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Sitafloxacin dihydrate crystal, and preparation method and composition tablet thereof

A technology of sitafloxacin and dihydrate, applied in the field of medicine, can solve the problems of inability to obtain antibacterial effect, slow dissolution, insoluble in water, etc., and achieves high tablet dissolution rate and bioavailability, simple process and stable good effect

Active Publication Date: 2017-05-31
SHANDONG YUXIN PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, since sitafloxacin is extremely difficult to dissolve in water, the tablet prepared by using the existing crystal form dissolves slowly in the body after oral administration, and it is difficult to achieve complete dissolution, resulting in a decrease in the bioavailability of the drug, and the ideal antibacterial effect cannot be achieved. Effect

Method used

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  • Sitafloxacin dihydrate crystal, and preparation method and composition tablet thereof
  • Sitafloxacin dihydrate crystal, and preparation method and composition tablet thereof
  • Sitafloxacin dihydrate crystal, and preparation method and composition tablet thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Embodiment 1: Preparation of sitafloxacin dihydrate crystal form

[0034] 1) Dissolve 1 kg of sitafloxacin crude product in 3 kg of absolute ethanol, 2 kg of anhydrous acetone and 5 kg of deionized water, and heat to reflux to obtain solution A;

[0035] 2) Cool down to 40°C-50°C, add 25g of activated carbon, stir for 30 minutes to obtain solution B, cool down to 20-25°C for crystallization for 1 hour, and grow crystal for 3 hours;

[0036] 3) Rinse with 2kg of absolute ethanol to obtain a white solid;

[0037] 4) Put the solid obtained in step 3) in a vacuum drying oven, vacuumize the system, and dry at 30° C. to constant weight to obtain the crystal form of sitafloxacin dihydrate.

[0038] The X-ray powder diffraction spectrogram (see figure 1 ) at 2θ of 3.7°, 5.3°, 10.3°, 11.5°, 15.3°, 16.8°, 17.7°, 19.8°, 21.7°, 24.8°, 27.6°, 30.6°, 34.1°, and 39.8° .

[0039] Elemental analysis:

[0040] Measured values: C51.21%, H4.98%, Cl7.97%, F8.51%, N9.45%, O17.95%.

[0...

Embodiment 2

[0044] Embodiment 2: Preparation of sitafloxacin dihydrate crystal form

[0045] 1) Dissolve 1 kg of sitafloxacin crude product in 8 kg of absolute ethanol, 5 kg of anhydrous acetone and 10 kg of deionized water, and heat to reflux to obtain solution A;

[0046] 2) Cool down to 40°C-50°C, add 25g of activated carbon, stir for 30 minutes, filter to obtain solution B, cool down to 20-25°C for crystallization for 1 hour, and grow crystals for 6 hours;

[0047] 3) Rinse with 3kg of absolute ethanol to obtain a white solid;

[0048] 4) Put the solid obtained in step 3) in a vacuum drying oven, vacuumize the system, and dry at 40° C. to constant weight to obtain the sitafloxacin dihydrate crystal form.

[0049] According to the XPRD data, the obtained crystal form is consistent with the crystal form in Example 1. The thermogravimetric analysis spectrum obtained by using the PEPyrisDiamondTG thermogravimetric analyzer of Perkin-Elmer Company of the United States is consistent with ...

Embodiment 3

[0050]Embodiment 3: Preparation of sitafloxacin dihydrate crystal form

[0051] 1) Dissolve 1 kg of sitafloxacin crude product in 5 kg of absolute ethanol, 3 kg of anhydrous acetone and 20 kg of deionized water, and heat to reflux to obtain solution A;

[0052] 2) Cool down to 40°C-50°C, add 25g of activated carbon, stir for 30 minutes, filter to obtain solution B, cool down to 20-25°C for crystallization for 1 hour, and grow crystals for 12 hours;

[0053] 3) Rinse with 5kg of absolute ethanol to obtain a white solid;

[0054] 4) The solid obtained in step 3) is placed in a vacuum drying oven, the system is evacuated, and dried at 50° C. to constant weight to obtain the crystal form of sitafloxacin dihydrate.

[0055] According to the XPRD data, the obtained crystal form is consistent with the crystal form in Example 1. The thermogravimetric analysis spectrum obtained by using the PEPyrisDiamondTG thermogravimetric analyzer of Perkin-Elmer Company of the United States is co...

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Abstract

The invention belongs to the technical field of medicines, and particularly relates to a sitafloxacin dihydrate crystal, and a preparation method and a composition tablet thereof. The preparation method of the sitafloxacin dihydrate crystal provided by the invention comprises the dissolving and crystallizing steps. The invention further provides a composition containing the sitafloxacin dihydrate crystal; the sitafloxacin dihydrate crystal as an active component comprises the following components in percent by weight: 32-33% of sitafloxacin dihydrate, 38-39% of mannitol, 19-20% of starch, 6-7% of hydroxy propyl cellulose, 1.3-1.4% of hydroxypropyl methyl cellulose and 0.9-1% of magnesium stearate; and a method for preparing the sitafloxacin tablet comprises the following steps of crushing, sieving, granulating, drying, granulating, totally mixing, tableting and the like. Compared with the prior art, the sitafloxacin tablet prepared through the method provided by the invention has the advantages of improved dissolvability and bioavailability.

Description

technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to a crystal form of sitafloxacin dihydrate, a preparation method and a composition tablet thereof. Background technique [0002] Sitafloxacin (sitafloxacin), the chemical name is 7-[(7S)-amino-5-azaspiro[2.4]hept-5-yl]-8-chloro-6-fluoro-1-[(1R,2S )-cis-2-fluorocyclopropyl]-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid is a fluoroquinolone antibacterial drug developed by Japan’s Daiichi Pharmaceutical Company, which is clinically used 3 / 2 hydrate. Sitafloxacin is a new oral N-1-fluorocyclopropyl new quinolone antibacterial drug with broad-spectrum antibacterial activity, which is effective against aerobic or anaerobic Gram-positive bacteria and Gram-negative bacteria, and Chlamydia have broad-spectrum antibacterial effect. The sitafloxacin compound has three chiral carbon atoms, and has 1 enantiomer and 6 diastereoisomers. Determining the absolute configuration of it...

Claims

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Application Information

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IPC IPC(8): C07D401/04A61K31/4709A61K9/20A61P31/04
CPCA61K9/2059C07B2200/13C07D401/04
Inventor 刘新泉王超孙运贝
Owner SHANDONG YUXIN PHARMA CO LTD
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