고산 홍경천에 포함된 스테로이드 화합물의 구성을 흡착 컬럼 크로마토그래픽 정제와 GC/MS를 이용하여 측정하였다. 스테롤은 에탄올과 디클로로메탄을 각각 초음파와 Soxhlet의 용매로 사용하여 추출하였다. 추출물은 클로로포름과 물로 액-액 추출을 수행하여 분배하였으며, 실리카 컬럼으로 정제하였으며, BSTFA를 사용하여 silyl유도 반응을 수행하였다. GC/MS를 이용하여 고산 홍경천에서 $\beta$-sitosterol, stigmasterol과 cycloartenol을 포함한 18가지 자유 스테롤과 9가지 포합체 스테롤을 검출할 수 있었다. 그중에서 cholest-5-ene-3-ol, cholesterol, stigmasterol, $\beta$-sitosterol은 스테롤 표준품으로 확인하고 정량분석을 수행하였다. 대부분의 스테롤은 클로로포름 분액에서 검출되었고, $C_{29}$는 여러 그룹 중에서 가장 많은 그룹이었다. $\beta$-sitosterol은 가장 많이 함유된 성분이며 상대함량은 45.94%이고, 차례로 ergost-7-ene-3-ol (11.33%), 4,14-dimethyl-ergosta-8,24(28)-diene-3-ol (7.07%), stigmasterol (6.09%), cycloartenol (5.43%)과 4-methyl-cholest-5-ene-3-ol (5.39%)이었다.
고산 홍경천에 포함된 스테로이드 화합물의 구성을 흡착 컬럼 크로마토그래픽 정제와 GC/MS를 이용하여 측정하였다. 스테롤은 에탄올과 디클로로메탄을 각각 초음파와 Soxhlet의 용매로 사용하여 추출하였다. 추출물은 클로로포름과 물로 액-액 추출을 수행하여 분배하였으며, 실리카 컬럼으로 정제하였으며, BSTFA를 사용하여 silyl유도 반응을 수행하였다. GC/MS를 이용하여 고산 홍경천에서 $\beta$-sitosterol, stigmasterol과 cycloartenol을 포함한 18가지 자유 스테롤과 9가지 포합체 스테롤을 검출할 수 있었다. 그중에서 cholest-5-ene-3-ol, cholesterol, stigmasterol, $\beta$-sitosterol은 스테롤 표준품으로 확인하고 정량분석을 수행하였다. 대부분의 스테롤은 클로로포름 분액에서 검출되었고, $C_{29}$는 여러 그룹 중에서 가장 많은 그룹이었다. $\beta$-sitosterol은 가장 많이 함유된 성분이며 상대함량은 45.94%이고, 차례로 ergost-7-ene-3-ol (11.33%), 4,14-dimethyl-ergosta-8,24(28)-diene-3-ol (7.07%), stigmasterol (6.09%), cycloartenol (5.43%)과 4-methyl-cholest-5-ene-3-ol (5.39%)이었다.
The steroid compounds in Rhodiola sachalinensis were determined with adsorption column chromatographic purification and GC/MS. Sterols were extracted by sonication and Soxhlet with ethanol and dichloromethane, respectively. The extract was partitioned with chloroform and water using liquid-liquid ex...
The steroid compounds in Rhodiola sachalinensis were determined with adsorption column chromatographic purification and GC/MS. Sterols were extracted by sonication and Soxhlet with ethanol and dichloromethane, respectively. The extract was partitioned with chloroform and water using liquid-liquid extraction, and purified with a silica column after the sterols had been converted to the corresponding silyl derivatives with BSTFA. Eighteen free sterols, including $\beta$-sitosterol, stigmasterol and cycloartenol, and nine sterol conjugates were found from Rhodiola sachalinensis by GC/MS. Among them, cholest-5-ene-3-ol, cholesterol, stigmasterol, $\beta$-sitosterol were confirmed and quantified with sterol standards. Most sterols were presented in the chloroform part, with $C_{29}$ being the most abundant group in this sterol group. $\beta$-sitosterol was the most abundant compound with a relative content of 45.94% followed by ergost-7-ene-3-ol (11.33%), 4,14-dimethyl-ergosta-8,24(28)-diene-3-ol (7.07%), stigmasterol (6.09%), cycloartenol (5.43%) and 4-methyl-cholest-5-ene-3-ol (5.39%).
The steroid compounds in Rhodiola sachalinensis were determined with adsorption column chromatographic purification and GC/MS. Sterols were extracted by sonication and Soxhlet with ethanol and dichloromethane, respectively. The extract was partitioned with chloroform and water using liquid-liquid extraction, and purified with a silica column after the sterols had been converted to the corresponding silyl derivatives with BSTFA. Eighteen free sterols, including $\beta$-sitosterol, stigmasterol and cycloartenol, and nine sterol conjugates were found from Rhodiola sachalinensis by GC/MS. Among them, cholest-5-ene-3-ol, cholesterol, stigmasterol, $\beta$-sitosterol were confirmed and quantified with sterol standards. Most sterols were presented in the chloroform part, with $C_{29}$ being the most abundant group in this sterol group. $\beta$-sitosterol was the most abundant compound with a relative content of 45.94% followed by ergost-7-ene-3-ol (11.33%), 4,14-dimethyl-ergosta-8,24(28)-diene-3-ol (7.07%), stigmasterol (6.09%), cycloartenol (5.43%) and 4-methyl-cholest-5-ene-3-ol (5.39%).
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제안 방법
In order to confirm the sterols determined, sterol standard mixture sample GC-MS analysis and Soxhlet extraction were carried out. And the results were cmipared with those obtained from above e冲eriments.
In this study, sterols in Rhodiola sachalinensis were extracted by sonication and Soxhlet, isolated by column chromatography, and then identified by GC/MS after they were converted into corresponding silyl derivatives.
The GC-MS conditions were same with those in analysis of extract samples. Under six replicate experiments including four standards and three extract samples, the relative standard deviations (RSD, %) of retention times were 2.3, 4.5, 2.5 and 2.2% for cholest-5-ene-3-ol, cholesterol, stigmasterol, p-sitosterol, respectively. And the same mass spectra profiles of sterol silyl derivatives were obtained for each corresponding standards.
대상 데이터
Eighteen free sterols (Table 1) were identified by GC/MS after the purification procedure. The total ion currents of these sterols are shown in Fig.
Anhydrous sodium sulfate and all glassware were burned at 400 ℃ for 12 hr and washed with solvent before use. Silica gel (75-150 jim) was purchased from Qingdao Hailong dried silica-gel factory (Shandong, China).
The Rhodiola sachalinensis samples used in this study were collected from the Yanji Food and Drug Administration, Jilin province, China in July of 2007. jV, O-bis (trimethylsilyl) trifluoroacetamide (BSTFA: 99% in 1% TMCS) was purchased from Chem Service (USA).
참고문헌 (23)
G. Zhou, Y. Guan, H. Chen and J. Ye, J. Chromatogr. A., 1142, 236-239(2007)
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