Liang Hao, Yuan Qipeng, Xiao Qian
Department of Pharmaceutical Engineering, Beijing University of Chemical Technology, Beijing 100029, PR China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2005 Dec 15;828(1-2):91-6. doi: 10.1016/j.jchromb.2005.09.041. Epub 2005 Oct 18.
Sulforaphane is an isothiocyanate that is present naturally in widely consumed Brassica oleracea vegetables and has been shown to block the formation of tumors. The contents of sulforaphane in five groups of B. oleracea seeds (broccoli, Brussels sprouts, cabbage, cauliflower and kale) were determined by RP-HPLC using linear gradient of acetonitrile in water. A new low-cost method to isolate and purify natural sulforaphane from B. oleracea seed meal was described in this work. Crude sulforaphane was first separated from B. oleracea seed meal by using immiscible solvent extraction with ethyl acetate, 10% ethanol and hexane, and the crude sulforaphane was used as raw materials to prepare high purity sulforaphane by low-pressure column chromatography of silica gel (200-300 mesh) with different eluents and elution modes. Compared with these different elution methods, the gradient elution was preferable to the isocratic elution for reducing the elution time and the eluent consumption and increasing the purity of sulforaphane product. The purity and recovery of sulforaphane were more than 90% in gradient elution.
萝卜硫素是一种异硫氰酸盐，天然存在于广泛食用的十字花科蔬菜中，已被证明能阻止肿瘤形成。采用乙腈在水中的线性梯度，通过反相高效液相色谱法（RP-HPLC）测定了五组十字花科种子（西兰花、抱子甘蓝、卷心菜、花椰菜和羽衣甘蓝）中萝卜硫素的含量。本文描述了一种从十字花科种子粕中分离纯化天然萝卜硫素的低成本新方法。首先通过用乙酸乙酯、10%乙醇和己烷进行不混溶溶剂萃取从十字花科种子粕中分离出粗萝卜硫素，并将粗萝卜硫素用作原料，通过使用不同洗脱剂和洗脱模式的硅胶（200-300目）低压柱色谱法制备高纯度萝卜硫素。与这些不同的洗脱方法相比，梯度洗脱在减少洗脱时间和洗脱剂消耗以及提高萝卜硫素产品纯度方面优于等度洗脱。在梯度洗脱中，萝卜硫素的纯度和回收率均超过90%。
