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用气相层析法从天然产物中分离纯化(微克级)生物活性物质是一种简便而有效的方法。然而在气相层析制备时,则由于用作密封玻璃柱的硅橡胶垫圈有分解现象,往往引起GC本底的明显增高,产生了误差。我们改用柔性石墨作为密封玻璃柱的垫圈后,GC本底显著降低,为制备较纯样品创造了条件。微量制备气相层析仪由上分102型改装。9.2％OV-1(二甲基硅酮)涂于Gas Chrom Q 80～100目;柱温:180℃;氮气流量:60毫升/分;用馏份收集管(长30厘米,ф2.0×0.5毫米的玻璃毛细管)收集15分钟,然后用10微升重蒸过的A.R四氯化碳冲洗下来,在Perkin～Elmer 580B红外分光光度计上测定。用硅橡胶垫圈及柔性石墨垫圈时,产生流出物的IR图如下:
Purification of natural (microgram) bioactive substances by gas chromatography is a simple and effective method. However, in gas phase chromatography, the decomposition of the silicone rubber gasket used as a sealing glass column tends to cause a noticeable increase in GC background with errors. When we use flexible graphite as a gasket for sealing glass columns, the GC background is significantly reduced, creating the conditions for the preparation of purer samples. Micro-preparative gas chromatography modified by the 102 sub-type. 9.2% OV-1 (Dimethyl Silicone) was applied to a Gas Chrom Q 80-100 mesh; column temperature was 180C; nitrogen flow rate was 60 ml / min; 0.5 mm glass capillaries) for 15 minutes and then rinsed with 10 [mu] l of resteemed AR carbon tetrachloride and measured on a Perkin Elmer 580B infrared spectrophotometer. The IR image of the effluent produced with the silicone rubber washer and the flexible graphite washer is as follows: