制备型液相色谱法分离纯化3-甲基吡啶光氯化产物中的2-氯-5-三氯甲基吡啶

色谱

制备型液相色谱法分离纯化3-甲基吡啶光氯化产物中的2-氯-5-三氯甲基吡啶

苏莉1,张勇2,黄可明3

1.Southwest University of Science and Technology, Mianyang 621010, China; 2.Institute of Chemical Materials, China Academy of Engineering Physics, Mianyang 621001, China;3.The Group Company of Lier Chemistry, Mianyang 621010, China

收稿日期:2006-01-05 修回日期:2006-04-19 出版日期:2006-11-30 发布日期:1986-06-25
通讯作者: 苏莉

Separation and Purification of 2-Chloro-5-Trichloromethylpyridine from Products of Photochemical Chlorination of 3-Methylpyridine Using Preparative Liquid Chromatography

SU Li1, ZHANG Yong2, HUANG Keming3

1.Southwest University of Science and Technology, Mianyang 621010, China; 2.Institute of Chemical Materials, China Academy of Engineering Physics, Mianyang 621001, China;3.The Group Company of Lier Chemistry, Mianyang 621010, China

Received:2006-01-05 Revised:2006-04-19 Online:2006-11-30 Published:1986-06-25
Contact: SU Li

摘要/Abstract

摘要： 利用制备型高效液相色谱从3-甲基吡啶光氯化产物中分离纯化得到2-氯-5-三氯甲基吡啶,对制备色谱的洗脱方式、洗脱剂组成及浓度、进样量等参数进行了优化。使用的制备柱为Zorbax-C18柱,以乙腈-水为流动相，采用速度梯度洗脱方式进行洗脱,用二极管阵列检测器在240 nm波长下检测，进样体积为100 μL。该方法的制备回收率为82.7%,相对标准偏差为4.0%（n=5）,产品纯度为99.01%。

关键词: 2-氯-5-三氯甲基吡啶, 3-甲基吡啶, 光氯化产物 , 速度梯度洗脱, 制备型液相色谱

Abstract: A preparative high performance liquid chromatographic technique was used to separate and purify 2-chloro-5-trichloromethylpyridine from the products of photochemical chlorination with 3-methylpyridine as raw material. The elution mode, the flow rate of the mobile phase and injection volume were optimized. The optimum operation parameters were selected as follows: Zorbox-C18 reversed-phase column with the flow rate gradient elution of 30% acetonitrile in water as the mobile phase (gradient elution program: 0-8 min at 4 mL/min, 8-14 min at 10 mL/min), and a diode array detector with wavelength set at 240 nm, injecting volume of 100 μL. The average recovery rate was 82.7% and relative standard deviation (RSD) was 4.0%（n=5）. High purity (99.01%) product was obtained. The effective and accurate method has been successfully applied to the preparation of pure 2-chloro-5-trichloromethylpyridine.

Key words: 2-chloro-5-trichloromethylpyridine, 3-methylpyridine, flow-rate gradient elution, photochemical chlorination product , preparative liquid chromatography

苏莉,张勇,黄可明. 制备型液相色谱法分离纯化3-甲基吡啶光氯化产物中的2-氯-5-三氯甲基吡啶[J]. 色谱.

SU Li, ZHANG Yong, HUANG Keming. Separation and Purification of 2-Chloro-5-Trichloromethylpyridine from Products of Photochemical Chlorination of 3-Methylpyridine Using Preparative Liquid Chromatography[J]. Chinese Journal of Chromatography.