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Supercritical fluid extraction of cordycepin and adenosine from Cordyceps kyushuensis and purification by high-speed counter-current chromatography

机译:九州冬虫夏草中虫草素和腺苷的超临界萃取及高速逆流色谱纯化

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摘要

Supercritical fluid extraction (SFE) was used to extract cordycepin and adenosine from Cordyceps kyushuensis. An orthogonal array design (OAD) test, L9(3)~4, including pressure, temperature, the mount of modifier and the flow rate of CO2 was performed to get the optimal conditions. The process was then scaled up by 30 times with a preparative SFE system under 40 MPa, 40℃, the mount of modifier (0.04 ml min~(-1)) and a flow rate of CO2 (2.01 min~(-1)). The preparative SFE extracts were separated and purified by highspeed counter-current chromatography (HSCCC) with a selected two-phase solvent system composed of ethyl acetate-n-butyl alcohol-water at an optimized volume ratio of 1:4:5, and the collected fractions were analyzed by high-performance liquid chromatography (HPLC). Two nucleosides were obtained and yielded 8.92 mg of cordycepin, 5.94 mg of adenosine with purities of 98.5 and 99.2% from 400 mg SFE crude extraction, in one-step separation, respectively.
机译:用超临界流体萃取(SFE)从九州冬虫夏草中提取虫草素和腺苷。进行了包括压力,温度,改性剂用量和CO2流量在内的正交阵列设计(OAD)测试,L9(3)〜4以获得最佳条件。然后使用制备型SFE系统在40 MPa,40℃,改性剂用量(0.04 ml min〜(-1))和CO2流速(2.01 min〜(-1))下将工艺放大30倍。 。制备的SFE提取物通过高速逆流色谱(HSCCC)分离和纯化,选择的两相溶剂体系由乙酸乙酯-正丁醇-水组成,优化的体积比为1:4:5,通过高效液相色谱法(HPLC)分析收集的级分。从400 mg SFE粗提物中,一步分离得到两个核苷,分别得到8.92 mg虫草素,5.94 mg腺苷,纯度分别为98.5和99.2%。

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