Search

CN-117503724-B - Preparation method of norfloxacin capsule

CN117503724BCN 117503724 BCN117503724 BCN 117503724BCN-117503724-B

Abstract

The invention provides a preparation method of norfloxacin capsules, which comprises the steps of auxiliary material pretreatment, premixing, wet granulation, drying, granule finishing, filling and the like, wherein the prepared norfloxacin capsules have small weight difference, high and stable dissolution rate, accelerated placement for 6 months and stable quality.

Inventors

  • FENG SHENGJUN
  • FENG CHAO
  • WEI JIE
  • GUO FENG
  • JIA LIJUN
  • Pang Shaoxia
  • FENG XINRUI

Assignees

  • 河北君临药业有限公司

Dates

Publication Date
20260505
Application Date
20231130

Claims (6)

  1. 1. The preparation method of the norfloxacin capsule comprises the following steps of (by weight percent) preparing 35% -45% of norfloxacin and 55% -65% of starch; the preparation method comprises the following steps: (1) Pre-treating auxiliary materials; Placing starch in a 50-60 ℃ oven, drying under reduced pressure and vacuum for 4-6 hours, and sieving with a 120-mesh sieve for standby; (2) Premixing and wet granulating: adding norfloxacin and starch into a wet mixing granulator, stirring and premixing, spraying adhesive water under stirring, granulating by wet method, controlling the spraying speed of water, uniformly spraying aqueous solution to ensure that the duration of the spraying aqueous solution is 120-160 seconds, and granulating for 60-110 seconds after spraying; (3) Drying and granulating: Drying at 55-65deg.C, measuring to obtain a dry weight loss not higher than 1.2%, adding the dried granule into a granulator, and sieving with sieve with a pore size of 2.0mm; (4) Filling, namely filling the particles into capsules; Wherein in the step (2), the granularity D 90 of norfloxacin is 20-30 mu m, the granularity D 50 is 12-15 mu m, the adding temperature of the aqueous solution is 32-35 ℃, and the parameters of premixing, spraying the binder solution and granulating are as follows: 。
  2. 2. The method of claim 1, wherein the capsule contents comprise 38% -42% norfloxacin and 58% -62% starch.
  3. 3. The preparation method as claimed in claim 1, wherein the capsule content is 40% norfloxacin and 60% starch.
  4. 4. The process according to claim 1, wherein in step (1), the drying is carried out under reduced pressure at 54 to 57 ℃.
  5. 5. The method of claim 1, wherein in step (4), each capsule contains 0.1g of norfloxacin.
  6. 6. The method of claim 1, wherein in step (4), the content of each capsule weighs 0.25g.

Description

Preparation method of norfloxacin capsule Technical Field The invention belongs to the field of pharmaceutical preparations, and relates to a preparation method of norfloxacin capsules. Background Norfloxacin (Norfloxacin), also known as norfloxacin, is chemically named as 1-ethyl-6-fluoro-1, 4-dihydro-4-oxo-7- (1-piperazinyl) -3-quinolinecarboxylic acid, has a structural formula shown below, is a third-generation quinolone antibacterial agent, can block the action of DNA gyrase (DNAGYRASE) of pathogenic bacteria in the digestive tract, block bacterial DNA replication, and is suitable for urinary tract infection, gonorrhea, prostatitis, intestinal infection, typhoid and other salmonella infections caused by sensitive bacteria. The domestic norfloxacin preparation mainly comprises norfloxacin injection, norfloxacin capsules, norfloxacin tablets, norfloxacin eye drops, norfloxacin ointment and the like, wherein 100mg of norfloxacin capsules are most commonly used, and the most manufacturers have the largest quality difference. The detection analysis of 37 batches of norfloxacin capsules, which are subjected to spot inspection in various regions of the pearl sea in 2016-2021, is carried out by the food and drug inspection institute in the pearl sea market, and shows that the dissolution rate of one batch of norfloxacin capsules is not qualified, and the other batches of norfloxacin capsules meet the limit requirements. However, the quality of norfloxacin capsules produced by different manufacturers is obviously different, even the same batch of norfloxacin capsules produced by the same manufacturer is obviously different, and the dissolution behavior is mainly reflected. The norfloxacin is easy to aggregate in a dissolution medium with pH of 6.8 and water, and the dissolution speed is slow, so that the curative effect of the clinically used norfloxacin capsule cannot be consistent with that of a norfloxacin tablet (reference preparation) of Japanese apricot forest. Therefore, the prescription and the preparation process of the norfloxacin capsule are necessary to be further researched, the dissolution rate of the norfloxacin is improved, the product quality is consistent with that of a reference preparation, and the medication safety and effectiveness are ensured. Disclosure of Invention The inventor of the invention unexpectedly found that the norfloxacin capsule prepared by controlling the particle size of norfloxacin and optimizing the preparation method has small weight difference, high and stable dissolution rate and stable quality, and is placed for 6 months at an accelerated speed. Firstly, the invention provides a preparation method of norfloxacin capsules, wherein the content of the capsules is 35-45% of norfloxacin and 55-65% of starch in percentage by weight, and the preparation method comprises the following steps: (1) Pre-treating auxiliary materials; drying starch in 50-60deg.C oven for 4-6 hr, and sieving with 120 mesh sieve. (2) Premixing and wet granulating: Adding norfloxacin and starch into a wet mixing granulator, stirring and premixing, then carrying out wet granulation by using adhesive water under the stirring condition, controlling the spraying speed of the water, uniformly spraying aqueous solution, enabling the duration of the spraying aqueous solution to be 120-160 seconds, and enabling the granulating time to be 60-110 seconds after the spraying is completed; (3) Drying and granulating: Drying at 55-65deg.C, measuring to obtain a dry weight loss not higher than 1.2%, adding the dried granule into a granulator, and sieving with sieve with a pore size of 2.0mm; (4) Filling, namely filling the granules into capsules. Preferably, the content of the capsule is 38% -42% of norfloxacin and 58% -62% of starch in percentage by weight. More preferably, the content of the capsule is 40% of norfloxacin and 60% of starch in percentage by weight. In step (1), it is preferably 54 to 57 ℃, more preferably vacuum drying under reduced pressure. In the step (2), the adding temperature of the aqueous solution is 32-35 ℃, the weight ratio of the aqueous solution to the norfloxacin is (0.05-0.08), and in the step (2), the granularity D 90 of the norfloxacin is 20-30 mu m, and the granularity D 50 is 12-15 mu m. In the step (2), the parameters of premixing, spraying the binder solution and granulating are as follows: Wherein rpm is revolutions per minute. Further, in the step (4), 0.1g of norfloxacin is contained in each capsule, and the weight of the content in each capsule is 0.25g. The invention optimizes the temperature, the adding time, the granulating time and the like of the aqueous solution of the adhesive by controlling the particle size of the norfloxacin and optimizing the preparation method, and the prepared norfloxacin capsule has small weight difference, high and stable dissolution and stable quality, and is placed for 6 months at an accelerated speed. Detailed Description The invention disc