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Int. J. Mol. Sci. 2016, 17(10), 1699; doi:10.3390/ijms17101699

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

1
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
2
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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Abstract

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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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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