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Method for preparing kanamycin monosulfate single crystal and application thereof

A technology of kanamycin monosulfate and single crystal, which is applied in the field of medicine and can solve the problems of inconvenient storage and transportation

Pending Publication Date: 2022-07-22
北京市药品检验研究院(北京市疫苗检验中心)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The water solubility of kanamycin sulfate is obviously higher than that of monosulfate kanamycin, yet, the solid bulk drug kanamycin sulfate (C 18 h 36 N 4 o 11 ·xH 2 SO 4 ) Although commonly used in the preparation of various preparations, this kanamycin sulfate (C 18 h 36 N 4 o 11 ·xH 2 SO 4 ) has extremely strong hygroscopicity and is inconvenient for storage and transportation, so some enterprises are more inclined to produce and use kanamycin monosulfate (C 18 h 36 N 4 o 11 ·H 2 SO 4 ) is transported and stored as a solid raw material, and the amount of sulfuric acid is adjusted to meet the formulation requirements during preparation production. In this sense, it will become a trend for domestic kanamycin raw materials to use its monosulfate

Method used

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  • Method for preparing kanamycin monosulfate single crystal and application thereof
  • Method for preparing kanamycin monosulfate single crystal and application thereof
  • Method for preparing kanamycin monosulfate single crystal and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0092] Example 1. Preparation of single crystal of kanamycin monosulfate

[0093] The present embodiment prepares the single crystal of kanamycin monosulfate, and the operation steps are as follows:

[0094] (1) Take 1000 mg of kanamycin monosulfate bulk drug, put it in a 50 ml Nessler colorimetric tube, add 20 ml of decarbonated water to dissolve, measure the pH value and adjust the pH value of the solution to 6.0~6.2 with 1M sulfuric acid solution , then add 1ml of isopropanol to mix;

[0095] (2) 10ml methanol is slowly added from the liquid level of the solution obtained in step (1) at a speed of 2ml / min under the temperature condition of 22~25°C;

[0096] (3) stand for 24 hours under the above-mentioned temperature conditions, precipitate columnar crystals, and take out. The obtained crystal may be referred to as kanamycin A monosulfate in the present invention.

[0097] The decarbonated water used was water obtained by boiling double-distilled water for 10 minutes a...

Embodiment 2

[0098] Example 2. Determination of kanamycin monosulfate crystals by single crystal X-ray diffraction (XRD)

[0099] In this example, a single crystal X-ray diffractometer (XRD) was used to measure the columnar crystals of kanamycin monosulfate obtained in Example 1 to prove its crystal structure.

[0100] According to the analysis of the collection of kanamycin monosulfate in the pharmacopoeia of various countries, including ChP2000 version, USP39, EP8.0, BP2016 and JP16, the difference of water molecules in the molecular formula of kanamycin monosulfate is recorded in this example. The kanamycin monosulfate crystals obtained by culture were measured by a single crystal X-ray diffractometer, the molecular formula of the obtained kanamycin monosulfate crystals was verified, and the absolute configuration, Conformation, unit cell, hydrogen bond and salt bond arrangement within unit cell.

[0101] Sample: the columnar crystal of kanamycin monosulfate obtained in Example 1, th...

Embodiment 3

[0132] Example 3. Consistency proof of kanamycin monosulfate single crystal and kanamycin monosulfate raw material crystal

[0133] In this example, the consistency of the crystals of the kanamycin monosulfate crystal obtained in Example 1 (kanamycin monosulfate A, single crystal) and the used kanamycin monosulfate raw material drug is verified.

[0134] 1. Electron microscope

[0135] Preliminary inspection was carried out by optical polarizing microscope, which proved that the commercial kanamycin monosulfate bulk drug had crystallinity. After recrystallization in Example 1, a new crystal (kanamycin monosulfate A) was obtained. The properties of the crystals were observed under a cold field emission scanning electron microscope. Figure 5 The electron microscope crystal structure of kanamycin monosulfate.

[0136] 2. Powder X-ray Diffraction

[0137] In order to further confirm the crystallinity of kanamycin monosulfate, the powder X-ray diffraction patterns of the raw ...

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Abstract

The invention relates to a method for preparing a kanamycin monosulfate single crystal and application thereof. Specifically, on one hand, the invention also relates to a single crystal form of a compound in the following formula, the single crystal form is a triclinic system, and the cell parameters are alpha = 88.48 (1) degrees, beta = 85.21 (1) degrees, and gamma = 89.19 (1) degrees. The invention also relates to a method for detecting the quality of the single crystal form, a method for preparing the single crystal form, and application of the single crystal form to identification of kanamycin monosulfate bulk drugs. The method disclosed by the invention has excellent effects as described in the specification.

Description

technical field [0001] The invention belongs to the technical field of medicine, and relates to a method for preparing kanamycin monosulfate crystals, in particular to a method for preparing kanamycin monosulfate single crystals, and also to the use of the single crystals in the pharmaceutical industry, which is used in commercially available Use of kanamycin sulfate monosulfate especially in molecular structure. Background technique [0002] Aminoglycoside antibiotics mainly have strong antibacterial effects on Staphylococcus aureus and aerobic gram-negative bacilli, including Pseudomonas aeruginosa, Serratia, Brucella, Salmonella, Haemophilus, Shigella and Mycobacterium tuberculosis and other mycobacteria also have good antibacterial effects, and aminoglycoside antibiotics have many advantages, such as good water solubility, strong antibacterial ability, stable properties, good absorption and excretion, etc., so they are widely used in clinical practice. [Cai Zhuoling, Li...

Claims

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Application Information

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IPC IPC(8): C07H15/234C07H1/06G01N30/02G01N30/06G01N30/74G01N30/86
CPCC07H15/234C07H1/06G01N30/02G01N30/06G01N30/74G01N30/8675C07B2200/13
Inventor 刘照振王成刚寇晋萍刘海涛陆岩黄晓春侯金凤齐麟郭玉东李彧刘琦刘祝月车宝泉戴红
Owner 北京市药品检验研究院(北京市疫苗检验中心)
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