CAJ | 학술논문

将超临界流体色谱技术应用于当归挥发油中Z-藁本内酯的提纯。采用ZorBax SB-C18色谱柱(250 mm×9.4 mm I.D.,5μm)，分别考察了改性剂、流速、压力、温度对色谱分离过程的影响，确定了较适宜的色谱提纯条件：CO2流速10 g×min-1，柱温313.15 K，柱压14 MPa；在此工艺条件下提纯制备Z-藁本内酯单体，得到的产品纯度为98.5％(wt)。研究了色谱过程的热力学规律，绘制色谱分离过程的 van’t Hoff 曲线，并由此得到了色谱相转移过程焓变为21.46 kJ×mol-1，并比较了 Z-藁本内酯与相邻组分从流动相到固定相分配过程中焓变和熵变的差值，在此条件下 Z-藁本内酯色谱分离过程为焓控过程。
장초림계류체색보기술응용우당귀휘발유중Z-고본내지적제순。채용ZorBax SB-C18색보주(250 mm×9.4 mm I.D.,5μm)，분별고찰료개성제、류속、압력、온도대색보분리과정적영향，학정료교괄의적색보제순조건：CO2류속10 g×min-1，주온313.15 K，주압14 MPa；재차공예조건하제순제비Z-고본내지단체，득도적산품순도위98.5％(wt)。연구료색보과정적열역학규률，회제색보분리과정적 van’t Hoff 곡선，병유차득도료색보상전이과정함변위21.46 kJ×mol-1，병비교료 Z-고본내지여상린조분종류동상도고정상분배과정중함변화적변적차치，재차조건하 Z-고본내지색보분리과정위함공과정。
Supercritical fluid chromatography (SFC) has received more and more attention in the area of pharmaceutical industry over the past few years. The application of supercritical fluid chromatography coupled with a UV detector to isolate Z-ligustilide from the roots of Angelica sinensis on C18 column was reported. The experimental conditions are temperature 305.15 ~323.15 K, pressure 10~19 MPa and flow rate of CO2 8~16 g×min-1, modifier concentration 0%~2%by mass, respectively. The effect of resolution of the modifier content in mobile phase, column temperature, column pressure, and flow rate of CO2 on the purification process was investigated through single-factor experiment. The optimum operation conditions found are temperature 313.15 K, pressure 14 MPa, and the CO2 flow rate 10 g×min-1, and under above conditions, Z-ligustilide concentration 98.5%by mass could be obtained. The thermodynamics of chromatographic process was studied. Using van’t Hoff plot, the enthalpy change of chromatographic phase transfer process is 21.46 kJ×mol-1. The process is enthalpically driven under experimental conditions.