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

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

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100μL。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%。

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.