Modified semen cassiae polysaccharide as well as preparation method and application thereof
A technology of cassia seeds and polysaccharides is applied in the directions of pharmaceutical formulations, organic active ingredients, medical preparations containing active ingredients, etc., to achieve the effects of reliable preparation method and stable structure
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Embodiment 1
[0042] The embodiment of the present invention provides a preparation method of modified cassia seed polysaccharide, comprising the following steps:
[0043] Step 1. Under nitrogen atmosphere, add 16.2g cassia polysaccharide, 5.4g N-bromosuccinimide and 0.81g triphenylphosphine to 24.3g N-methyl-2-pyrrolidone, and react at 3°C 15 minutes, then heated up to 60°C, reacted for 3 hours, ethanol precipitation, suction filtration, and repeated washing with ethanol to obtain 14.2 g of brominated cassia polysaccharide;
[0044] Step 2: Under nitrogen atmosphere, add 8g of bromocassia polysaccharide, 4.86g of 4-hydroxycoumarin and 0.64g of sodium carbonate to 14g of dimethyl sulfoxide, react at 45°C for 15h, ethanol precipitation, and wash , and dried to obtain 6.5 g of modified cassia seed polysaccharides, with a yield of 81.3%.
Embodiment 2
[0046] The embodiment of the present invention provides a preparation method of modified cassia seed polysaccharide, comprising the following steps:
[0047] Step 1. Under nitrogen atmosphere, add 16.2g cassia polysaccharide, 8.9g N-bromosuccinimide and 1.3g thiourea to 32.4g N-methyl-2-pyrrolidone, react at 0°C for 30min, then Raise the temperature to 70°C, react for 2.5 hours, ethanol precipitation, suction filtration, and repeated washing with ethanol to obtain 14.6 g of brominated cassia polysaccharide;
[0048] Step 2. Under a nitrogen atmosphere, 8g of bromocassia polysaccharide, 8.8g of 4-hydroxy-6-methylcoumarin and 2.76g of potassium carbonate were added to 16g of dimethyl sulfoxide, and reacted at 60°C for 10h. Precipitate with ethanol, wash and dry to obtain 6.9 g of modified cassia seed polysaccharide with a yield of 86.2%.
Embodiment 3
[0050]The embodiment of the present invention provides a preparation method of modified cassia seed polysaccharide, comprising the following steps:
[0051] Step 1. Under nitrogen atmosphere, add 16.2g cassia polysaccharide, 12.4g N-bromosuccinimide and 1.6g urea to 40.5g N-methyl-2-pyrrolidone, react at 5°C for 20min, then raise the temperature to 80°C, react for 2 hours, ethanol precipitation, suction filtration, and repeated washing with ethanol to obtain 14.9 g of brominated cassia polysaccharide;
[0052] Step 2: Under a nitrogen atmosphere, add 8g of bromocassia polysaccharide, 13.3g of 6-chloro-4-hydroxycoumarin and 2.28g of potassium hydroxide to 15.8g of dimethyl sulfoxide, and react at 75°C for 7h , ethanol precipitation, washing and drying to obtain 7.1 g of modified cassia seed polysaccharide with a yield of 88.7%.
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