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Int. J. Mol. Sci. 2016, 17(10), 1699;

Validated HPAEC-PAD Method for the Determination of Fully Deacetylated Chitooligosaccharides

Key Laboratory of Pesticide Chemistry and Application, Ministry of Agriculture, Institute of Plant Protection, Chinese Academy of Agricultural Sciences, No. 2 Yuanmingyuan West Road, Beijing 100193, China
Institute for the Control of Agrochemicals, Ministry of Agriculture, No. 22 Maizidian Street, Beijing 110000, China
Author to whom correspondence should be addressed.
Academic Editor: Hermann Ehrlich
Received: 28 July 2016 / Revised: 29 September 2016 / Accepted: 30 September 2016 / Published: 10 October 2016
(This article belongs to the Special Issue Frontiers of Marine Biomaterials)
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An efficient and sensitive analytical method based on high-performance anion exchange chromatography with pulsed amperometric detection (HPAEC-PAD) was established for the simultaneous separation and determination of glucosamine (GlcN)1 and chitooligosaccharides (COS) ranging from (GlcN)2 to (GlcN)6 without prior derivatization. Detection limits were 0.003 to 0.016 mg/L (corresponding to 0.4–0.6 pmol), and the linear range was 0.2 to 10 mg/L. The optimized analysis was carried out on a CarboPac-PA100 analytical column (4 × 250 mm) using isocratic elution with 0.2 M aqueous sodium hydroxide-water mixture (10:90, v/v) as the mobile phase at a 0.4 mL/min flow rate. Regression equations revealed a good linear relationship (R2 = 0.9979–0.9995, n = 7) within the test ranges. Quality parameters, including precision and accuracy, were fully validated and found to be satisfactory. The fully validated HPAEC-PAD method was readily applied for the quantification of (GlcN)1–6 in a commercial COS technical concentrate. The established method was also used to monitor the acid hydrolysis of a COS technical concentrate to ensure optimization of reaction conditions and minimization of (GlcN)1 degradation. View Full-Text
Keywords: chitooligosaccharides; HPAEC-PAD; method validation; quantification; hydrolysis chitooligosaccharides; HPAEC-PAD; method validation; quantification; hydrolysis

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This is an open access article distributed under the Creative Commons Attribution License which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited (CC BY 4.0).

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Cao, L.; Wu, J.; Li, X.; Zheng, L.; Wu, M.; Liu, P.; Huang, Q. Validated HPAEC-PAD Method for the Determination of Fully Deacetylated Chitooligosaccharides. Int. J. Mol. Sci. 2016, 17, 1699.

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