摘要
The analysis of sucrose esters with long acyl chain by improved high performance liquid chromatographic method with evaporative light scattering detection (HPLC-ELSD) and electrospray ionization mass spectrum (ESI-MS) is investigated. The improved HPLC-ELSD method for the separation and quantitation of commercial and synthesized sucrose esters is described. Samples are analyzed by means of a reversed-phase (RP) HPLC using a Hypersil C8 column (250 mm× 4.6 mm, 5 μm particle size) with methanol-tetrahydrofuran (vo)ume ratio of 90 : 10) and water under gradientcondition as the mobile phase, in which the flow rate is 1.0 ml·min^-1 and the column temperature is set at 40℃. This procedure provides a complete separation and determination ot monoester, diester, triester and higher esters with different acyl chain lengths in each fraction by a single run, in combination with the ESI-MS technology. With this method, it is possible to determine the approximate compositions of monoto polyesters in one analysis and quantitate pure positional isomers precisely using an external standard method. It is found that the method of ESI-MS coupling with HPLC system for the analysis of sucrose esters is straight forward, rapid and inexpensive, and can be readily applied in synthesis, purification and structure studies.
有由改进高效液体的长酰链的蔗糖酉旨的分析察觉(HPLC-ELSD ) 和电镀物品祈祷的有成为蒸气的轻散布的色析法的方法电离团光谱(ESIMS ) 被调查。为商业、综合的蔗糖酉旨的分离和 quantitation 的改进 HPLC-ELSD 方法被描述。样品被分析借助于一反向阶段( RP )用 Hypersil C8 列的 HPLC ( 250 mm× ; 4.6 公里, 5 μ ; m 粒子尺寸)与 methanol-tetrahydrofuran ( 90:10 的体积比率)和在是的坡度状况下面的水活动阶段,在哪个流动率是 1.0 ml· ; min <sup>−1</sup>和列温度被放在 40 ° ; C 。这个过程提供单音的酉旨的完全的分离和决心, diest 嗯, triest 嗯并且有在由一个单身者的每部分的不同的酰链长度的更高的酉旨跑,在有 ESIMS 技术的联合。与这个方法,决定近似作文是可能的单音 -- 到在一分析的聚酯并且测定精确使用一个外部标准方法的纯位置的异构体。为蔗糖酉旨的分析结合 HPLC 系统的 ESIMS 的方法笔直地前面、快速、便宜,这被发现,并且能乐意地在合成被使用,咕噜咕噜叫 i ? 阳离子和结构研究。
基金
Supported by the National Natural Science Foundation of China (20906052), the Science Foundation of Nantong City Municipality (K2007011, K2008023), the Science Foundation of Nantong University (08R08) and the University Science Research Project of Jiangsu Province (09KJB530008).