Abstract
Diosgenin in an Indonesian Costus speciosus was determined by capillary gas-liquid chromatography (GLC). The experimental conditions for the hydrolysis, extraction and acetylation of the diosgenin, and the determination by GLC were investigated. 0.20g of dried sample powder was refluxed in the solution of 3N HCI and xylene at 95∼100${\circ}C$ for 4 hours and the xylene layer was separated. The residue evaporated the xylene was refluxed in 20 : 80 acetic anhydride-pyridine for 30 minutes and the diosgenin acetate was extracted with diethyl ether. Dehydrated with anhydrous $Na_2SO_4$ and evaporated the ether, the residue was dissolved in 5.00ml of n-hexane and injected into GLC. Capillary column of SE-30 25m ${\times}$ 0. 33mm was installed in GLC and the column temperature was increased from 180${\circ}$ to 270${\circ}C$ at rate of 10${\circ}C$/min. The flow rate of carrier gas $N_2$ was 2ml/min and FID was used to detect. The analytical result of the diosgenin was 0.281% and relative standard deviation of 5 measures was 1.8%.
모세관 기체-액체프로마토그래피(GLC)에 의해 인도네시아산 Costus speciosus중의 diosgenin을 정량하기 위해 가수분해 및 추출, 아세틸화 반응 및 GLC의 측정 조건등을 검토하였다. 건조된 diosgenin분말 1.20g을 3N HCI과 xylene의 혼합용액으로 95∼100${\circ}C$에서 4시간 환류시킨 다음 xylene층을 분리하였다. Xylene을 증발시켜 날려보내고 20:80의 acetic anhydride-pyridine을 가하고 30분간 환류시켜 아세틸화시킨 후 diethyl ether로 추출하였다. 무수 $Na_2SO_4$로 탈수시키고 ether를 날려 보낸 다음 찌끼를 n-hexane 5.00ml에 녹여 GLC로 분석하였다. SE-30 25m ${\times}$ 0. 33mm의 모세관을 사용하였고 컬럼온도는 180${\circ}$에서 270${\circ}C$까지 10${\circ}C$/min의 속도로 온도를 상승시켰다. 운반기체 $N_2$의 유속은 2ml/min이었고 FID로 검출하였다. Diosgenin의 분석결과는 0.281%이었고, 상대표준편차는 1.8%로서 재현성이 좋았다.