高效液相色谱分析法测定2-氯-5-三氯甲基吡啶及其类似化合物
HPLC DETERMINATION OF 2-CHLORO-5-TRICHLOROMETHYLPYRIDINE AND ANALOGOUS COMPOUNDS
摘 要
采用高效液相色谱法对高效除草剂盖草能的中间体2-氯-5-三氯甲基吡啶(TCMP)及相关化合物的分析条件进行了探讨和优化.使用Zorbax eclipse XDB-C18色谱柱,以乙腈-水(30+70,体积比)为流动相,控制流速1 mL·min-1,采用紫外可变波长检测器,检测波长为240 nm,方法的线性关系良好,相关系数为0.998 4,回收率为99.05%.在实样分析中同时测定了合成TCMP过程中的两个主要副产物2-氯-5-氯甲基吡啶和2-氯-3-三氯甲基吡啶.
2-氯-5-三氯甲基吡啶
盖草能
HPLC
2-Chloro-5-trichloromethylpyridine
Haloxy-fop-methyl
Abstract
HPLC was applied to the determination of 2-chloro-5-trichloromethylpyridine (TCMP),an important intermediate for the synthesis of the weedicide haloxy-fop-methyl.The conditions of the method were studied in detail,and the optimum conditions found were as follws.Zorbax eclipse XDB-C18 was used as RP-chromatographic column,a mixed solution of acetonitrile and water in the proportion of 30 to 70 was used as mobile phase,flow-rate of the mobile phase was 1 mL·min-1.UV-detection at 240 nm was adopted in the measurement.Linear relationship between the peak area and concentration of TCMP was obtained in the range of 0.004 to 0.020 mg·L-1 (r=0.998 4).Recovery test was performed and a result of average recovery of 99.05% was obtained.In the analysis of some substantial samples,TCMP was determined by this method together with two main by-products,ECMP and CCMP obtained simultaneously in the synthesis of TCMP.
中图分类号 O657
所属栏目 试验与研究
基金项目
收稿日期 2005/12/13
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备注苏莉(1972-),女,四川蓬溪县人,讲师,主要从事有机合成及分析的教学与研究工作.
引用该论文: SU Li. HPLC DETERMINATION OF 2-CHLORO-5-TRICHLOROMETHYLPYRIDINE AND ANALOGOUS COMPOUNDS[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2006, 42(10): 793～795
苏莉. 高效液相色谱分析法测定2-氯-5-三氯甲基吡啶及其类似化合物[J]. 理化检验－化学分册, 2006, 42(10): 793～795
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参考文献
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【7】孙京国,姚国伟.红霉素肟及相关化合物的高效液相色谱分析[J].分析化学,2003,31(9):1089-1092．
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