Ohta Kazutoku, Towata Atsuya, Ohashi Masayoshi
Ceramics Research Institute, National Institute of Advanced Industrial Science and Technology, 2266-98 Anagahora, Simoshidami, Moriyama-ku, Nagoya 463-8560, Japan.
J Chromatogr A. 2003 May 16;997(1-2):95-106. doi: 10.1016/s0021-9673(03)00079-7.
The addition of C1-C7 alcohols (methanol, ethanol, propanol, butanol, heptanol, hexanol and heptanol) to dilute sulfuric acid as eluent in ion-exclusion chromatography using a highly sulfonated styrene-divinylbenzene co-polymer resin (TSKgel SCX) in the H+ form as the stationary phase was carried out for the simultaneous separations of both (a) C1-C7 aliphatic carboxylic acids (formic, acetic, propionic, isobutyric, butyric, isovaleric, valeric, 2-methylvaleric, isocaproic, caproic, 2,2-dimethyl-n-valeric, 2-methylhexanoic, 5-methylhexanoic and heptanoic acids) and (b) benzenecarboxylic acids (pyromellitic, hemimellitic, trimellitic, o-phthalic, m-phthalic, p-phthalic, benzoic and salicylic acids and phenol). Heptanol was the most effective modifier in ion-exclusion chromatography for the improvement of peak shapes and a reduction in retention volumes for higher aliphatic carboxylic acids and benzenecarboxylic acids. Excellent simultaneous separation and relatively highly sensitive conductimetric detection for these C1-C7 aliphatic carboxylic acids were achieved on the TSKgel SCX column (150 x 6 mm I.D.) in 30 min using 0.5 mM sulfuric acid containing 0.025% heptanol as eluent. Excellent simultaneous separation and highly sensitive UV detection at 200 nm for these benzenecarboxylic acids were also achieved on the TSKgel SCX column in 30 min using 5 mM sulfuric acid containing 0.075% heptanol as eluent.
在离子排斥色谱中,使用H⁺形式的高度磺化苯乙烯 - 二乙烯基苯共聚物树脂(TSKgel SCX)作为固定相,将C1 - C7醇(甲醇、乙醇、丙醇、丁醇、己醇和庚醇)添加到稀硫酸中作为洗脱剂,用于同时分离(a)C1 - C7脂肪族羧酸(甲酸、乙酸、丙酸、异丁酸、丁酸、异戊酸、戊酸、2 - 甲基戊酸、异己酸、己酸、2,2 - 二甲基 - n - 戊酸、2 - 甲基己酸、5 - 甲基己酸和庚酸)和(b)苯羧酸(均苯四甲酸、偏苯三酸、苯三甲酸、邻苯二甲酸、间苯二甲酸、对苯二甲酸、苯甲酸和水杨酸以及苯酚)。庚醇是离子排斥色谱中最有效的改性剂,可改善较高脂肪族羧酸和苯羧酸的峰形并降低保留体积。使用含0.025%庚醇的0.5 mM硫酸作为洗脱剂,在TSKgel SCX柱(内径150×6 mm)上30分钟内实现了对这些C1 - C7脂肪族羧酸的出色同时分离和相对高灵敏度的电导检测。使用含0.075%庚醇的5 mM硫酸作为洗脱剂,在TSKgel SCX柱上30分钟内也实现了对这些苯羧酸的出色同时分离和在200 nm处的高灵敏度紫外检测。