【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%。更多还原

【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.更多还原