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Alprostadil compound and preparation method thereof

A kind of technology of alprostadil and compound, applied in the field of high-purity alprostadil compound and its preparation method, can solve the problems of low purity of alprostadil, achieve the effect of improving clinical adverse reactions, easy to control and industrialized production

Inactive Publication Date: 2013-03-06
HAINAN MEILAN SMITH KLINE PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In order to overcome the defects of the above-mentioned prior art, especially overcome the defect of low purity of alprostadil prepared by the prior art, the invention provides a kind of preparation method of high-purity alprostadil compound

Method used

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  • Alprostadil compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Get 10g alprostadil crude product, the content of alprostadil recorded by high performance liquid chromatography is 80%, this alprostadil crude product is dissolved in 100ml ethanol, then adds 0.1g sodium bisulfate, 50 ℃ of insulated and stirred 20 minutes, Filtrate, abandon solid impurity, obtain the filtrate containing alprostadil.

[0037] Add the obtained filtrate to a silica gel column for separation and purification, and use a particle size of 45-250 μm and a pore size of fine-pored silica gel. The mobile phase is a mixed solution of pH5.6 phosphate buffer solution and methanol with a volume ratio of 3:7, a flow rate of 0.5-2ml / min, a column temperature of 30-40°C, and a wavelength of 245nm. Collect the alprostadil parts in the eluate, mainly combine the fractions with a drug content greater than 90%, and concentrate the eluate under reduced pressure at 40-50°C.

[0038] The above concentrated solution was heated to a temperature of 55-60° C. and kept for half ...

Embodiment 2

[0042] Get 10g alprostadil crude product, the content of alprostadil recorded by high performance liquid chromatography is 82%, this alprostadil crude product is dissolved in 200ml ethanol, then adds 0.5g sodium dihydrogen phosphate, 50 ℃ of insulated and stirred 15 minutes , filter, discard the solid impurities, and obtain the filtrate containing alprostadil.

[0043] Add the obtained filtrate to a silica gel column for separation and purification, and use a particle size of 85-220 μm and a pore size of fine-pored silica gel. The mobile phase is a mixed solution of phosphorus pH5.6 salt buffer solution and methanol with a volume ratio of 3:7, the flow rate is 1.0-2ml / min, the column temperature is 35-40°C, and the wavelength is 245nm. Collect the alprostadil parts in the eluate, mainly combine the fractions with a drug content greater than 93%, and concentrate the eluate under reduced pressure at 40-50°C.

[0044] The above concentrated solution was raised to a temperature...

Embodiment 3

[0046] Get 10g alprostadil crude product, the content of alprostadil recorded by high performance liquid chromatography is 81%, this alprostadil crude product is dissolved in 150ml ethanol, then adds 0.3g sodium dihydrogen phosphate, 45 ℃ of insulated and stirred 40 minutes , filter, discard the solid impurities, and obtain the filtrate containing alprostadil.

[0047] Add the obtained filtrate to a silica gel column for separation and purification, and use a particle size of 75-200 μm and a pore size of fine-pored silica gel. The mobile phase is a mixed solution of pH5.6 phosphate buffer solution and methanol with a volume ratio of 3:7, the flow rate is 1.5-2ml / min, and the column temperature is 30-40°C. Collect the alprostadil parts in the eluate, mainly combine the fractions with a drug content greater than 90%, and concentrate the eluate under reduced pressure at 40-50°C.

[0048] The above concentrate was heated to a temperature of 57-60° C. and kept for 50 minutes. A...

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Abstract

The invention relates to a high-purity alprostadil compound with the structural formula in the specification, and a preparation method for the alprostadil compound. The preparation method comprises the following steps of: 1) dissolving alprostadil in ethanol, treating by using an acid salt substance, and filtering; 2) separating and purifying filtrate by using a chromatographic column, collecting an alprostadil part in eluent, and concentrating under reduced pressure to obtain an n alprostadil-containing solution; 3) heating the obtained solution, keeping for a certain period of time, adding acetonitrile, cooling in a gradient way for recrystallization, and drying to obtain the purified alprostadil compound. The alprostadil prepared by the method has the purity of not lower than 99.5 percent, and has low heavy metal content. By the method, the quality of a preparation product is improved, the toxic and side effects are reduced, and the method is suitable for industrial production.

Description

technical field [0001] The invention relates to a high-purity alprostadil compound and a preparation method thereof, belonging to the technical field of medicine. Background technique [0002] Alprostadil, also known as prostaglandin E 1 (prostaglandin E 1 , PGE 1 ), a natural PG substance. Its chemical name: (1R, 2R, 3R)-3-hydroxy-2(E)-(3S)-3-hydroxy-1-octenyl-5-oxocyclopentane heptanoic acid, the molecular formula is C 20 h 34 o 5 , molecular weight is 354.48, structural formula: [0003] [0004] Alprostadil has a wide range of biological effects, mainly including expansion of vascular smooth muscle, anti-platelet aggregation and cytoprotection, and contraction of pregnant uterine smooth muscle. Clinically, it can be used to prevent and treat various cardiovascular diseases (including hypertension, coronary heart disease, hyperlipidemia, etc.) , has the characteristics of small dosage and small scraping effect. [0005] The synthetic route of alprostadil used ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C405/00
Inventor 杨明贵
Owner HAINAN MEILAN SMITH KLINE PHARMA
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