食品与发酵工业

pH精制区带逆流色谱分离制备红曲中的酸式莫那可林K

  • 刘玉芹 ,
  • 郑振佳 ,
  • 杜金华 ,
  • 王岱杰 ,
  • 王晓 ,
  • 刘建华
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网络出版日期: 2011-11-25

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

  • Liu Yu-qin~ ,
  • Zheng Zhen-jia~ ,
  • Du Jin-hua~ ,
  • Wang Dai-jie~ ,
  • Wang Xiao~ ,
  • Liu Jian-hua~
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Online published: 2011-11-25

摘要

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。

本文引用格式

刘玉芹 , 郑振佳 , 杜金华 , 王岱杰 , 王晓 , 刘建华 . pH精制区带逆流色谱分离制备红曲中的酸式莫那可林K[J]. 食品与发酵工业, 2011 , 37(11) : 216 -219 . DOI: 10.13995/j.cnki.11-1802/ts.2011.11.025

Abstract

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 ? H2O 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.
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