OV-215毛细管色谱柱的研制及应用

Preparation and application of OV-215 capillary column

采用静态法研制了OV-215高效毛细管色谱柱。依次使用KOH水溶液、水、HCl溶液和水通过毛细管柱中,配制50 mg/mL三氟丙基三甲氧基硅烷和甲基三甲氧基硅烷(2:1,m/m)乙酸乙酯溶液进行表面去活,以改进固定液的湿润性。配制5 mg/mL的固定液通过加压装置通入毛细管中,以萘的每米理论塔板数评价毛细管柱的分离性能。结果发现:萘的每米理论塔板数为4033板数/m,交联度为90. 2%,耐温温度达到320℃,以N2为载气最佳线速度范围10~13 cm/s。用此毛细管柱分离了乙苯和二甲苯、硝基甲苯、氯化苄基氯等异构体。建立了制备OV-215毛细管柱的方法。

High performance OV-215 capillary column was prepared by static coating techniques. In order to improve the consistency of stationary phase deposition,the walls of fused-silica capillary chromatographic columns were pretreated by KOH,distilled water,HCl,distilled water and 5% 3,3,3-(trifluoropropyl) trimethoxysilane and methyl-trithoxysilicane(2: 1,m/m) ethyl acetate solution,respectively. Subsequently,the 0. 5% mixed stationary liquid was put into capillary chromatographic columns through pressurization device. The properties and separation performance of the prepared chromatographic columns could be demonstrated through the resolution of naphthalene with dichloromethane and the theoretical stage number for naphthalene. The results showed that the numbers of theoretical plate of capillary column with N2 were 4033 per meter,the supreme temperature was320℃ and line speed was 10-13 cm/s. On this column,ethyl-benzene and dimethylbenzene homologue isomers,nitrotoluene homologue isomers,dichlorotoluene homologue isomers were separated successfully. A rapid and simple preparation method of OV-215 capillary chromatographic column was developed.