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三唑并嘧啶磺酰胺类除草剂的定性鉴别

Qualitative Identification of Triazolopyrimidine Sulfonamide-Herbicides

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【作者】 狄矢聪强音陈青徐春春林苗

【Author】 DI Shi-cong;QIANG Yin;CHEN Qing;XU Chun-chun;LIN Miao;Key Laboratory of Science and Technology of Eco-Textile,Ministry of Education,College of Chemistry,Chemical Engineering and Biotechnology,Donghua University;Shanghai Entry-Exit Inspection and Quarantine Bureau;

【机构】 东华大学化学化工与生物工程学院生态纺织教育部重点实验室上海出入境检验检疫局

【摘要】 采用红外吸收光谱,核磁共振氢谱,超高效液相色谱-四极杆飞行时间质谱对3种三唑并嘧啶磺酰胺类除草剂进行分析。红外吸收谱图表明:3 3603 180,1 630,1 540,1 500,1 300,1 150cm-1附近的峰是此类除草剂的特征吸收,根据嘧啶环上取代基的不同引起的波数变化可加以区分鉴别;氢核磁共振谱图表明:δH7.469.38,δH10.8211.91分别为嘧啶环氢和磺酰胺基氢特征位移,根据嘧啶环上取代基不同引起的化学位移的差异可加以区分鉴别;超高效液相色谱-四极杆飞行时间质谱图表明:磺酰胺基桥链是最容易断裂的基团,并产生相应特征离子碎片。3种谱图联用可对此类化合物定性鉴别。

【Abstract】 IRS,1 H-NMR and UHPLC-Q/TOF MS were used for analysis of 3 triazolopyrimidine sulfonamide-herbicides.As shown by the IR spectra,characteristic absorption peaks of the 3herbicides were found at 3 360-3 180,1 630,1 540,1 500,1 300,1 150cm-1.They could be distinguished from each other according to the change of wave number aroused from different substitute groups in the pyrimidine ring.It was shown by the1 H-NMR spectra,that characteristic shifts atδH7.46-9.38andδH10.82-11.91 were due to the hydrogen atoms present in the pyrimidine ring and the sulfonamide group.They could be distinguished from each other according to the chemical shifts aroused from different substitute groups in the pyrimidine ring.As shown in the mass spectra obtained by UHPLC-Q/TOF MS,sulfaminebridging group was easy to break,and the corresponding characteristic ion fragments were produced.By co-interpretation of the spectra obtained by the above mentioned methods qualitative identification of the 3kinds of herbicides was attained effectively.

【基金】 国家质检总局科研专项(2014IK259)
  • 【文献出处】 理化检验(化学分册) ,Physical Testing and Chemical Analysis(Part B:Chemical Analysis) , 编辑部邮箱 ,2016年08期
  • 【分类号】O657.63;TQ457.2
  • 【被引频次】2
  • 【下载频次】178
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