• Title/Summary/Keyword: 크로마토그래픽 인자

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A Study on the New Development for Determination of Dead Time in GC-OTC/FID (GC-OTC/FID에서 Dead Time 결정을 위한 새로운 방법 개발에 대한 연구)

  • Oh, Doe Seok;Kim, Sung Wha;Ko, Eun Ah;Jeon, Hyung Woo
    • Journal of the Korean Chemical Society
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    • v.63 no.4
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    • pp.246-252
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    • 2019
  • In the system of GC-OTC/FID (Gas chromatography-Open Tubular Column/Flame Ionization Detector), DMSO (Dimethyl sulfide) solvent was used to separate the polar solvents (Alcohols). In this system DMSO was eluted later than the separated polar solvents. At this system to calculate chromatographic factors [adjusted retention time ($t_R^{\prime}=t_R-t_O$), capacity factor{$k^{\prime}=(t_R-t_O)/t_O$} and separation factor {${\alpha}=(t_{R2}-t_O)/(t_{R1}-t_O)$}], dead time($t_O$) is necessary, but the method to calculate it has not been reported yet. Therefore, we have tried to develop $t_O$. To calculate $t_O$, we conversed DMSO retention time (DMSO $t_R$) to logarithm ($f(x)={\log}\;t_{R(DMSO)}{\rightarrow}t_O$, $t_O={\log}$ 9.551=0.980). To confirm the optimization of the developed method, we compared with $CH_4\;t_R$ and ${\ln}\;t_{R(DMSO)}$. Both of the values calculated by $CH_4\;t_R$ and ${\ln}\;t_{R(DMSO)}$ were not suitable in the calculation k' and ${\alpha}$. The developed method in this study{${\log}\;t_{R(DMSO)}$} has satisfied both of the values k' criteria (1${\alpha}(1<{\alpha}<2)$. The developed calculation method in this study was easy and convenient, therefore it can be expected to be applied to these similar systems.

Primary study of sterols composition of Rhodiola sachalinensis by using GC/MS (GC/MS를 이용한 고산 홍경천의 스테롤 구성에 대한 초기연구)

  • Jin, Yinzhe;Li, Xifeng;Li, Donghao;Row, Kyung Ho
    • Analytical Science and Technology
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    • v.22 no.3
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    • pp.219-227
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    • 2009
  • 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%).