[1]曹军艳,葛庆平,李娇娇,等.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[J].郑州大学学报(工学版),2012,33(06):100-103.[doi:10.3969/j.issn.1671-6833.2012.06.024]
　CAO Junyan,GE Qingping,LI Jiaojiao.The Simultaneous Determination of 3 ,6-DCP and 3 ,4 ,$ ,6-TCP in ElectrochemicalSynthesis Reaction Liquid by High Pevformance Liquid Chromalography[J].Journal of Zhengzhou University (Engineering Science),2012,33(06):100-103.[doi:10.3969/j.issn.1671-6833.2012.06.024]
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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()
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《郑州大学学报(工学版)》[ISSN:1671-6833/CN:41-1339/T]

卷:
33
期数:
2012年06期
页码:
100-103
栏目:
出版日期:
2012-11-10

文章信息/Info

Title:
The Simultaneous Determination of 3 ,6-DCP and 3 ,4 ,$ ,6-TCP in ElectrochemicalSynthesis Reaction Liquid by High Pevformance Liquid Chromalography
作者:
曹军艳; 葛庆平; 李娇娇; 等.
郑州大学 化工能源学院,河南郑州,450001, 河南省产品质量监督检验院,河南郑州,450004
Author(s):
CAO Junyan; GE Qingping; LI Jiaojiao
1.School Chemical Engineering and Energy, Zhengzhou University, 2hengzhou 450001 , China;2. Henan Institute of Products Qaulity Supervision and Inspection,Zhengzhou 450004,China
关键词:
高效液相色谱;  电化学合成;  3;  6-二氯吡啶甲酸;  4;  5;  6-四氯吡啶甲酸
Keywords:
high performance liquid chromatography ; electrochemical gvnthes1s:6-dichloropicolinie aeid :3; 4; 5 ; 6-tetrachloropicolinie acid
分类号:
0657.7
DOI:
10.3969/j.issn.1671-6833.2012.06.024
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％.
Abstract:
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 electrochemieal synthesis reaction liquidby high performance liquid chromatography ( HPLC). The analysis was perfored on a Hypersi C18 columnwith a mixture of V( acetonitrile) : V( volume fraction of 19 acetic acid aqueous solution) = 15 :85 as the mo-bile phase at a flow rate of 1.0ml/min, The samples were detected at 280 nm with an UV detector and thecolumn temperature was 25℃, lt was found that 3 ,6-DCP and 3,4,5,6-TCP could be well separated underthe chromatographic conditions. The maximum relative standard deviations were 0. 58% and 0. 40%6 and thedetection limits were 2.01 x 10~’g/L and 5.09 x 10-’g/L for 3 ,6-DCP and 3 ,4,$ ,6-TCP. The recoveries forthem were 99.88%~100.5%and 99.89%~100.1%，respectively.

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