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化学学报
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化学学报 ›› 2011, Vol. 69 ›› Issue (12): 1445-1449. 上一篇    下一篇

研究论文

新型杀菌剂唑菌酯吡唑环14C标记合成和鉴定

刘训悦，阚登蕾，丁兴成*   

  1. (浙江大学原子核农业科学研究所 杭州 310029)
  • 投稿日期:2010-10-08 修回日期:2011-02-16 发布日期:2011-02-28
  • 通讯作者: 丁兴成 E-mail:dingxch@zju.edu.cn
  • 基金资助:

    新型高效杀菌剂唑菌酯14C标记化合物的设计、合成与环境行为研究;杀菌剂唑菌酯(SYP-3343)14C标记合成及降解途径与产物组成研究;新型杀菌剂唑菌酯14C标记化合物的微量合成研究

Synthesis and Identification of 14C labelled Pyraoxystrobin

LIU Xun-Yue, HAN Deng-Lei, DING Xing-Cheng   

  1. (Institute of Nuclear-Agricultural Science, Zhejiang University, Hangzhou 310029)
  • Received:2010-10-08 Revised:2011-02-16 Published:2011-02-28

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为研究新型杀菌剂唑菌酯在土壤中的代谢途径、作用机理及环境行为, 以14C-对氯苯甲酸为原料, 通过取代、环化、缩合三步反应合成吡唑环14C标记的唑菌酯. 采用高效液相色谱-质谱联用仪(电喷雾离子源)[HPLC-MS (ESI)], 质谱法(电子轰击离子源)[MS (EI)], 核磁共振氢谱法(1H NMR)验证了其结构, 通过HPLC外标法确定其质量纯度大于98%;液相色谱-流动液闪联用仪(HPLC-LSC)和薄层色谱-同位素成像分析法(TLC-IIA)两种方法分析表明, 其放射化学纯度大于98%, 比活度为(5.042±0.076) mCi/mmol. 以总反应收率计, 合成反应的化学收率和放化收率均为43.93%.

关键词: 唑菌酯, 14C标记合成, 鉴定, 杀菌剂

In order to study the metabolism, mode of action and other environmental behaviors of novel fungicide pyraoxystrobin, a 14C labelled pyraoxystrobin was synthesized from 4-chlorobenzoic acid as 14C labeled carbon source via substitution, cyclization and condensation. Its chemical structure was identified by HPLC-MS (ESI), MS (EI) and 1H NMR, its purity was determinated by HPLC with more than 98% in mass ratio. HPLC-LSC and TLC-IIA determination demonstrated that its radiochemical purity was more than 98% with specific activity of (5.042±0.076) mCi/mmol. According to the total synthetic yield, the total chemical yield and radiochemical yield were both 43.93%.

Key words: pyraoxystrobin, 14C labeled synthesis, identification, fungicide