Iwata Tomotaka, Mori Masanobu, Itabashi Hideyuki, Tanaka Kazuhiko
Graduate School of Engineering, Gunma University, 1-5-1 Tenjin-cho, Kiryu, Gunma 376-8515, Japan.
Talanta. 2009 Sep 15;79(4):1026-30. doi: 10.1016/j.talanta.2009.03.042. Epub 2009 Mar 28.
In this study, a cation-exchange resin (CEX) of the K(+)-form, i.e., an enhancer resin, is used as a postcolumn conductimetric enhancer in the ion-exclusion chromatography of aliphatic carboxylic acids. The enhancer resin is filled in the switching valve of an ion chromatograph; this valve is usually used as a suppressor valve in ion-exchange chromatography. An aliphatic carboxylic acid (e.g., CH(3)COOH) separated by a weakly acidic CEX column of the H(+)-form converts into that of the K(+)-form (e.g., CH(3)COOK) by passing through the enhancer resin. In contrast, the background conductivity decreases because a strong acid (e.g., HNO(3)) with a higher conductimetric response in an eluent converts into a salt (e.g., KNO(3)) with a lower conductimetric response. Since the pH of the eluent containing the resin enhancer increases from 3.27 to 5.85, the enhancer accelerates the dissociations of analyte acids. Consequently, peak heights and peak areas of aliphatic carboxylic acids (e.g., acetic acid, propionic acid, butyric acid, and valeric acid) with the enhancer resin are 6.3-8.0 times higher and 7.2-9.2 times larger, respectively, than those without the enhancer resin. Calibrations of peak areas for injected analytes are linear in the concentration range of 0.01-1.0mM. The detection limits (signal-to-noise ratio=3) range from 0.10 microM to 0.39 microM in this system, as opposed to those in the range of 0.24-7.1 microM in the separation column alone. The developed system is successfully applied to the determination of aliphatic carboxylic acids in a chicken droppings sample.
在本研究中,钾离子形式的阳离子交换树脂(CEX),即增强剂树脂,被用作脂肪族羧酸离子排斥色谱中的柱后电导增强剂。增强剂树脂填充在离子色谱仪的切换阀中;该阀通常在离子交换色谱中用作抑制阀。通过氢离子形式的弱酸性CEX柱分离的脂肪族羧酸(如CH₃COOH),通过增强剂树脂后转化为钾离子形式(如CH₃COOK)。相反,背景电导率降低,因为洗脱液中具有较高电导响应的强酸(如HNO₃)转化为具有较低电导响应的盐(如KNO₃)。由于含有树脂增强剂的洗脱液的pH从3.27增加到5.85,增强剂加速了分析物酸的离解。因此,使用增强剂树脂时,脂肪族羧酸(如乙酸、丙酸、丁酸和戊酸)的峰高和峰面积分别比不使用增强剂树脂时高6.3 - 8.0倍和大7.2 - 9.2倍。注入分析物的峰面积校准在0.01 - 1.0mM的浓度范围内呈线性。该系统的检测限(信噪比 = 3)在0.10μM至0.39μM范围内,而仅在分离柱中的检测限在0.24 - 7.1μM范围内。所开发的系统成功应用于鸡粪样品中脂肪族羧酸的测定。