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以5-甲基己酸为洗脱剂,在磺化苯乙烯-二乙烯基苯共聚物树脂柱上对C1-C6脂肪族羧酸进行离子排斥色谱分离。

Ion-exclusion chromatographic separations of C1-C6 aliphatic carboxylic acids on a sulfonated styrene-divinylbenzene co-polymer resin column with 5-methylhexanoic acid as eluent.

作者信息

Ohta Kazutoku, Towata Atsuya, Ohashi Masayoshi

机构信息

Ceramics Research Institute, National Institute of Advanced Industrial Science and Technology 2266-98 Anagahora, Simoshidami, Moriyama-ku, Nagoya 463-8560, Japan.

出版信息

J Chromatogr A. 2003 May 16;997(1-2):107-16. doi: 10.1016/s0021-9673(03)00627-7.

Abstract

The application of C7 aliphatic carboxylic acids (heptanoic, 2-methylhexanoic, 5-methylhexanoic and 2,2-dimethyl-n-valeric acids) as eluents in ion-exclusion chromatography with conductimetric detection for C1-C6 aliphatic carboxylic acids (formic, acetic, propionic, isobutyric, butyric, isovaleric, valeric, isocaproic and caproic acids) was carried out using a highly sulfonated styrene-divinylbenzene co-polymer resin (TSKgel SCX) in the H+ form as a stationary phase. When using 0.05 mM sulfuric acid at pH 4.0 as the eluent, peak shapes of hydrophobic carboxylic acids (isovaleric, valeric, isocaproic and caproic acids) were tailed strongly. In contrast, when using 1 mM these C7 carboxylic acids at pH ca. 4 as the eluents, although system peaks (vacant peaks) corresponding to these C7 carboxylic acids appeared, peak shapes of these hydrophobic acids were improved drastically. Excellent simultaneous separation and relatively high sensitive conductimetric detection for these C1-C6 aliphatic carboxylic acids were achieved in 25 min on the TSKgel SCX column (150 x 6 mm I.D.) using 1 mM 5-methylhexanoic acid at pH 4.0 as the eluent.

摘要

以高磺化苯乙烯 - 二乙烯基苯共聚物树脂(TSKgel SCX)的H⁺形式作为固定相,开展了C7脂肪族羧酸(庚酸、2 - 甲基己酸、5 - 甲基己酸和2,2 - 二甲基戊酸)作为洗脱剂用于离子排斥色谱法并采用电导检测法测定C1 - C6脂肪族羧酸(甲酸、乙酸、丙酸、异丁酸、丁酸、异戊酸、戊酸、异己酸和己酸)的研究。当使用pH 4.0的0.05 mM硫酸作为洗脱剂时,疏水性羧酸(异戊酸、戊酸、异己酸和己酸)的峰形严重拖尾。相比之下,当使用pH约为4的1 mM这些C7羧酸作为洗脱剂时,虽然出现了与这些C7羧酸对应的系统峰(空峰),但这些疏水性酸的峰形得到了极大改善。使用pH 4.0的1 mM 5 - 甲基己酸作为洗脱剂,在TSKgel SCX柱(内径150×6 mm)上25分钟内实现了对这些C1 - C6脂肪族羧酸的出色同时分离和相对高灵敏度的电导检测。

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