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蔗糖酯的薄层色谱分析

Analysis of Sucrose Esters by Thin-Layer Chromatography

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【作者】 李延科张淑芬杨锦宗

【Author】 LI Yan ke, ZHANG Shu fen, YANG Jin zong (State Key Laboratory of Fine Chemicals, Dalian University of Technology, Dalian 116012, China)

【机构】 大连理工大学精细化工国家重点实验室大连理工大学精细化工国家重点实验室 辽宁大连116012辽宁大连116012辽宁大连116012

【摘要】 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 ,为研究获得不同单酯含量的蔗糖酯的合成条件和确定蔗糖酯的应用范围提供了依据

【Abstract】 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.

  • 【文献出处】 色谱 ,Chinese Journal of Chromatography , 编辑部邮箱 ,2002年05期
  • 【分类号】O657.7
  • 【被引频次】53
  • 【下载频次】566
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