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Preparation method of high-purity lincomycin hydrochloride

A lincomycin hydrochloride, high-purity technology, applied in the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., can solve problems such as difficult removal, achieve drug safety, simplify process flow, and achieve good economic benefits. Effect

Pending Publication Date: 2021-06-29
TOPFOND PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since there is only one methyl group difference between lincomycin component B and component A, their physical and chemical properties are relatively close, and impurity B is located behind the main peak of lincomycin in the HPLC spectrum, making it more difficult to remove
[0006] CN109481397A discloses a kind of lincomycin hydrochloride injection and its preparation method, but its focus is on reducing the content of lincomycin B in lincomycin hydrochloride injection, and other impurities, especially impurity B, have not been deeply studied. In the implementation case, the content of lincomycin B can be reduced to 1.5%-3.5%, which is still far from the quality of the original research unit Pfizer (T58764 batch impurity B 0.14%, lincomycin B 0.1%)
However, its focus is only on reducing the content of lincomycin B in lincomycin hydrochloride raw materials, and has not studied other impurities, especially impurity B. Through its implementation cases, the content of lincomycin B can be reduced to 1.98%-5.31 %, which is still far behind the quality of the original research unit Pfizer (T58764 batch impurity B 0.14%, lincomycin B 0.1%)

Method used

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  • Preparation method of high-purity lincomycin hydrochloride
  • Preparation method of high-purity lincomycin hydrochloride
  • Preparation method of high-purity lincomycin hydrochloride

Examples

Experimental program
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Effect test

Embodiment 1

[0059] 1) Weigh 16.5kg of potassium dihydrogen phosphate and add 330L of purified water, weigh 390.97kg of lincomycin hydrochloride dry powder, heat up to 72.7°C, keep warm and melt until clarification, slowly add 100kg of sodium chloride, stir and hold at 69.3°C for 35min, then cool down Crystallization, when the temperature drops to 42.7°C, centrifuge and filter at 1500r / min to obtain intermediate wet product 1;

[0060] 2) Put the filtered intermediate wet product 1 back into the dissolution tank, and add 47.62kg / m according to purified water (L): dry powder (wet product is decomposed after moisture detection, kg) = 1:1.128 3 Potassium dihydrogen phosphate, saturated sodium chloride solution, repeat 1) operation step 2 times, obtain 380.9kg lincomycin hydrochloride intermediate wet product 2 altogether.

[0061] 3) Dissolve 380.9kg of lincomycin hydrochloride intermediate wet product 2 in purified water to 64116u / ml, and adjust the pH to 10.27 with 12% NaOH solution;

[00...

Embodiment 2

[0067] 1) Weigh 16.5kg of potassium dihydrogen phosphate and add 330L of purified water, weigh 386.86kg of lincomycin hydrochloride dry powder, heat up to 63.6°C, keep warm and melt until clarified, slowly add 100kg of sodium chloride, stir and hold at 68.3°C for 30min, then cool down Crystallization, when the temperature dropped to 41.2°C, centrifuged at 1500r / min to obtain intermediate wet product 1;

[0068] 2) Put the filtered intermediate wet product 1 back into the dissolution tank according to purified water (L): dry powder (wet product detection moisture is converted to dry, kg) = 1:1.116, add 47.62kg / m 3 Potassium dihydrogen phosphate, saturated sodium chloride solution repeat 1) operation step 3 times, obtain 350.6kg lincomycin hydrochloride intermediate wet product 2 altogether.

[0069] 3) Dissolve 350.6kg of lincomycin hydrochloride intermediate wet product 2 with purified water to 72371u / ml, and adjust the pH to 10.56 with 15% NaOH solution;

[0070] 4) Flow the...

Embodiment 3

[0075] 1) Weigh 16.5kg of potassium dihydrogen phosphate and add 330L of purified water, weigh 397.32kg of lincomycin hydrochloride dry powder, heat up to 78.6°C, keep warm and melt until clarified, slowly add 100kg of sodium chloride, stir and hold at 71.1°C for 30min, then cool down Crystallization, when the temperature drops to 43.5°C, centrifuge and filter at 1500r / min to obtain intermediate wet product 1;

[0076] 2) Put the filtered intermediate wet product 1 back into the dissolving tank according to purified water (L): purified water (L): dry powder (wet product detection moisture converted to dry, kg) = 1:1.146, add 47.62kg / m 3 Potassium dihydrogen phosphate, saturated sodium chloride solution repeat 1) operation step 2 times, obtain 369.8kg lincomycin hydrochloride intermediate wet product 2 altogether.

[0077] 3) Dissolve 369.8kg of lincomycin hydrochloride intermediate wet product 2 in purified water to 59513u / ml, and adjust the pH to 9.78 with 17% NaOH solution; ...

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Abstract

The invention discloses a preparation method of high-purity lincomycin hydrochloride, and belongs to the field of antibiotic extraction and production. According to the invention, lincomycin hydrochloride dry powder is used as a starting material, a salting-out recrystallization method and a macroporous resin adsorption method are combined, the appropriate optimization is carried out, and different polarities oflincomycin hydrochloride A and B components, an impurity B and the likein the salt solution with a certain pH buffer ability and a salting-out recrystallization principle are utilized so as to fulfill the aims of reducing the lincomycin B component, the impurity B and the like and obtain the high-purity lincomycin hydrochloride. The salting-out recrystallization method can effectively reduce the content of impurities such as the impurity B, the lincomycin B component and the like, and macroporous resin adsorption can effectively reduce the content of inorganic salt.

Description

technical field [0001] The invention belongs to the field of antibiotic extraction and production, and specifically relates to a method for preparing high-purity lincomycin hydrochloride. The invention also provides a method suitable for industrial production of high-purity lincomycin hydrochloride. Background technique [0002] Lincomycin, known abroad as Lincomycin (Lincomycin), also known as lincomycin, is a lincosamine-type alkaline antibiotic produced by Streptomyces lincolnensis. Lincomycin and its semi-synthesized downstream product Clindamycin (Clindamycin) is a high-efficiency broad-spectrum antibiotic that has been widely used clinically for many years and has obvious curative effects. It has a strong effect on Gram-positive bacteria and Gram-negative bacteria, and is used for osteomyelitis, sepsis, respiratory system and soft tissue infections. This product has a strong ability to penetrate bone and is the first choice for osteomyelitis. [0003] Lincomycin hydr...

Claims

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Application Information

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IPC IPC(8): C07H1/06C07H15/16
CPCC07H1/06C07H15/16
Inventor 张宏周赖珅朱德育谢书琴张紫阳陈风武妍杰年蓓蕾杨明刘继方任河毅刘学威王岩
Owner TOPFOND PHARMA CO LTD
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