Supercritical fluid extraction of quinolizidine alkaloids from Sophora flavescens Ait. and purification by high-speed counter-current chromatography

Supercritical fluid extraction of quinolizidine alkaloids from Sophora flavescens Ait. and purification by high-speed counter-current chromatography
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超临界流体萃取苦参中喹啉西啶生物碱。

DOI:
10.1016/j.chroma.2007.01.080
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发表时间:
2007-03-23
影响因子:
4.1
通讯作者:
Zhang, Chang Kai
Zhang, Chang Kai
中科院分区:
化学2区
文献类型:
--
作者:
Ling, Jian Ya;Zhang, Guo Ying;Zhang, Chang Kai

文献摘要

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采用超临界流体萃取法(SFE)提取苦参中喹诺嗪类生物碱。(Kushen)。通过L-9(3)(4)对压力、温度、CO2流量、改性剂用量进行正交试验,得到最佳工艺条件。在25 MPa、50℃、CO2流量(21/min)、改性剂用量(0.04 ml/min)的条件下,采用制备SFE体系,将该工艺放大30倍。采用氯仿-甲醇-2.3 × 10(-2) M NaH2PO4 (27.5:20:12.5, v/v)两相溶剂体系对粗提物进行高速逆流色谱(HSCCC)分离纯化,并对所得馏分进行高效液相色谱(HPLC)分析。得到3种喹诺嗪类生物碱,一步分离得到苦参碱10.02 mg、氧膦碱22.07 mg、氧化苦参碱79.93 mg,纯度分别为95.6%、95.8、99.6%。(c) 2007年Elsevier B.V.出版
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 CO2 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 CO2 (21/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 NaH2PO4 (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. (c) 2007 Published by Elsevier B.V.