开发用于枸杞中多糖和单糖定量的柱前衍生超高效液相色谱法。

IF 2.8 3区 工程技术 Q2 CHEMISTRY, ANALYTICAL Journal of separation science Pub Date : 2024-09-04 DOI:10.1002/jssc.202400507
Zhilong Zhao, Yunfeng Bai, Huan Chen, Weibiao Wang, Shuqin Ding, Yue Zhang, Yuping Sa, Guoning Chen, Xueqin Ma
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引用次数: 0

摘要

鉴于目前官方比色法定量枸杞多糖的特异性和准确性有限,我们的研究旨在建立一种新型、特异、准确、经济的柱前衍生超高效液相色谱(UHPLC)方法,用于测定枸杞中的单糖和多糖含量。首先对枸杞多糖的提取、水解和衍生化(使用 1-苯基-3-甲基-5-吡唑啉酮)过程进行了优化,然后使用 C18 柱超高压液相色谱法在 20 分钟内分离出 9 种单糖。随后,研究人员开发了一种称为 "单标记多成分定量分析 "的新方法,利用添加剂 2-脱氧-D-核糖或样品中存在的任何单糖作为单一参考标准,同时检测枸杞多糖和九种单糖的含量。为了验证所建立方法的准确性,我们将其定量结果与外标法和内标法进行了比较。在三种方法中,单糖定量测定的相对误差最小,这证实了该方法的可靠性。通过分析 20 批次枸杞样品,D-半乳糖醛酸的含量最高,多糖含量在 3.02 至 13.04 mg/g 之间。所有数据表明该方法具有特异性和准确性。
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Development of a pre-column derivatization ultra-high-performance liquid chromatography method for polysaccharide and monosaccharide quantification in Lycium barbarum

Given the limited specificity and accuracy observed in the current official colorimetric quantification of polysaccharide in Lycium barbarum, our study aims to establish a novel, specific, accurate, and economic pre-column derivatization ultra-high-performance liquid chromatography (UHPLC) method for determining the monosaccharide and polysaccharide content in L. barbarum. The optimization of extraction, hydrolysis, and derivatization (using 1-phenyl-3-methyl-5-pyrazolone) processes for polysaccharide from L. barbarum was conducted initially, followed by separation of nine monosaccharides within 20 min using UHPLC with a C18 column. Subsequently, a novel method known as quantitative analysis of multiple components by single marker was developed, utilizing either additive 2-deoxy-D-ribose or any monosaccharide present in the sample as a single reference standard to simultaneously detect the contents of polysaccharide and nine monosaccharides in L. barbarum. To validate the accuracy of the established method, the quantitative results of our approach were compared to both external and internal standard method methods. The minimal relative errors in the quantitative determination of monosaccharides among the three methods confirmed the dependability of the method. By analyzing 20 batches of L. barbarum samples, D-galacturonic acid exhibited the highest content and the polysaccharide levels ranged from 3.02 to 13.04 mg/g. All data implied the specificity and accuracy of the method.

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来源期刊
Journal of separation science
Journal of separation science 化学-分析化学
CiteScore
6.30
自引率
16.10%
发文量
408
审稿时长
1.8 months
期刊介绍: The Journal of Separation Science (JSS) is the most comprehensive source in separation science, since it covers all areas of chromatographic and electrophoretic separation methods in theory and practice, both in the analytical and in the preparative mode, solid phase extraction, sample preparation, and related techniques. Manuscripts on methodological or instrumental developments, including detection aspects, in particular mass spectrometry, as well as on innovative applications will also be published. Manuscripts on hyphenation, automation, and miniaturization are particularly welcome. Pre- and post-separation facets of a total analysis may be covered as well as the underlying logic of the development or application of a method.
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