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以[~(14)C]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~(14)C-毒氟磷(N-[2-(4-甲基苯并[2-~(14)C]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,~(14)C-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。
The [~ (14) C] barium carbonate was used as a raw material for radioisotope to prepare isotope carbon-14 labeled toxic fluorine phosphorus by Grignard reaction, Curtius rearrangement, nucleophilic addition, The crude product was purified by reverse-phase high-performance liquid chromatography (RP-HPLC) to obtain the pure product labeled with ~ (14) C- ] Thiazolyl)] - 2-amino-2-fluorophenyl-O, O-diethylmethylphosphonate, 38.3 mCi). The chemical yield / radiochemical yield of the 7-step reaction was 10%. Its structure was confirmed by 1H NMR, MS and HPLC-FSA. (TLC-IIA), high performance liquid chromatography-liquid scintillation spectrometry (HPLC-LSC), high performance liquid chromatography-flow liquid scintillation spectrometry / diode array detector / mass spectrometry (HPLC- FSA / PDA / MS) and LSC analysis showed that the radiochemical purity and chemical purity of ~ (14) C-detoxifloxacin were both higher than 98% and the specific activity was 58.0 mCi / mmol, which could be used as radiotracer in Toxic fluorine phosphorus metabolism and environmental behavior research.