摘要
研究了稳定同位素标记的玉米赤霉烯酮-苯环-^(13)C_(6)的全合成路线,即以苯-^(13)C_(6)为起始原料,经过硝化反应、硝基还原反应、Vilsmeier-Haack反应、Mitsunobu反应、Stille交叉偶联反应、格氏反应、关环复分解反应等共21步反应合成得到稳定同位素标记的玉米赤霉烯酮-苯环-^(13)C_(6)。产品结构、纯度和同位素丰度经核磁共振波谱(NMR)、高效液相色谱(HPLC)和质谱(MS)等仪器表征确定,玉米赤霉烯酮-苯环-^(13)C_(6)的色谱纯度和同位素丰度均高于98.0%。该化合物可以作为同位素内标,用于玉米赤霉烯酮的含量检测。
The synthesis of stable isotope-labeled zearalenone-bezene ring^(13)C_(6) had been achieved in 21 steps,including nitration,nitroreduction,Vilsmeier-Haack,Mitsunobu,Stille cross-coupling,Grignard reaction,ring-closing metathesis and so on.The structure,chemical purity and isotopic enrichment of the product were identified by NMR,HPLC and MS.The chemical purity and isotopic enrichment were higher than 98.0%.The result showed that the zearalenone-benzene ring^(13)C_(6) could be used as internal standard in the determination of zearalenone.
作者
邓晓军
赵超敏
曲栗
曹晨
陈武炼
李仁军
朱倩
徐敏
胡旭平
郭会
DENG Xiao-jun;ZHAO Chao-min;QU Li;CAO Chen;CHEN Wu-lian;LI Ren-jun;ZHU Qian;XU Min;HU Xu-ping;GUO Hui(Animal,Plant and Food Inspection and Quarantine Technology Center,Shanghai 200135,China;Anpel Laboratory Technologies(Shanghai)Inc.,Shanghai 201600,China)
出处
《化学研究与应用》
CAS
CSCD
北大核心
2021年第9期1744-1754,共11页
Chemical Research and Application
基金
国家食品安全重点科技专项项目(2017YFC1601300)资助。
关键词
玉米赤霉烯酮
稳定同位素标记
合成
表征
zearalenone
stable isotope labeled
synthesis
characterization
