DEVELOPMENT OF AN HPLC METHOD FOR THE DETERMINATION OF GLYCEROL OXIDATION PRODUCTS

Abstract

An HPLC method for the separation of glycerol oxidation products, namely glyceraldehyde, dihydroxyacetone, mesoxalic, tartronic, and glycolic and glyceric acids on an ion-exchange 8% cross-linked calcium sulfonated divinylbenzene-styrene resin column was developed and validated. The conditions reported include temperature (70°C), flow rate (0.5 mL/min) and concentration of the mobile phase (3 mM H₂SO₄) using isocratic elution with ultraviolet and refractometric detectors. The effect of the mobile phase flow rate and concentration as well as column temperature on the resolution of peaks is described. Excellent correlation coefficient in the calibration model was observed for all analytes over the concentration range of 0.5 to 10 mg/mL. The method was also validated in terms of intra-day precision, sensitivity, accuracy, and detection and quantification limits. The method conditions were applied to the identification of products derived from the chemical oxidation of glycerol.

Supplemental materials are available for this article. Go to the publisher's online edition of the Journal of Liquid Chromatography & Related Technologies to view the supplemental file.

Keywords:

• dihydroxyacetone
• glyceraldehyde
• glycerol oxidation
• HPLC method
• ion exchange
• validation

ACKNOWLEDGMENT

The project was financially supported by the European Regional Development Fund (ERDF) under the Project CEBIA-Tech No. CZ.1.05/2.1.00/03.0089, with support of Operational Program Research and Development for Innovations co-funded by the ERDF and national budget of Czech Republic, within the framework of project Center of Polymer Systems (reg. number: CZ.1.05/2.1.00/03.0111) and Tomas Bata University Internal Grant (IGA/FAI/2012/029). J. C. Beltrán-Prieto is also grateful for the doctoral scholarship provided by Tomas Bata University in Zlín and the National Council of Science and Technology (CONACYT) in Mexico.

Notes

^a Resolution was calculated according to the expression (4).

^a Range 0–10 mg/mL.

n.a., not applicable.

n.a., not applicable.

n.a., not applicable.