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作 者:皮运清[1] 郭伟[1,2] 冯精兰[1] 孙剑辉[1]
机构地区:[1]河南师范大学环境学院,河南省环境污染控制重点实验室,黄淮水环境与污染防治省部共建教育部重点实验室,新乡453007 [2]新乡医学院化学教研室,新乡453003
出 处:《分析试验室》2014年第4期408-411,共4页Chinese Journal of Analysis Laboratory
基 金:河南省创新型科技人才队伍建设工程;河南省科技创新人才计划(134200510014);河南省基础与前沿技术研究(102300410098;112300410204;132330410138);河南省重点科技攻关项目(102102310244;102102310303)资助
摘 要:建立了利用红外色谱辅助高效液相色谱串联质谱鉴定中间产物的方法。Fenton试剂(H2O2和Fe2+的混合溶液)降解氧氟沙星反应中得到的样品,经过高效液相色谱的梯度洗脱将中间产物分离,随后直接进入质谱检测,得到中间产物的分子式;同样经过冷冻干燥的样品,通过红外色谱的辅助确定降解中间产物缺失的官能团,从而得到中间产物的结构。方法适用于中间产物的鉴定,可以有效解决因中间降解产物浓度低,难以分离而无法确定其结构的弊端。An analytical method for the determination of transformation product (TP) formed upon the oxidative degradation of ofloxacin within Fenton reaction by high performance liquid chromatography-high resolution mass spectrometry (LC-MS) and Infrared chromatography was established. High performance liquid chromatographyhigh resolution mass spectrometry (LC-MS) was employed to identify the TP, where the molecular weight and formula of the TP can be obtained. Infrared chromatography was then used to aid the determination of the specific functional group lost during the degradation process, thereby giving rise to the detailed structural information of the TP. This method is of great importance because it offers insights into tackling the drawbacks existing in the conventional approaches, where the exact structures of the TP could not be determined due to their limited concentrations and separation difficulty.
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