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%。
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.
出处
《色谱》
CAS
CSCD
北大核心
2006年第6期578-580,共3页
Chinese Journal of Chromatography
关键词
制备型液相色谱
速度梯度洗脱
2-氯-5-三氯甲基吡啶
3-甲基吡啶
光氯化产物
preparative liquid chromatography
flow-rate gradient elution
2-chloro-5-trichloromethylpyridine
3-methylpyridine
photochemical chlorination product