为放射性同位素原料，通过格氏反应、Curtius重排、亲核加成、硫代及关环等7步反应，制备了同位素碳-14标记的毒氟磷粗品，经反相高效液相色谱（RP-HPLC）纯化获得标记物纯品14C-毒氟磷（N-2-（4-甲基苯并2-14C]噻唑基）]-2-氨基-2-氟代苯基-O，O-二乙基甲基膦酸酯，38.3 mCi）。7步反应的化学收率/放化收率为10%。其结构经核磁共振氢谱、质谱和放射性高效液相色谱（HPLC-FSA）分析确认。放射性薄层成像分析（TLC-IIA）、高效液相色谱-液体闪烁测量联用分析（HPLC-LSC）、高效液相色谱-流动液体闪烁测量/二极管阵列检测器/质谱联用分析（HPLC-FSA/PDA/MS）和LSC分析表明，14C-毒氟磷的放化纯度和化学纯度均大于98%，比活度为58.0 mCi/mmol，可作为放射性示踪剂，用于毒氟磷的代谢和环境行为等研究。

Synthesis and analysis of carbon-14 labelled Dufulin with high specific activity

Carbon-14 labelled Dufulin, diethyl ((2-fluorophenyl)((4-methylbenzo2-¹⁴C]thiazol-2-yl) amino)methyl)phosphonate was synthesized from barium ¹⁴C]carbonate via Grignard reaction, Curtius arrangement, nucleophilic addition, thionation reaction, cyclization reaction, etc. The labelled product (38.3 mCi) was obtained after RP-HPLC purification in the overall radiochemical/chemical yield of 10%. The product was characterized by ESI-MS, ¹H NMR and HPLC-FSA. Its technical data (radiochemical purity > 98%, chemical purity > 98%, specific activity 58.0 mCi/mmol) was determined by TLC-IIA, HPLC-LSC, HPLC-FSA/PDA/MS and LSC. This carbon-14 labelled Dufulin can be used as radiotracer in the study on its metabolism and environmental behavior by employing radioisotope tracing techniques.