Preparation Of Cellulose Derivatives Stationary Phase And Applications To Chromatographic Separation

The Dissertation consists of four chapters.In chapter one, a review is presented about advances of chromatographic separation of optical isomers of chiral compounds and developments of cellulose-based chiral stationary phases (CSPs) for the direct separation of enantioners in high-performance liquid chromatography (HPLC).In Chapter two, Cellulose derivatives were synthesized by homogeneous reaction of phenyl isocyanate or toluoyl chloride with microcrystalline cellulose in pyridine and triethylamine at about 110癈. 4-N,N-dimethylaminopyridine was used as hypernucleophilic acylation catatlyst. Elemental analysis and IR indicated that almost all hydroxy groups of the microcrystalline cellulose were converted into esters moieties.In chapter three, Silica gel (mean partical, Sum; mean pore diameter, 100 nm; specific surface, 210 m2/g) was treated a large excess of (3-aminopropyl)- triethoxysilane at refluxing temperation in toluene. The silanized gel was coated with about 16% of cellulose tris(4-methylbenzoate). And, the material was packed into a stainless-steel column(250 mm X 4.6mm I.D.) at 300 kg/cm2 by a slurry method. Optical isomers of chiral compounds! were separated on the cellulose tris(4-methylbenzoate) (MCTB). The experimental results showed as the following.1. The iptio isomers of naproanilide could be separated on MCTB chiral column and ethanol using as mobile phase at the flow 0.5mL/min .Its capacity factors were 1.54 and 2.21 respectively, the separation factor was 1.43 and the separation factor was 1.20.2. The option isomers of methyl 2-(4-(2,4-dichlorophenoxy) phenoxy)-propionate could be separated on MCTB chiral column and ethanol using as mobile phase at the flow 0.3 mL/min. Its capacity factors were 2.90 and 3.45, respectively. The separation factor was 1.19 and the separation factor was 1.21.3. The resolution of ethyl ester of buprofen enantiomers has been achieved by MCTB chiral column and a mixture solution of methanol and water (85/15, V/V) uses asmobile phase at the flow 0.4mL/min. Its capacity factors were 3.08 and 3.97, respectively. The separation factor was 1.29 and the separation factor was 1.24. 4. Separation of enantiomers 2-(4-hydoxyphenoxy) propionates could be separated on MCTB chiral column and a mixture solution of methanol and water (75/25, V/V) as mobile phase at the flow 0.5mL/min. Its capacity factors were 2.69 and 3.99, respectively. The separation factor was 1.48 the separation factor was 1.90. In Chapter four, the cellulose derivatives were supported on GDX-103. The adsorption capabilities of MCTB /GDX-103, CTPC/ GDX-103 and GDX-103 as gas chromatographic stationary phases were characterized by a variety of probe molecules. And some materials such as aliphatic alcohols and esters with low boiling points were separated on these stationary phases.