Abstract
To isolate oryzanol from the by-product of rice bran oil refinning, experiment of solvent fractional crystallization was carried out at various conditions with the dark oil obtained by acidifying the soap stock of micella refinning process and the pitch obtained from vacuum distillation of the dark oil. The impurity interfering the crystallization process such as waxes can be removed as precipitates by cooling the 1:1 mixtrue of acetone and dark oil to $0^{\circ}C$, From the dewaxed dark oil, oryzanol concentrate with 51.3% purity was obtained by fractional crystallization at$0^{\circ}C$ with the mixture of 8 part volume of hexane and 1 part of the dewaxed dark oil. The concentrate was recrystallized at room temperature with 20 part volume of methanol to yield oryzanol crystal of 98.3% purity. The optimum condition of vacuum distillation was temperature of $180^{\circ}C\;at\;0.2{\sim}0.4\;torr$ with 2% steam sparging. At this condition, the free fatty acid in the dark oil was removed as distillate without thermal deomposition to yield 82.3% of oryzanol as the pitch of 27.3% purity. After concentration from the pitch with 20 part volume of hexane to yield yellow powder of 75.4% purity, the yellow powder was recrystallized in methanol at room temperature to obtain the crystal containing 99.0% oryzanol. The overall oryzanol yield from the dark oil and the pitch was 9.5 and 28.5%, respectively. The change of the composition of sterols and triterpenoid alcohols in the compounds isolated during fractionation was analyzed by GC-MS.
미강유 정제 부산물로부터 오리자놀을 분리하기위해, dark oil과 dark oil의 증류잔류물인 pitch로부터 용매분리법 이용하여 오리자놀을 분리하였다. 분리과정 중 방해물질인 왁스분은 dark oil과 acetone을 1 : 1(w/v)로 혼합하여, $0^{\circ}C$에서 침전시켜 제거하였고, 여기에서 얻어진 dewaxed dark oil에 8 part의 hexane을 섞어 저온분리하여 오리자놀함량이 51.3%인 농축물을 얻었다. 이 농축물에 methanol 20 part를 가하고 재결성하여 98.3%의 오리자놀결정물을 얻었다. Dark oil로부터 pitch를 제조하는 적정조건은$180^{\circ}C$와 $0.2{\sim}0.4torr$의 진공상태에서 2%(w/w)의 steam을 가하는 증류조건이 오리자놀의 파괴를 최소화 하였다. 이로부터 얻어진 pitch의 오리자놀순도와 회수율은 27.3%와 82.3%였다. Pitch에 hexane을 가하고 저온분리하여 오리자놀순도가 75.4%인 오리자놀결정물을 얻었으며 이 농축물에 methanol을 가한 후 재결정하여 순도가 99%인 결정물을 얻었다. 이상과 같은 저온윤리법을 이용하였을 때 오리자놀의 회수율은 dark oil 9.5%, pitch 28.5%로 나타났다.