Method for controlling mass of semen cassiae polysaccharide by utilizing multi-dimensional fingerprint
A technology of fingerprints and standard fingerprints, which is applied in the field of controlling the quality of cassia seed polysaccharides by using fingerprints, can solve the problems of not being able to accurately determine the type and content of polysaccharides in cassia seeds, and achieve the effect of stable quality
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Embodiment 1
[0060] Example 1 Cassia Semen Polysaccharide Extraction
[0061] Weigh 1.0 g of cassia seed sample over 40 mesh, and degrease with petroleum ether (30-60° C.) for 8 hours. Add 100 ml of water to the degreased and dried cassia seed sample, place in a water bath at 80° C. and magnetically stir for 3 hours, and combine the filtrates. Accurately weigh 0.01 g of papain, add to the filtrate, place in a constant temperature water bath shaker at 60°C, shake slowly for 2 hours, and cool to room temperature. Add 50mL of sevaga solution to the above-mentioned enzymatic sugar extract, shake it quickly on a constant temperature oscillator for 20min, centrifuge the mixed solution at a speed of 4000rpm for 5min, take the supernatant after phase separation, and repeat the above-mentioned "sevaga method to remove Protein" process until there is no milky white flocculent precipitate between the upper and lower phases, so as to remove the vegetable protein in the extract. Then add 15% (V / V) ma...
Embodiment 2
[0062] The GC analysis method of embodiment 2 cassia seed polysaccharide
[0063] 10 batches of cassia seed raw materials were subjected to polysaccharide extraction (using the method of Example 1).
[0064] Hydrolysis process of cassia seed polysaccharide: Precisely weigh 10mg of crude polysaccharide sample, put it into a 5mL ampoule, add 2.0ml, 0.5mol / L TFA solution, seal it with an alcohol blowtorch, place it at 110°C for 3h, after the reaction is completed, put The sample was taken out, cooled to room temperature, rinsed with methanol, transferred to a 5mL centrifuge tube, and centrifuged at 4000rpm for 5min; the supernatant was taken, transferred to a round bottom flask, evaporated to dryness under reduced pressure at 50°C, and ultrasonically dissolved with methanol, 50 °C to spin dry, repeat the treatment 4 times to remove residual TFA, evaporate the sample under reduced pressure, and set aside.
[0065] Derivatization of sugar nitrile acetate derivatization of cassia s...
Embodiment 3
[0075] The HPLC analysis method one of embodiment 3 cassia seed polysaccharide
[0076] Extraction and preparation of cassia seed polysaccharides: 10 batches of cassia seed raw materials were subjected to polysaccharide extraction and preparation according to Example 1.
[0077]Complete hydrolysis process of cassia seed polysaccharides: 10 batches of cassia seed polysaccharides were prepared by complete hydrolysis according to Example 2.
[0078] The 1-phenyl-3-methyl-5-pyrazolone (PMP) derivatization process of cassia seed polysaccharide hydrolyzate: dissolve the polysaccharide hydrolyzate in water, then transfer to a 10ml volumetric flask and constant volume, and accurately measure Put 0.2ml polysaccharide hydrolyzate into a 5ml stoppered glass centrifuge tube, add 0.2ml, 0.5mol / L PMP methanol solution and 0.2ml, 0.3mol / L NaOH solution in sequence, mix with ultrasonic, and react in 70℃ water bath for 60min, Cool to room temperature, add 0.2ml, 0.3mol / L HCl solution to neutr...
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