Institute of Food and Biological Engineering, Zhejiang Gongshang University, 149 Jiaogong Road, Hangzhou, Zhejiang 310035, China.
J Chromatogr A. 2011 Sep 9;1218(36):6187-90. doi: 10.1016/j.chroma.2010.12.062. Epub 2010 Dec 21.
The flash high speed counter-current chromatographic (FHSCCC) separation of gingerols and 6-shogaol was performed on a HSCCC instrument equipped with a 1200-ml column (5 mm tubing i.d.) at a flow rate of 25 ml/min. The performance met the FHSCCC feature that the flow rate of mobile phase (ml) is equal to or greater than the square of the diameter of the column tubing (mm). The separation employed the upper phase of stationary phase of the n-hexane-ethyl acetate-methanol-water (3:2:2:3, v/v) as the stationary phase. A stepwise elution was performed by eluting with the lower phase of n-hexane-ethyl acetate-methanol-water (3:2:2:3, v/v) for first 90 min and the lower phase of the n-hexane-ethyl acetate-methanol-water (3:2:6:5, v/v) for the second 90 min. In each separation 5 g of the ethyl acetate extract of rhizomes of ginger was loaded, yielding 1.96 g of 6-gingerol (98.3%), 0.33 g of 8-gingerol (97.8%), 0.64 g of 6-shogaol (98.8%) and 0.57 g of 10-gingerol (98.2%). The separation can be expected to scale up to industrial separation.
采用高速逆流色谱仪(HSCCC),以正己烷-乙酸乙酯-甲醇-水(3:2:2:3,v/v)为上相,正己烷-乙酸乙酯-甲醇-水(3:2:6:5,v/v)为下相,在 25ml/min 的流速下,对生姜中的姜醇和 6-姜烯酚进行 Flash 高速逆流色谱分离。该仪器配备了一个 1200ml 的柱(5mm 管内径),满足高速逆流色谱的特征,即流动相的流速(ml)等于或大于柱管直径(mm)的平方。在上相的流速为 25ml/min 时,每次分离上相体积为 5g,对生姜的乙酸乙酯提取物进行分离,可得到 1.96g 的 6-姜醇(98.3%)、0.33g 的 8-姜醇(97.8%)、0.64g 的 6-姜烯酚(98.8%)和 0.57g 的 10-姜酚(98.2%)。该分离方法有望放大到工业规模。