HPLC를 이용한 ketoprofen racemate의 분리

Ketoprofen racemate is very useful pharmaceutical intermediate, but the hardness of separation to each enantiomer is most a barrier to apply pharmaceutical industry. To overcome this difficulty, we would like to separate S-ketoprofen from ketoprofen racemate. To design suitable mobile phase, hexane and t-BME(tri-buthyl-methyle-ether) were used to elute peaks of ketoprofen racemate separately. When the ratio of hexane/t-BME/acetic acid was 60/40/0.1(%v/v), each component was separated successfully. In order to separate large amount of S-ketoprofen, sample concentration was increased from 100ppm to 2000ppm. In this case, resolution was decreased due to the overlapping of peaks(1.65${\rightarrow}$0.94).

Ketoprofen racemate를 각 enantiomer로 분리하고자 이동상의 조성을 변화하여 실험을 수행한 결과, hexane과 t-BME의 비가 60/40(%v/v)인 경우 적합한 체류시간과 분리도를 얻을 수 있었으며, 이동상의 acetic aicd를 0.1%(v/v) 첨가한 경우 낮은 pH에서 분리가 효율적으로 일어났다. 또한, 시료의 농도를 변화시켜 실험을 수행한 경우, 2000ppm까지는 선택도에 큰 변화없이 분리를 수행할 수 있었으나, 농도가 1000ppm 이상인 경우 분리도가 1.00미만으로 낮은 값을 보였다.