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Polysaccharide is widely distributed in natural resources, and currently attracts scientists' attention for their various bio‐functions including immunomodulatory activity, hypoglycemic activity, hypolipidemic activity, antitumor activity, promoting effects on gastrointestinal function, and so on. The purity and structure characteristics of different polysaccharides greatly restrict the in‐depth study of their bioactivity mechanism. Therefore, this guideline will display the extraction, isolation, purification, and structural characterization of polysaccharides from natural resources. The extraction methods of acid‐soluble polysaccharides, water‐soluble polysaccharides, and alkaline soluble polysaccharides are included. Common purification methods like membrane filtration, alcohol precipitation, and column chromatographic separation are explained in detail. A comprehensive procedure for polysaccharide structural characterization is given from molecular weight and monosaccharide composition study to Fourier transform infrared and nuclear magnetic resonance analysis. Examples are added where necessary to help you better understand this guideline.

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