Purification method of acetyl pullulan polysaccharide folate conjugate and preparation method of nanometer particles thereof

A technology of pullulan polysaccharide folic acid and pullulan polysaccharide, which is applied in the directions of non-active ingredients such as medical preparations, pharmaceutical formulations, powder delivery, etc., to achieve the effects of stable structure, controllable preparation conditions and small particle size distribution range.

Inactive Publication Date: 2010-09-15
INST OF BIOMEDICAL ENG CHINESE ACAD OF MEDICAL SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the present invention, on the basis of previous studies, the product is precipitated with conventional reagent absolute ethanol, and sodium carbonate buffer is dialyzed to separate and purify. In addition, the nanoparticle prepared from this material is used as a drug carrier by dialysis. None of the above studies See any literature or patent reports

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  • Purification method of acetyl pullulan polysaccharide folate conjugate and preparation method of nanometer particles thereof
  • Purification method of acetyl pullulan polysaccharide folate conjugate and preparation method of nanometer particles thereof
  • Purification method of acetyl pullulan polysaccharide folate conjugate and preparation method of nanometer particles thereof

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Embodiment 1

[0024] Example 1: Precipitation and purification method of folic acid acetyl pullulan conjugate:

[0025] Dissolve 1g (2.27mmol) of folic acid in 15ml of dimethyl sulfoxide (DMSO), dropwise add 5 drops of triethylamine, stir to dissolve completely, add 0.9g (4.4mmol) of N,N'-dicyclohexylcarbodiethylene Amine (DCC), 0.25g (2.05mmol) 4-dimethylaminopyridine (DMAP), stirred for 1 hour, then added 0.615g of acetyl pullulan dissolved in 6.15ml of DMSO, and reacted in the dark for 5 days under electromagnetic stirring. Remove the DCU precipitate by filtration, add the filtrate dropwise to 250ml of absolute ethanol solution, centrifuge (8000 rpm, 4°C, centrifuge for 15min) to collect the yellow precipitate, dialyze in sodium carbonate buffer for 24h, dialyze in deionized water for 48h, freeze-dry or vacuum After drying, a yellow powder is obtained, which is a folic acid-coupled acetyl pullulan derivative.

[0026] The proton magnetic spectrum ( 1 H-NMR) is basically consistent with...

Embodiment 2

[0027] Embodiment 2: the preparation of FPA nanoparticle

[0028] Accurately weigh 48 mg of acetyl pullulan polysaccharide folic acid conjugate and dissolve it in 4.8 ml of dimethyl sulfoxide at a concentration of 10 mg / ml. Transfer the solution to a dialysis bag for dialysis. The molecular weight cut-off of the dialysis bag is 14000 Da, and the dialysate is For deionized water, change the water every 1-2 hours at the beginning, change it 4 times, and then change the water every 4-6 hours, for a total of 48 hours of dialysis. The final solution is a solution with yellow opalescence, which is transferred to a graduated centrifuge tube, and after 100W ultrasound for 3 minutes, it is the final nanoparticle suspension, and the final concentration is the volume of the added material (48mg) and the final nanoparticle solution ( 12ml) than 4mg / ml. According to the needs of the experiment, it can be diluted with water or other solutions to the target concentration, or the nanoparticl...

Embodiment 3

[0029] Embodiment 3: the preparation of the FPA nanoparticle that packs epirubicin

[0030] Accurately weigh 40 mg of acetyl pullulan folic acid conjugate, and dissolve it in 3.2 ml of dimethyl sulfoxide to make the concentration 12.5 mg / ml. Dissolve 10 mg of epirubicin in 2 ml of dimethyl sulfoxide at a concentration of 5 mg / ml, add 4.9 μl of triethylamine (2 times the molar amount), and stir at room temperature for 12 hours in the dark to dehydrochloride the epirubicin. Mix the drug / material solution at a volume ratio of 4:1, transfer the solution to a dialysis bag for dialysis, the molecular weight cut-off of the dialysis bag is 10,000 Da, and the dialysate is deionized water. Change the water once every 1 to 2 hours, and change it 4 times Afterwards, the water was changed every 4 to 6 hours for a total of 48 hours of dialysis. The final solution is an orange-red opalescent solution, which is transferred to a graduated centrifuge tube. After 100W ultrasonication for 3 minu...

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Abstract

The invention relates to a purification method of acetyl pullulan polysaccharide folate conjugate and a preparation method of nanometer particles thereof. Folate, acetyl pullulan polysaccharide solution, 4-dimethylaminopyridine (DMAP) and a carbodiimide dehydrating agent are mixed for reaction for 5 to 7 days at the temperature of 25 to 28 DEG C, excessive absolute ethyl alcohol is dropwise added into filter liquor for sedimentation, and centrifugation is carried out, the sediment is collected, is dialyzed for 24 to 48 hours by sodium carbonate buffer solution and is dialyzed for 24 to 48 hours in deionized water, and a material is obtained through freezing-drying or vacuum drying. The material is dissolved in dimethyl sulfoxide (DMSO) or other organic solvents, and a dialysis method is adopted for preparing the nanometer particles. The invention has less steps, simple operation and good repeatability and dose not need other stabilizing agents and emulsifiers, and the nanometer particles are in ball shapes, have uniform grain sizes, low absolute potential, and good stability, and do not have significant toxicity for single mainline to mice.

Description

Technical field: [0001] The invention relates to the purification of acetyl pullulan polysaccharide folic acid conjugate (Folate-conjugated pullulan acetate, FPA) and the preparation method of nano-particles (Folate-conjugated pullulan acetate nanoparticles, FPAN). Background technique: [0002] Nano-drug carrier refers to a nanoscale system that can change the way the drug enters the human body and its distribution in the body, controls the release rate of the drug and delivers the drug to the target organ. The ideal drug delivery carrier has the following characteristics (Wim H DeJong, et al., Int J Nanomedicine. 2008, 3(2): 133-149; S.M. Moghimi, et al., FASEB J. 2005, 19(3): 311-330; Karina R, et al., Adv Drug Deliv Rev.2008, 60(8): 929-938): It can encapsulate and release drugs well, has stable structure, good biocompatibility, low toxicity, and has biodistribution and targeting capabilities and effects. In addition, Good biodegradability after drug delivery is also re...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B37/00A61K47/36A61K9/14
Inventor 张其清唐红波李学敏刘玲蓉张彤李磊白永刚周志敏
Owner INST OF BIOMEDICAL ENG CHINESE ACAD OF MEDICAL SCI
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