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3-溴噻吩烷基化系列反应中原料、产物及副产物的高效液相色谱实时分离检测

祁争健,冯卫东,孙岳明   

  • 收稿日期:2007-01-26 修回日期:2007-04-24 出版日期:2007-09-30 发布日期:1985-03-25
  • 通讯作者: 祁争健

In Situ Separation and Determination of Raw Material, Product and By-products during A Series of Reactions of Alkylated 3-Bromthiophene with High Performance Liquid Chromatography

  • Received:2007-01-26 Revised:2007-04-24 Online:2007-09-30 Published:1985-03-25

摘要:

建立了一种采用反相高效液相色谱(RP-HPLC)实时检测5种 3-烷基取代噻吩合成反

应中 3-烷基(丁基、己基、辛基、异辛基、十二烷基)噻吩、原料 3-溴噻吩及副产物含

量变化的方法。试样经水洗、萃取及旋转蒸发浓缩等预处理后,采用RP-HPLC二极管阵列

紫外检测法测定,外标法定量,实现了反应产物(3-烷基噻吩)与原料(3-溴噻吩)及副产

物组分的完全分离,互不干扰。5种烷基化产物及 3-溴噻吩在0.100~10.0 mg/L 范围内

线性良好,方法的最低检出限为20.0 μg/L (S/N=3)。该方法简便,快捷,准确,既可用于

测定反应产物的含量,又可用于跟踪反应过程中反应原料、反应生成物的动态变化,为反

应动力学的研究提供了可靠依据。

于跟踪反应过程中反应原料、反应生成物的动态变化,为反应动力学的研究提供可靠依据。

关键词: 3-烷基取代噻吩(3-alkylthiophene), 3-溴噻吩(3-bro mothiophene) , 高效液相色谱法(HPLC)

Abstract: A novel method to determine in situ the changes in constituents of 3-bromthiophene, 3-alkylthiophenes (3-butylthiophene, 3-hexylthiophene, 3-octylthiophene, 3-isooctylthiophene, 3-dodecylthiophene) and by-products during the alkylated reactions was developed using a reversed-phase high performance liquid chromatography. After washed with water, extracted and flash distillation, 3-alkyl thiophenes were analyzed by RP-HPLC-photo diode array detector and quantified by external standard method under the critically examined chromatographic conditions. 3-Alkyl thiophene could be completely separated from 3-bromthiophene and other by-products without interference from each other. All the linear ranges of five 3-alkyl thiophenes and 3-bromthiophene were 0.100-10.0 mg/L with the correlation coefficients of 0.9952-0.9993 and the limits of detection of 20.0 g/kg (S/N=3). The average recoveries and relative standard deviations(RSD)were in the ranges from 89.2% to 102.6% and 1.04% to 4.98%, respectively. The results indicated that the proposed method was easy, fast, accurate, and could meet the requirement for determination of 3-alkylthiophenes and be applied for tracing the changes of raw material and products during preparation, which might in situ provide available information for reaction kinetics research.