基于超高效液相色谱-四极杆/静电场轨道离子阱高分辨质谱法非靶向筛查典型三嗪类除草剂  

Non-targeted screening of triazine herbicides using ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry

作　　者：岳宁 李晓慧 王琦 李敏洁[1] 邵华[1] 郑鹭飞[1] 王静[1] 金芬[1] YUE Ning;LI Xiaohui;WANG Qi;LI Minjie;SHAO Hua;ZHENG Lufei;WANG Jing;JIN Fen(Institute of Quality Standard and Testing Technology for Agro-products,Chinese Academy of Agricultural Science,Beijing 100081,China)

机构地区：[1]中国农业科学院农业质量标准与检测技术研究所,北京100081

出　　处：《分析试验室》2023年第2期159-166,共8页Chinese Journal of Analysis Laboratory

基　　金：国家重点研发计划(2018YFC1602403)资助。

摘　　要：采用超高效液相色谱-四极杆/静电场轨道阱高分辨质谱(UPLC-Q-Orbitrap)研究典型三嗪类除草剂的特征质谱裂解规律。14种三嗪类除草剂的标准溶液经Acquity BEH C_(18)色谱柱(100 mm×3.0 mm,1.7μm)分离,用甲醇和0.1%甲酸水溶液进行梯度洗脱,在电喷雾正离子模式下采集离子信息。通过分析主要特征离子碎片发现:含O、含Cl和含S 3类亚型三嗪类除草剂质谱断裂方式包括:均三嗪环上氨基取代基的碳氮键断裂、均三嗪环上杂原子取代基自由基的丢失和均三嗪环的开环反应。含O三嗪类除草剂的主要特征离子碎片为m/z 142.07234和m/z 100.05060,含Cl三嗪类除草剂的主要特征离子碎片为m/z104.00017,含S三嗪类除草剂的主要特征离子碎片为m/z 116.02769。本研究中得到的三嗪类除草剂的裂解规律可作为非靶向筛查具有相似结构特征的三嗪类化合物的重要依据。Ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry(UPLC-Q-Orbitrap)was used to study the mass spectroscopic fragmentation pathway of triazine herbicides.A mixture of fourteen standard solutions of triazine herbicides was separated by Acquity BEH C_(18)column(100 mm×3.0 mm,1.7μm)using methanol and 0.1%formic acid solution as mobile phases for gradient elution.The precise mass-to-charge ratio of the first and second ions was collected under electrospray positive ion mode,and the fragmentation pathways of triazine herbicides were discussed based on fragmentation mechanism of organic compounds.The mass spectroscopic fragmentation pathways of fourteen oxytriazine,chlorotriazine and sulfur-containing triazine herbicides were studied,which mainly included the cleavage of carbon nitrogen bond of amino substituent on homotriazine ring,the loss of heteroatomic substituent radical on homotriazine ring and ring-opening reaction of homotriazine ring.The similar fragmentation patterns were found in mass spectra for triazine herbicides,in which four oxytriazine herbicides have the same fragment ion m/z 142.07234 and m/z 100.05060,five chlorotriazine herbicides have the same fragment ion m/z 104.00017,and five sulfur-containing triazine herbicides have the same fragment ion m/z 116.02769.The mass spectroscopic fragmentation pathway proposed provides an important basis for the rapid identification and analysis of triazine compounds with similar structural characteristics in complex systems.

关 键 词：三嗪类化合物 除草剂 超高效液相色谱-四极杆/静电场轨道离子阱质谱 裂解规律 

分 类 号：O657.63[理学—分析化学]