Preparation method of phenacetin micropowder

A technology of Xiding micropowder and phenacetin, which is applied in the field of medicine and chemical industry, can solve the problems of narrow particle size distribution, high energy consumption, and low efficiency, and achieve the effects of easy process control, simple production process, and safe operation

Inactive Publication Date: 2017-03-08
HUAZHONG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Although jet milling and ball milling are commonly used methods to reduce the particle size of drugs, they generally have disadvantages such as high energy consumption, low efficiency, wide product particle size distribution, and easy structural damage and degradation of thermally unstable drugs. Will cause problems such as dust pollution and static electricity safety
Although spray drying and supercritical fluid technology can produce micronized drugs with narrow particle size distribution, the cost of equipment is high

Method used

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  • Preparation method of phenacetin micropowder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add 100 g of ethanol to 100 g of phenacetin bulk drug, heat to 78° C., heat and stir to dissolve. Control the stirring rate to 250 rpm, and add the phenacetin ethanol solution to 500 g of purified water at 40° C. while hot. After the dropwise addition, continue to stir for 30 minutes, then lower the temperature to 15°C, stir and crystallize for 2 hours, filter, and dry to obtain 98.8 g of phenacetin micropowder, with a yield of 98.8%, residual ethanol ≤ 0.1%, and a particle size below 120 mesh accounted for 96%.

Embodiment 2

[0023] Add 180 g of ethanol to 100 g of phenacetin bulk drug, heat to 57° C., heat and stir to dissolve. Control the stirring rate at 330 rpm, and add the phenacetin ethanol solution to 900 g of purified water at 35° C. while hot. After the dropwise addition, continue to stir for 30 minutes, then lower the temperature to 20°C, stir and crystallize for 3 hours, filter, and dry to obtain 98.5 g of phenacetin micropowder, with a yield of 98.5%, residual ethanol ≤ 0.1%, and a particle size below 120 mesh accounted for 96%.

Embodiment 3

[0025] Add 200 g of ethanol to 100 g of phenacetin bulk drug, heat to 50° C., heat and stir to dissolve. Control the stirring rate at 350 rpm, and add the phenacetin ethanol solution to 1000 g of purified water at 30°C while it is hot. After the dropwise addition, continue to stir for 30 minutes, then lower the temperature to 24°C, stir and crystallize for 4 hours, filter, and dry to obtain 96.8 g of phenacetin micropowder, with a yield of 96.8%, residual ethanol ≤ 0.1%, and a particle size below 120 mesh Occupy 97%.

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Abstract

The invention discloses a preparation method of phenacetin micropowder. The preparation method comprises steps as follows: (1) ethanol is added to a raw material of phenacetin, and the solution is heated to 50-78 DEG C, kept at the constant temperature and stirred to be dissolved; (2) the stirring rate is controlled between 250 rpm and 350 rpm, the phenacetin ethanol solution is added to purified water at 25-40 DEG C while hot; (3) after addition, the solution is continuously stirred for 30 min, then cooled to 15-30 DEG C and stirred for crystallization for 2-4 h, and the phenacetin micropowder is obtained after filtering and drying. Compared with the prior art, the preparation method has the advantages as follows: 1) the micropowder is uniform in particle and smaller in particle size, and 95% or higher of the micropowder has the particle size of 120 meshes or below; 2) the dissolution rate of the micropowder is obviously increased, the dissolution rate of phenacetin is remarkable increased, and the bioavailability of phenacetin is improved; 3) the preparation method is high in yield, adopts a mild condition, a simple production technology and an easily controllable process and is safe to operate, low in cost and suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of medicine and chemical industry, and relates to a preparation method of phenacetin micropowder. Background technique [0002] Phenacetin, the chemical name is p-acetaminophenethyl ether, the molecular formula is C 10 h 13 NO 2 . Phenacetin is a common bulk antipyretic and analgesic. It was first synthesized by Morse in 1878 and listed in the United States in 1887. It is the first synthetic antipyretic and analgesic on the market. It is often used to treat headaches, Fever, neuralgia, etc. Phenacetin is the main component of compound preparations such as Qutong Tablets and compound aspirin, which are used for antipyretic and analgesic, and to treat colds and colds. The antipyretic effect of phenacetin is stronger than the analgesic effect. The potency is comparable to that of aspirin, with slow and long-lasting action and low toxicity. It has good curative effect on treating headache, neuralgia, arth...

Claims

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Application Information

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IPC IPC(8): C07C231/24C07C233/25
CPCC07C231/24C07C233/25
Inventor 冯旋刘玉亭王勇付林代先朋曾纬田玉林
Owner HUAZHONG PHARMA
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