蔗糖酯的薄层色谱分析

Analysis of Sucrose Esters by Thin-Layer Chromatography

以硅胶G板为固定相、甲苯 乙酸乙酯 甲醇 水 (体积比为 1 0∶5∶4 5∶0 2 )为流动相 ,研究建立了蔗糖酯薄层色谱分析方法。在蔗糖酯上行展开后 ,用脲 磷酸 水饱和正丁醇溶液显色 ,斑点呈蓝色 ,蔗糖单酯的Rf 值为 0 1 6 ,多酯的Rf 值为 0 38～ 0 93。在 70℃显色 2 0min的最佳条件下 ,蔗糖单酯的检测量为 2 5 μg～ 2 50 μg时 ,其斑点面积与其检测量有良好的线性关系。用归一法和外标法对该分析方法的准确度进行考察和认证 ,两种方法对已知单酯含量的S 1 570样品测定结果的t 检验结果分别为 |t| =0 62 7(<2 571 )和 |t|=1 1 2 3(<2 571 ) ,相对标准偏差(RSD) (n =6)分别为 3 0 3 %和 3 0 8% ,最低检出限为 0 1 μg。用该方法对不同蔗糖酯样品中的单酯含量进行了测定 。

The thin layer chromatographic method of sucrose esters was developed by the use of toluene ethyl acetate methanol water (10∶5∶4 5∶0 2 in volume ratio) as a mobile phase. Sucrose esters were developed by ascending technique on the silica gel G plate, visualized by urea phosphoric acid n butanol with blue spots. The R f value of monoester was 0 16 and those of higher esters were 0 38-0 93. The calibration curve was linear in the range of 25 μg-250 μg with the detection limit of 0 1 μg. Accuracies were certified by normalization method and external standard method with t test. The results were | t |=0 627(< 2 571 ) and | t |=1 123(< 2 571 ) and RSDs were 3 03% and 3 08%( n =6) respectively for S 1570. Contents of monoester of different sucrose esters were determined, which could provide reference for synthetic conditions and application range of sucrose esters.