Shandong Analysis and Test Center, Shandong Academy of Sciences, 19 Keyuan Street, Jinan, Shandong 250014, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2010 Oct 15;878(28):2881-5. doi: 10.1016/j.jchromb.2010.08.028. Epub 2010 Sep 24.
Monacolin K from red yeast rice was extracted by accelerated solvent extraction (ASE). The effects of various extraction parameters including extraction temperature, static extraction time and cycle index on yield were investigated using a DIONEX ASE 300 system to select the optimal conditions by an orthogonal test design L(9) (3)(3). The optimum extraction conditions were determined as follows: extraction temperature 120°C, static extraction time 7min, and cycle index 3. Under the optimal conditions, the yield of ASE extract and monacolin K was 5.35% and 9.26mg/g of dry red yeast rice, respectively. A separation and purification method of monacolin K was then established using high-speed counter-current chromatography (HSCCC) with a two-phase solvent system composed of n-hexane-ethyl acetate-methanol-water (8:2:5:5, v/v/v/v). From 300mg of crude extract, 51.2mg of monacolin K was obtained with the purity of 98.7%. The chemical structure of isolated compound was identified by UV, ESI-MS and (1)H NMR.
红曲米中的莫纳可林 K 通过加速溶剂萃取（ASE）进行提取。使用 Dionex ASE 300 系统，通过正交试验设计 L(9)（3）（3）研究了不同提取参数（包括提取温度、静态提取时间和循环指数）对产率的影响，以选择最佳条件。最佳提取条件确定为：提取温度 120°C，静态提取时间 7min，循环指数 3。在最佳条件下，ASE 提取物和莫纳可林 K 的产率分别为 5.35%和 9.26mg/g 干红曲米。然后使用由正己烷-乙酸乙酯-甲醇-水（8:2:5:5，v/v/v/v）组成的两相溶剂系统，通过高速逆流色谱（HSCCC）建立了莫纳可林 K 的分离和纯化方法。从 300mg 粗提取物中，获得了 51.2mg 纯度为 98.7%的莫纳可林 K。通过 UV、ESI-MS 和（1）H NMR 鉴定了分离得到的化合物的化学结构。
