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建立了制备型凝胶渗透色谱(GPC)技术制备毫克量级的氧化三酰甘油二聚物(TGD)和氧化三酰甘油寡聚物(TGO)的方法。首先,采用制备型快速柱层析(PFC),经FLASH柱分离出油脂极性组分(polarcompounds,PCs),45℃旋转蒸干,薄层色谱(TLC)验证PCs分离效果;然后,将PCs四氢呋喃溶液按4.2mL/min流速进入制备型凝胶渗透色谱系统,按照分子量大小的差异,对PCs中的TGO和TGD进行分离,然后根据这些物质出峰时间,分别进行收集。TGO、TGD的收集时间分别为29.00～32.10min、32.25～33.50min,收集的溶液45℃旋转蒸近干,0.1MP烘干30min。制取的TGD、TGO与原料PCs同步进行HPSEC分析,验证了各制备组分的真实性。
A method for the preparation of milligram oxidized triacylglycerol dimers (TGDs) and oxidized triacylglycerol oligomers (TGOs) by preparative gel permeation chromatography (GPC) was established. Firstly, PFCs were separated by flash column, and polar compounds (PCs) were separated by flash column. The separation of PCs was verified by thin layer chromatography (TLC) at 45 ℃. Then, The tetrahydrofuran solution enters the preparative gel permeation chromatography system at a flow rate of 4.2 mL / min. The TGO and TGD in PCs are separated according to the difference in molecular weight, and then collected separately according to the peak time of these substances. TGO, TGD collection time were 29.00 ~ 32.10min, 32.25 ~ 33.50min, the collected solution 45 ℃ rotary steam near dry, 0.1MP drying 30min. Preparation of TGD, TGO and raw materials simultaneously with HPSEC PCs analysis to verify the authenticity of the preparation components.