Zhang Wenbin, Xu Shiying
School of Food Science and Technology, Southern Yangtze University, Wuxi 214036, PR China.
J Chromatogr Sci. 2007 Apr;45(4):177-82. doi: 10.1093/chromsci/45.4.177.
A simplified and efficient method is developed for the large-scale purification of the secoisolariciresinol diglucoside (SDG) from defatted flaxseed after aqueous ethanol extraction. Extractant from defatted flaxseed with aqueous ethanol is hydrolyzed with basic solution, concentrated under vacuum, subjected to Sephadex LH-20 column chromatography, and eluted with aqueous ethanol of different concentrations. Elution is monitored by a UV detector at 280 nm, and fractions containing SDG are pooled, concentrated, and applied to a second column chromatography under the same conditions. Elution with water results in a better resolution of SDG [94.5% by high-performance liquid chromatography (HPLC)] than that with pure ethanol or 50% (v/v) aqueous ethanol. HPLC-photodiode array detection-mass spectrometry and NMR are applied to identify SDG and to determine the purity of the eluted fraction. This simplified purification scheme avoids toxic organic solvent used in the common silica gel separation process and, thus, increases the safety of the process.
开发了一种简单高效的方法，用于从乙醇水溶液提取后的脱脂亚麻籽中大规模纯化开环异落叶松脂素二葡萄糖苷（SDG）。用碱性溶液水解乙醇水溶液提取的脱脂亚麻籽提取物，真空浓缩，进行葡聚糖凝胶LH - 20柱色谱分离，并用不同浓度的乙醇水溶液洗脱。在280 nm处用紫外检测器监测洗脱过程，合并含有SDG的馏分，浓缩，并在相同条件下进行第二次柱色谱分离。用水洗脱比用纯乙醇或50%（v/v）乙醇水溶液洗脱能得到更好的SDG分离效果[高效液相色谱（HPLC）测定纯度为94.5%]。应用HPLC - 光电二极管阵列检测 - 质谱联用和核磁共振技术鉴定SDG并测定洗脱馏分的纯度。这种简化的纯化方案避免了普通硅胶分离过程中使用的有毒有机溶剂，从而提高了该过程的安全性。
