α位双取代氯甲基萘同分异构体的分离和检测

Separation and Detection of Dichloromethyl Naphthalene Isomers in α Position

目的建立1-氯甲基萘中1, 4-二氯甲基萘和1, 5-二氯甲基萘两个同分异构体分离和检测方法。方法采用以硅胶表面涂敷纤维素-三(4-甲基苯甲酸酯)为填料的CHIRALCEL?OJ-RH色谱柱(4.6 mm×150 mm,5μm);流动相甲醇-水溶液(83:17),流速1.0 ml/min;紫外检测波长285 nm。结果 1, 4-二氯甲基萘和1, 5-二氯甲基萘可被有效分离,且对应的线性范围内,线性相关系数分别为1.0000,1.0000;检测限分别为0.922,1.506μg/ml;平均回收率分别为95.34%,101.74%,RSD分别为1.4%,1.3%。结论本法可用于1-氯甲基萘中1, 4-二氯甲基萘和1, 5-二甲基萘的分离检测。

Objective To establish a method for the separation and detection of two isomers of 1, 4-dichloromethylnaphthalene and 1, 5-dimethylnaphthalene in 1-chloromethylnaphthalene. Methods A chromatographic column(CHIRALCEL;OJ-RH, 4.6 mm×150 mm, 5 μm) coated with cellulose-tris(4-methylbenzoate) on the surface of silica gel as the filler. Methanol-water solution(83:17) at the flow rate of 1.0 ml/min was used as mobile phase and UV detection wavelength was set at 285 nm. Results 1, 4-dichloromethylnaphthalene and 1, 5-dimethylnaphthalene were separated effectively. The linear correlation coefficients were 1.0000 and 1.0000 respectively within the corresponding linear range;the detection limits were 0.922 μg/ml and 1.506 μg/ml, the average recoveries were 95.34 % and 101.74 %, the relative standard deviations were 1.4 % and 1.3 %, respectively. Conclusion The method can be used for the separation and detection of 1, 4-dichloromethylnaphthalene and 1, 5-dimethylnaphthalene in 1-chloromethylnaphthalene.