高效液相色谱法测定电合成反应液中的3,6-DCP和3,4,5,6-TCP  

The Simultaneous Determination of 3,6-DCP and 3,4,5,6-TCP in Electrochemical Synthesis Reaction Liquid by High Pevformance Liquid Chromalography

作　　者：曹军艳[1] 葛庆平 李娇娇[1] 王建设[1] 王留成[1] 宋成盈[1] 赵建宏[1] 

机构地区：[1]郑州大学化工能源学院,河南郑州450001 [2]河南省产品质量监督检验院,河南郑州450004

出　　处：《郑州大学学报（工学版）》2012年第6期100-103,共4页Journal of Zhengzhou University（Engineering Science）

基　　金：河南省基础与前沿技术研究计划资助项目(09230041006)

摘　　要：建立了同时测定电化学合成反应液中的3,6-二氯吡啶甲酸(3,6-DCP)和3,4,5,6-四氯吡啶甲酸(3,4,5,6-TCP)的高效液相色谱分析方法.实验采用Hypersil C18色谱柱,紫外检测器,检测波长280nm,采用V(乙腈)∶V(体积分数为1%的冰乙酸水溶液)=15∶85作流动相,恒定流速为1.0 mL/min,柱温25℃.结果表明,3,6-DCP和3,4,5,6-TCP在上述条件下可实现较好分离,两种物质测定结果的最大相对标准偏差分别为0.58%和0.40%,检出限分别为2.01×10-3g/L和5.09×10-3g/L,加标回收率分别在99.88%～100.5%和99.89%～100.1%.A method was presented for the simultaneous determination of 3,6-dichloropicolinic acid（3,6-DCP） and 3,4,5,6-tetrachloropicolinic acid（3,4,5,6-TCP） in the electrochemical synthesis reaction liquid by high performance liquid chromatography（HPLC）.The analysis was performed on a Hypersil C18 column with a mixture of V（acetonitrile）：V（volume fraction of 1% acetic acid aqueous solution）=15：85 as the mobile phase at a flow rate of 1.0mL/min.The samples were detected at 280 nm with an UV detector and the column temperature was 25℃.It was found that 3,6-DCP and 3,4,5,6-TCP could be well separated under the chromatographic conditions.The maximum relative standard deviations were 0.58% and 0.40% and the detection limits were 2.01×10^-3g/L and 5.09×10^-3g/L for 3,6-DCP and 3,4,5,6-TCP.The recoveries for them were 99.88%～100.5% and 99.89%～100.1%,respectively.

关 键 词：高效液相色谱 电化学合成 3 6-二氯吡啶甲酸 3 4 5 6-四氯吡啶甲酸 

分 类 号：O657.7[理学—分析化学]