氯甲苯同分异构体专用毛细管色谱柱的研制及应用

Preparation and application of capillary column for detection of chlorotoluene isomers

针对氯甲苯异构体体系,自制了有机皂土-34、M103液晶、全甲基-β-环糊精、2,3-二-O-乙酰基-6-O-叔丁基二甲基硅烷基-β-环糊精毛细管色谱柱。其中2,3-二-O-乙酰基-6-O-叔丁基二甲基硅烷基-β-环糊精对氯甲苯异构体的分离最好。对2,3-二-O-乙酰基-6-O-叔丁基二甲基硅烷基-β-环糊精毛细管色谱柱的制备和分析条件进行了优化,研制出适合分离分析氯甲苯异构体的专用毛细管色谱柱。色谱柱为0.25 mm×30 m×0.5μm,其中2,3-二-O-乙酰基-6-O-叔丁基二甲基硅烷基-β-环糊精占XE-60固定液的比例为25%,载气(N2)最佳线速度为14 cm/s,汽化和检测温度为200℃,柱温为125℃,分流比为200∶1,FID检测。

The self-made capillary gas chromatographic column prepared with 2,3-di-O-acetyl-6-O-tert-butyl-dimethylsilyl-β-cyclodextrin had the best selectivity towards chlorotoluene isomers compared with bentonite-34,M103 liquid crystal,and permethylated-β-cyclodextrin was used as stationary phases.With optimized preparation and analysis conditions,the 2,3-di-O-acetyl-6-O-tert-butyl-dimethylsiyl-β-cyclodextrin capillary chromatographic column was customized for the separation of chlorotoluene isomers.The size of chromatographic column was 0.25 mm×30 m×0.5 μm,with 2,3-di-O-acetyl-6-O-tert-butyl-dimethylsilyl-β-cyclodextrin accounted for 25%of XE-60 as stationary phase.The experimental conditions were as follows：the optimal nitrogen carrier gas velocity of 14 cm/s,the injection and detection temperature of 200 ℃,oven temperature of 125 ℃,split ratio of 200∶1,and FID detector.