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A kind of preparation method of b component reference substance in lincomycin hydrochloride

A technology of lincomycin hydrochloride and reference substances, which is applied in the preparation of test samples, analysis materials, sampling, etc., can solve the problems that the preparation method of lincomycin B component has not been mentioned, and achieve simple operation , easy to realize, and low preparation cost

Active Publication Date: 2020-09-08
XINYU PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In recent years, there have been many studies on the purification method of lincomycin A component, such as Chinese patents CN105111254A, CN106518936A and CN104356179A; but there is no mention of the research on the preparation method of lincomycin B component

Method used

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  • A kind of preparation method of b component reference substance in lincomycin hydrochloride
  • A kind of preparation method of b component reference substance in lincomycin hydrochloride
  • A kind of preparation method of b component reference substance in lincomycin hydrochloride

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Embodiment 1

[0029] The present invention provides a kind of preparation method of B component reference substance in lincomycin hydrochloride, comprising the following steps:

[0030] S1. Dissolve 400 g of lincomycin hydrochloride with a component B content of 4.0% in 4 L of purified water, and use WZ-17 resin column for adsorption, and the volume of the resin column is 3.5 L;

[0031] S2. After the adsorption is completed, wash with water at a flow rate of 0.5BV / h for 2 hours to remove impurities;

[0032] S3. Dissolve 36 g of lincomycin hydrochloride with a content of 0.6% in component B in 360 mL of purified water, and use a resin column to absorb and wash at the top;

[0033] S4. After the adsorption top washing is completed, wash with water at a flow rate of 0.5BV / h for 1 hour, and collect the washing water;

[0034] S5. Separating and purifying the collected washing water with a secondary resin, the secondary resin is WZ-17, and the volume of the resin is 750mL; 14h to remove unkn...

Embodiment 2

[0039] The present invention provides a kind of preparation method of B component reference substance in lincomycin hydrochloride, comprising the following steps:

[0040] S1. Dissolve 400 g of lincomycin hydrochloride with a component B content of 4.0% in 4 L of purified water, and use an LX-1500 resin column for adsorption, and the volume of the resin column is 3 L;

[0041] S2. After the adsorption is completed, wash with water at a flow rate of 0.5BV / h for 2 hours to remove impurities;

[0042] S3. Dissolve 36 g of lincomycin hydrochloride with a content of 0.6% in component B in 360 mL of purified water, and use a resin column to absorb and wash at the top;

[0043] S4. After the adsorption top washing is completed, wash with water at a flow rate of 0.5BV / h for 1 hour, and collect the washing water;

[0044] S5. Separating and purifying the collected washing water with a secondary resin, the secondary resin is LX-1500, and the volume of the resin is 700mL; Remove unknow...

Embodiment 3

[0049] The present invention provides a kind of preparation method of B component reference substance in lincomycin hydrochloride, comprising the following steps:

[0050] S1. Dissolve 400 g of lincomycin hydrochloride with a component B content of 4.0% in 4 L of purified water, and use an XAD-18 resin column for adsorption. The volume of the resin column is 2.8 L;

[0051] S2. After the adsorption is completed, wash with water at a flow rate of 0.5BV / h for 2 hours to remove impurities;

[0052] S3. Dissolve 36 g of lincomycin hydrochloride with a content of 0.6% in component B in 360 mL of purified water, and use a resin column to absorb and wash at the top;

[0053] S4. After the adsorption top washing is completed, wash with water at a flow rate of 0.5BV / h for 1 hour, and collect the washing water;

[0054] S5. Separation and purification of the collected washing water by secondary resin, the secondary resin is XAD-18, and the resin volume is 650mL; after the adsorption is...

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Abstract

The invention discloses a preparation method of a B component reference substance in lincomycin hydrochloride. The preparation method comprises the following steps: dissolving lincomycin hydrochlorideof which the content of B component is greater than or equal to 3.0 percent into water and absorbing with a resin column; washing and removing impurities; adsorbing the lincomycin hydrochloride solution of which the content of the B component is smaller than or equal to 0.7 percent by using the resin column; washing and collecting washing water after the adsorption is finished; carrying out second-time resin separation and purification, pre-washing with a solvent, removing impurities and then desorbing with the solvent and collecting a desorption solution; concentrating the collected desorption solution and discharging to obtain lincomycin hydrochloride B component wet powder; carrying out centrifugal treatment on the lincomycin hydrochloride B component wet powder and then pulping for 0.5 hour; drying the lincomycin hydrochloride B component wet powder under vacuum conditions to obtain a lincomycin hydrochloride B component reference substance with the purity of 98 percent or above.The resin separation and purification method disclosed by the invention for preparing lincomycin hydrochloride B component reference substance has the advantages of low preparation cost, simple operation and easiness in realization.

Description

technical field [0001] The invention relates to the technical field of medicinal chemistry, in particular to a method for preparing a component B reference substance in lincomycin hydrochloride. Background technique [0002] Lincomycin hydrochloride is an alkaline spectrum antibiotic that is effective against most Gram-positive bacteria and is clinically used for the treatment of infections caused by Staphylococcus aureus, Streptococcus viridans, and Streptococcus pneumoniae. Lincomycin hydrochloride is an antibiotic that is mainly isolated through microbial fermentation and culture. Its molecular structure has multiple chiral centers and multiple isomers. During the fermentation process of lincomycin hydrochloride, in addition to mainly producing lincomycin A component, a small amount of by-product lincomycin B component and other components are also produced. [0003] In recent years, there have been many studies on the purification method of lincomycin A component, such ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N1/28G01N1/34G01N1/40
CPCG01N1/28G01N1/34G01N1/4022G01N2001/2893
Inventor 丁振东王珍许计强朱雅琪
Owner XINYU PHARM CO LTD