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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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:3 360~3 180,1 630,1 540,1 500,1 300,1 150 cm-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:δH 7.46~9.38,δH 10.82~11.91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, 1H-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 3 herbicides were found at 3 360-3 180, 1 630, 1 540, 1 500, 1 300, 1 150 cm-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 the 1H-NMR spectra, that characteristic shifts at δH 7.46-9.38 and δH 10.82-11.91 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 3 kinds of herbicides was attained effectively.