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锆改性硅胶作为固定相在羧酸离子排斥色谱中的应用。II. 以均苯四甲酸为洗脱剂并采用抑制型电导检测法分离脂肪族羧酸

Application of zirconium-modified silica gel as a stationary phase in the ion-exclusion chromatography of carboxylic acids. II. Separation of aliphatic carboxylic acids with pyromellitic acid as eluent and with suppressed conductimetric detection.

作者信息

Ohta K

机构信息

National Industrial Research Institute of Nagoya, Japan.

出版信息

J Chromatogr A. 2001 Jun 22;920(1-2):181-91. doi: 10.1016/s0021-9673(01)00682-3.

DOI:10.1016/s0021-9673(01)00682-3
PMID:11452997
Abstract

The application of zirconium-modified silica gels (Zr-Silica) as stationary phases for ion-exclusion chromatography with conductimetric detection (IEC-CD) for C1-C8 aliphatic carboxylic acids (formic, acetic, propionic, butyric, valeric, caproic, heptanoic and caprylic acids) was carried out using pyromellitic acid as the eluent. Zr-Silicas were prepared by the reaction of the silanol group on the surface of silica gel with zirconium tetrabutoxide [Zr(OCH2CH2CH2CH3)4] in ethanol solution. An ASRS-Ultra anion self-regenerating suppressor in the K+ form was used for the enhancement of conductimetric detector response of these aliphatic carboxylic acids. A Zr-Silica adsorbed on 10 mg zirconium g(-1) silica gel was the most suitable stationary phase in IEC-CD for the separation of these aliphatic carboxylic acids. Excellent simultaneous separation and highly sensitive detection for these aliphatic carboxylic acids were achieved in 25 min by IEC-CD with the Zr-Silica column (250x4.6 mm I.D.) and a 0.2 mM pyromellitic acid containing 0.15% heptanol as the eluent.

摘要

以均苯四甲酸为洗脱剂,研究了锆改性硅胶(Zr-硅胶)作为固定相用于离子排斥色谱-电导检测(IEC-CD)分析C1-C8脂肪族羧酸(甲酸、乙酸、丙酸、丁酸、戊酸、己酸、庚酸和辛酸)的应用。Zr-硅胶是通过硅胶表面的硅醇基团与乙醇溶液中的四丁氧基锆[Zr(OCH2CH2CH2CH3)4]反应制备的。采用K+形式的ASRS-Ultra阴离子自再生抑制器来增强这些脂肪族羧酸的电导检测器响应。在IEC-CD中,吸附有10 mg锆/g硅胶的Zr-硅胶是分离这些脂肪族羧酸最合适的固定相。使用Zr-硅胶柱(内径250x4.6 mm),以含有0.15%庚醇的0.2 mM均苯四甲酸为洗脱剂,通过IEC-CD在25分钟内实现了对这些脂肪族羧酸的优异同时分离和高灵敏度检测。

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