UV-VIS 분광기기 밸리데이션 및 아미노산유도체 이성질체의 광학분할 연구

Abstract

For the increasing demand for the validation of analytical results, one of the important concerns of the analyst is to be assured that the instrumentation is working to qualified conditions. In this study, several validation guidelines of the performance verification of UV-VIS spectrophotometer used in pharmacopoeias of major countries and UV-VIS instrument analytical companies were investigated and compared. And the practically useful validation guidelines of UV-VIS spectrophotometer were proposed. Based on our proposed validation guidelines of UV-VIS spectrophotometer, several UV-VIS spectrophotometers used in drug manufacturing laboratories were validated for their performances. The liquid chromatographic enantiomer separation of N-fluorenylmethoxycarbonyl (FMOC) protected α-amino acids was performed on nine polysaccharide-derived chiral stationary phases (CSPs). Among all CSPs, in general, the cellulose derived coated CSPs, Chiralcel OD-H and Chiralcel OD showed the greatest performance for resolution of N-FMOC α-amino acids and, therefore, all analytes enantiomers were base-line separated on Chiralcel OD-H or Chiralcel OD. It was observed that the coated type CSPs (Chiralpak AD and Chiralcel OD-H or Chiralcel OD) show generally higher enantioseparation for these analytes than the covalently bonded type CSPs (Chiralpak IA and Chiralpak IB) with the same chiral selector, respectively. Also it was shown that the covalently bonded CSP, Chiralpak IB has the advantage of the use of a broad range of solvents over the coated type CSPs.