Ling Jian Ya, Zhang Guo Ying, Cui Zhao Jie, Zhang Chang Kai
State Key Laboratory of Microbial Technology, Shandong University, Jinan 250100, China.
J Chromatogr A. 2007 Mar 23;1145(1-2):123-7. doi: 10.1016/j.chroma.2007.01.080. Epub 2007 Jan 27.
Supercritical fluid extraction (SFE) was used to extract quinolizidine alkaloids from Sophora flavescens Ait. (Kushen). An orthogonal test L(9)(3)(4) including pressure, temperature, flow rate of CO(2) and the amount of modifier was performed to get the optimal conditions. The process was then scaled up by 30 times with a preparative SFE system under 25 MPa, 50 degrees C and a flow rate of CO(2) (2l/min) and the amount of modifier (0.04 ml/min). The crude extracts were separated and purified by high-speed counter-current chromatography (HSCCC) with a two-phase solvent system composed of chloroform-methanol-2.3 x 10(-2)M NaH(2)PO(4) (27.5:20:12.5, v/v), and the collected fractions were analyzed by high-performance liquid chromatography (HPLC). Three kinds of quinolizidine alkaloids were obtained, yielding 10.02 mg of matrine, 22.07 mg of oxysophocarpine and 79.93 mg of oxymatrine with purities of 95.6, 95.8, 99.6% in one-step separation, respectively.
采用超临界流体萃取（SFE）法从苦参中提取喹诺里西啶生物碱。进行了包括压力、温度、二氧化碳流速和改性剂用量的正交试验L(9)(3)(4)以获得最佳条件。然后在25MPa、50℃、二氧化碳流速为2l/min和改性剂用量为0.04ml/min的条件下，使用制备型SFE系统将该工艺放大30倍。粗提物通过高速逆流色谱（HSCCC）进行分离纯化，所用两相溶剂系统为氯仿 - 甲醇 - 2.3×10(-2)M NaH(2)PO(4)（27.5:20:12.5，v/v），收集的馏分通过高效液相色谱（HPLC）进行分析。得到了三种喹诺里西啶生物碱，一步分离得到的氧化苦参碱、氧化槐果碱和苦参碱的产量分别为10.02mg、22.07mg和79.93mg，纯度分别为95.6%、95.8%和99.6%。
