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Clindamycin palmitate hydrochloridum compound and preparation method thereof

A technology of clindamycin hydrochloride and palmitate, applied in the field of medicine, can solve the problems of low purity of clindamycin hydrochloride palmitate, difficulty in obtaining high purity and high yield of clindamycin hydrochloride palmitate, etc. The effect of reducing toxic and side effects, improving clinical adverse reactions and improving quality

Inactive Publication Date: 2013-01-23
HAINAN YONGTIAN PHARMA INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] In order to overcome the defects of the above-mentioned existing purification technology, especially the defect of low purity of clindamycin hydrochloride palmitate prepared by the prior art, the inventors found that the above-mentioned documents and general purification and separation methods are difficult to obtain through a large number of screening experiments. Clindamycin Hydrochloride Palmitate with High Purity and High Yield

Method used

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  • Clindamycin palmitate hydrochloridum compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Accurately weigh 10 g of clindamycin palmitate hydrochloride with a purity of 92.34% prepared according to the patent GB 1205083, and dissolve it in 100 ml of water. Heat to 50°C, stir to dissolve completely, cool down after 1 hour and perform suction filtration, discard solid impurities, and collect the filtrate.

[0044] Add the obtained filtrate to the top of the packed column, the filler is fine-pored neutral alumina with a particle size of 20-80 μm and a pore size of 6 nm, and the column pressure is 0.08 MPa, and then pump a mixture of chloroform and methanol with a volume ratio of 1:3. The solvent was subjected to column chromatography, the flow rate was 1.0ml / min, and the column temperature was maintained at 40°C. Timing, sampling, tracking and monitoring were started, and segmental collection was carried out to collect the clindamycin hydrochloride palmitate part in the eluent.

[0045] At a temperature of 65°C, add 0.005M dilute hydrochloric acid aqueous soluti...

Embodiment 2

[0049] Accurately weigh 10 g of clindamycin palmitate hydrochloride bulk drug (Sichuan Creed Pharmaceutical Co., Ltd., H20083170) (purity 94.87%), and dissolve it in 150 ml of methanol. Heat to 50°C, stir to dissolve completely, cool down after 1 hour and carry out suction filtration, discard solid impurities, and collect the filtrate.

[0050] Add the obtained filtrate to the top of the packed column, the filler is fine-pored neutral alumina with a particle size of 100-220 μm and a pore size of 6 nm, and the column pressure is 0.15 MPa, and then pump a mixture of chloroform and methanol with a volume ratio of 1:2. The solution was dissolved for column chromatography, the flow rate was 2.5ml / min, and the column temperature was maintained at 50°C. Timing, sampling, tracking and monitoring were started, and segmental collection was carried out to collect clindamycin hydrochloride palmitate in the eluate.

[0051] At a temperature of 68°C, add 0.01M dilute hydrochloric acid aqueo...

Embodiment 3

[0053] Accurately weigh 10 g of clindamycin palmitate hydrochloride bulk drug (Chongqing Kailin Pharmaceutical Co., Ltd., H20057714) (purity 93.66%), and dissolve it in 120 ml of a mixed solvent of chloroform and methanol with a volume ratio of 1:2. Heat to 45°C, stir to dissolve completely, cool down after 1 hour and filter with suction, discard solid impurities, and collect the filtrate.

[0054] Add it to the top of the packed column. The filler is fine-pored neutral alumina with a particle size of 180-300 μm and a pore size of 6 nm. For analysis, the flow rate was 2ml / min, and the column temperature was maintained at 45°C. Start timing, sampling, follow-up monitoring, segmental collection, and collect the clindamycin hydrochloride palmitate part in the eluent.

[0055] At a temperature of 66°C, add 0.05M dilute hydrochloric acid aqueous solution to the obtained clindamycin palmitate hydrochloride solution, adjust the pH value between 5-6, and lower the temperature to 45-50...

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Abstract

The invention discloses a high-purity clindamycin palmitate hydrochloridum compound with the following structural formula and additionally relates to a preparation method of the clindamycin palmitate hydrochloridum compound. The preparation method comprises the following steps of: 1) dissolving the clindamycin palmitate hydrochloridum in solvent, heating in any way, cooling, conducting suction filtration and abandoning solid impurities to obtain the filtrate of the clindamycin palmitate hydrochloridum; 2) loading samples through column chromatography, using eluent for elution, collecting the part of the clindamycin palmitate hydrochloridum in the eluent; and 3) at temperature being not higher than 70 DEG C, adding diluted hydrochloric acid aqueous solution in the eluent containing the clindamycin palmitate hydrochloridum to adjust pH value, decreasing temperature in a gradient way for recrystallization and drying to obtain the clindamycin palmitate hydrochloridum. By adopting the preparation method disclosed by the invention, the quality of preparation products is improved, the toxic and side effects are reduced and the large-scale industrialized production is realized.

Description

technical field [0001] The invention relates to a high-purity clindamycin hydrochloride palmitate compound and a preparation method thereof, belonging to the technical field of medicine. Background technique [0002] Clindamycin Palmitate Hydrochloridum, chemical name 6-(1-methyl-trans-4-propyl-L-2-pyrrolidinecarboxamido)-1-thio-7(S )-Chloro-6,7,8-trideoxy-L-threo-α-D-galactopyranoside 2-palmitate hydrochloride, molecular formula C 34 h 63 ClN 2 o 6 S.HCl, molecular weight 699.87, structural formula: [0003] [0004] Clindamycin palmitate hydrochloride is a derivative of clindamycin, which has no antibacterial activity in vitro, but is hydrolyzed by esterase to form clindamycin in vivo to exert antibacterial activity. The mechanism of action of clindamycin is to inhibit bacterial cell wall Synthesis. [0005] Clinically, clindamycin hydrochloride palmitate is mainly used for the following infectious diseases caused by Gram-positive bacteria, tonsillitis, suppurativ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H15/16C07H1/00
Inventor 陶灵刚
Owner HAINAN YONGTIAN PHARMA INST
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