The Synthesis Of Polymer Bonded With β-cylodextrin And The Chiral Separation Of Ibuprofen

Firstly we prepared1-5μm styrene seed by radical polymerization, then prepared15μm macroporous styrene-divinylbenzene resin by using the two-step seed swelling method. Then we took macroporous styrenedivinylbenzene resin as a skeleton to synthetize the nitro resin with the using of mixed acid of concentrated nitric acid/concentrated sulfuric acid. On the other side we obtained the optimum nitration conditions:65%concentrated nitric acid/85%concentrated sulfuric acid (2/5, volume ratio), reaction temperature50°C, the reaction time5hours. We used the tindichloride as the reductant to change the nitro group to the amino group with hydrochloric acid/ethanol as the reaction medium. Finally, using the amino group as the reactive group and glutaraldehyde as a linking agent, we bonded the P-cyclodextrin to the styrene-divinylbenzene resin. After the study of reaction time, the concentration of hydrochloric acid and the quantity of P-cyclodextrin, we optimized the reaction conditions. The optimum reaction conditions were:80°C;1mol/1hydrochloric acid solution; P-cyclodextrin/macroporous resin=4(m/m). The stainless steel column parameters was250mm×4.6mm and we packed the column under25Mpa and with the95%ethanol as a solvent.Finally, we choose the racemic drug ibuprofen as the object of chiral separation in high-performance liquid chromatography, and at the same time we optimized the separation parameters. Optimized separation parameters:the composition of mobile phase:methanol: acetic acid triethylamine solution(pH=4.5,0.2%)=30:70(v/v); flow rate was1ml/min; column temperature=30℃.The separation degree Rs was1.5or more, and the baseline was completely separated.