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

文献类型： 外文期刊

第一作者： Li, Xiuhuan

作者： Li, Xiuhuan;Zheng, Li;Wu, Miaomiao;Huang, Qiliang;Wu, Jinlong;Liu, Pingping

作者机构：

关键词： chitooligosaccharides;HPAEC-PAD;method validation;quantification;hydrolysis

期刊名称：INTERNATIONAL JOURNAL OF MOLECULAR SCIENCES （ 影响因子：5.923； 五年影响因子：6.132 ）

ISSN： 1422-0067

年卷期： 2016 年 17 卷 10 期

页码：

收录情况： SCI

摘要： 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 x 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 (R-2 = 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.

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