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采用高效液相色谱-电喷雾飞行时间质谱法定量分析 中的多糖组成。

Quantitative Analysis of Polysaccharide Composition in by HPLC-ESI-TOF-MS.

机构信息

School of Pharmaceutical Sciences, Peking University, Beijing 100191, China.

Kangmei Pharmaceutical Co.Ltd, Puning 515300, China.

出版信息

Molecules. 2019 Jul 10;24(14):2526. doi: 10.3390/molecules24142526.

DOI:10.3390/molecules24142526
PMID:31295903
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC6681038/
Abstract

is a well-known and important medicinal fungus in Asia. Its polysaccharides possess interesting bioactivities such as antitumor, antioxidant, hepatoprotective and immunomodulatory effects. A qualitative and quantitative method has been established for the analysis of 12 monosaccharides comprising polysaccharides of based on high-performance liquid chromatography coupled with electrospray ionization-ion trap-time of flight-mass spectrometry. The hydrolysis conditions of the polysaccharides were optimized by orthogonal design. The results of optimized hydrolysis were as follows: neutral sugars and uronic acids 4 mol/L trifluoroacetic acid (TFA), 6 h, 120 °C; and amino sugars 3 mol/L TFA, 3 h, 100 °C. The resulting monosaccharides derivatized with 1-phenyl-3-methyl-5-pyrazolone have been well separated and analyzed by the established method. Identification of the monosaccharides was carried out by analyzing the mass spectral behaviors and chromatography characteristics of 1-phenyl-3-methyl-5-pyrazolone labeled monosaccharides. The results showed that polysaccharides in were composed of mannose, glucosamine, rhamnose, ribose, lyxose, erythrose, glucuronic acid, galacturonic acid, glucose, galactose, xylose, and fucose. Quantitative recoveries of these monosaccharides in the samples were in the range of 96.10-103.70%. This method is simple, accurate, and sensitive for the identification and quantification of monosaccharides, and can be applied to the quality control of as a natural medicine.

摘要

是亚洲地区一种著名且重要的药用真菌。其多糖具有有趣的生物活性,如抗肿瘤、抗氧化、保肝和免疫调节作用。已经建立了一种基于高效液相色谱-电喷雾离子阱-飞行时间质谱联用技术分析包含多糖的 12 种单糖的定性和定量方法。通过正交设计优化了多糖的水解条件。优化水解的结果如下:中性糖和糖醛酸 4 mol/L 三氟乙酸(TFA),6 h,120°C;氨基糖 3 mol/L TFA,3 h,100°C。用 1-苯基-3-甲基-5-吡唑啉酮衍生的单糖通过建立的方法得到了很好的分离和分析。通过分析 1-苯基-3-甲基-5-吡唑啉酮标记单糖的质谱行为和色谱特征,对单糖进行了鉴定。结果表明, 中的多糖由甘露糖、葡萄糖胺、鼠李糖、核糖、木糖、赤藓糖、葡萄糖醛酸、半乳糖醛酸、葡萄糖、半乳糖、木糖和岩藻糖组成。这些单糖在样品中的定量回收率在 96.10-103.70%范围内。该方法简单、准确、灵敏,可用于鉴定和定量分析单糖,可作为天然药物对 进行质量控制。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/7b3b/6681038/4a18e8d026f3/molecules-24-02526-g002.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/7b3b/6681038/d5e679c8f989/molecules-24-02526-g001.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/7b3b/6681038/4a18e8d026f3/molecules-24-02526-g002.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/7b3b/6681038/d5e679c8f989/molecules-24-02526-g001.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/7b3b/6681038/4a18e8d026f3/molecules-24-02526-g002.jpg

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