Green and efficient preparation method of cynanchum bungei short sugar chain C21 steroid glycoside
A technology of Radix Polygoni Multiflori and steroidal glycosides, applied in chemical instruments and methods, catalyst activation/preparation, glycoside steroids, etc., can solve the problems of serious environmental pollution and difficulty in controlling the degree of hydrolysis, and achieve reduced environmental pollution, controllable reactions, product controllable effect
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Embodiment 1
[0027] Fe 3 o 4 @SiO 2 Preparation of nanoparticles immobilized carrier:
[0028] Fe was first prepared by a modified hydrothermal method 3 o 4 nanoparticles. Dissolve 1.2g of ferric chloride and 2.0g of sodium acetate in a beaker, add them into 20mL of ethylene glycol, stir well until the solution turns clear yellow, transfer to a polytetrafluoroethylene reactor, and react at 200°C for 12h. The magnetic nanoparticles were separated under an external magnetic field, washed several times with deionized water and ethanol, and dried in vacuum to obtain Fe 3 o 4 Nanoparticles.
[0029] Then Fe was prepared by sol-gel method 3 o 4 @SiO 2 nanoparticles. Take 0.5g of prepared Fe 3 o 4 Nanoparticles, 30mL distilled water, 100mL ethanol and 2mL ammonia water were placed in a 250mL three-necked round-bottomed flask, then 5mL tetraethyl silicate was added to 20mL ethanol, and then their mixture was added dropwise to the above reaction system, Continue to react at room tempe...
Embodiment 2
[0031] Weigh 0.5g Fe 3 o 4 @SiO 2 Nanoparticles and 30mL distilled water were placed in a 250mL three-necked round-bottomed flask. After the system was dispersed, 0.5g of acidic ionic liquid [Bmim][HSO 4 ] was dissolved in 20mL of ethanol, added dropwise to the above reaction system, and continued to react at 60°C for 2h. After the reaction, the nanoparticles were magnetically separated, washed several times with deionized water and ethanol, and dried in vacuum to obtain the immobilized ionic liquid nanoparticles.
[0032] After fully dissolving 0.5 g of Radix Polygoni Multiflori C21 steroidal glycosides with 10 mL of 70% ethanol aqueous solution, 0.5 g of immobilized ionic liquid nanoparticles were added, and hydrolyzed at 50° C. for 4 h. After the reaction is completed, the nanoparticles are magnetically separated, and the hydrolyzed product is concentrated and dried to obtain the short sugar chain C21 steroidal glycoside of Radix Polygoni Multiflori. Through high-perfor...
Embodiment 3
[0034] Weigh 0.5g Fe 3 o 4 @SiO 2 Nanoparticles and 30mL distilled water were placed in a 250mL three-necked round-bottomed flask. After the system was dispersed, 0.5g of acidic ionic liquid [Hmim][HSO 4 ] was dissolved in 20mL of ethanol, added dropwise to the above reaction system, and continued to react at 60°C for 2h. After the reaction, the nanoparticles were magnetically separated, washed several times with deionized water and ethanol, and dried in vacuum to obtain the immobilized ionic liquid nanoparticles.
[0035]After fully dissolving 0.5 g of Radix Polygoni Multiflori C21 steroidal glycosides with 10 mL of 70% ethanol aqueous solution, 0.5 g of immobilized ionic liquid nanoparticles were added, and hydrolyzed at 60° C. for 3 h. After the reaction is completed, the nanoparticles are magnetically separated, and the hydrolyzed product is concentrated and dried to obtain the short sugar chain C21 steroidal glycoside of Radix Polygoni Multiflori. Through high-perform...
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