pH精制区带逆流色谱分离制备红曲中的酸式莫那可林K

Preparative Separation Monacolin K Acid Form from Red Yeast Rice by pH-zone-refining Counter-current Chromatography

建立了pH精制区带逆流色谱分离制备红曲中功能成分酸式莫那可林K的新方法。首先用体积分数95%乙醇提取红曲中的莫纳可林K,然后经过碱化处理使内酯式莫那可林K转化为酸式,最后采用溶剂系统V（石油醚）：V（乙酸乙酯）：V（甲醇）：V（水）=5：5：4：6,上相添加HCl（10mmol/L）作为固定相,下相添加氨水（10mmol/L）为流动相进行pH精制区带逆流色谱分离。分离所得的酸式莫那可林K经HPLC检测纯度,并用UV,ESI-MS和~1H-NMR鉴定其化学结构。从2.0g粗提物一次分离得到纯度为93.4%的酸式莫那可林K147mg。

An efficient method was developed for the separation and purification of monacolin K acid from the crude extract of red yeast rice by pH-zone-refining counter-current chromatography（pH-ZRCCC）.Monacolin K was first extracted from red yeast rice by 95%ethanol,then it was transformed from lactone to acid form by alkalization method and separated by pH-ZRCCC with the two-phase solvent system composed of petroleum ether/ethyl acetate/ methanol/water（5：5：4：6,V/V）,10 mmol/L HCl in organic phase used as the stationary phase and 10 mmol/L NH_3 ？ H_2O in aqueous phase used as the stationary phase.The purity of monacolin K acid form from separation fraction was analyzed by HPLC and identified by UV,ESI-MS and ^1H-NMR.From 2.0 g of crude extract,147 mg of monacolin K acid form was obtained at 93.4%purity in one-step separation.