Preparation And Application Of Stearyl Methacrylate Micro-monolithic Column For Capillary Liquid Chromatography

Capillary liquid chromatography (CLC) commonly uses the columns of 0.10 -1.00 mm inter diameter, thus leading to the advantages including simple operation, low mobile phase and sample consumption, little pollution of environment and easy combination with other dectection devices.Seperation column plays an important part in chromatography. ODS packed columns can finish 80% of chromatographic analysis task, which is generally used in CLC presently. However, ODS packed columns suffers from the shortcomings such as friting, complicated preparation and the high-pressure. In this thesis, A capillary monolithic column was prepared by in-situ free radical polymerization of stearyl methacrylate (SMA) with ethylene glycol dimethacrylate (EDMA) in the presence of the initiator AIBN and a mixture of porogens including iso-amyl alcohol and 1,4-butanediol. This capillary monolithic column has the C18 alkyl chains same as the moieties on ODS, and thus has the good features including high-efficiency, high-resolution and good compatibility to mass spectrometry. Additionally, SMA monolithic stationary phase has the unique advantages such as simple preparation, no needs for frits, good permeability, a wide range of using pH and rapid separation.Reasonable retention times and general selectivity can be obtained by varying the composition and thus adjusting the polarity of mobile phase. In this thesis, four benzenes, threel anilines and five ketones were baseline separated respectively on identical column in 15 min after optimizing several separation conditions. The SMA monolithic column was furtherly applied to quantitative analysis of the ofloxacin and chloramphenicol in eye drops and the chlorogenicacid in Oral Liquid. The quantitative methods were evaluated in terms of linear range, precision, detection limit and recovery.In the present work, a conventional detector of HPLC was used. But the volume of flow cell is too large to be applied in CLC. In order to reslove this problem, a home- made flow cell was used instead of the one with conventional detector..