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Preparation and structure identification method of unknown impurities of amikacin sulfate injection

A technology of amikacin sulfate and unknown impurities, applied in the field of preparation and structure identification of unknown impurities in amikacin sulfate injection, can solve the problems of uncontrollable adverse reactions, affecting safety, limiting the content of impurities, etc. Ensuring the quality and drug safety, the effect of the method is simple

Pending Publication Date: 2022-05-13
杭州沐源生物医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Amikacin sulfate contains unknown impurities, which will directly affect the safety of the product and lead to uncontrollable adverse reactions. In order to further ensure the quality of the drug, a thorough study of the impurities in the sample is conducted to analyze the reasons and strictly limit the content of impurities. A technical problem that needs to be solved

Method used

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  • Preparation and structure identification method of unknown impurities of amikacin sulfate injection
  • Preparation and structure identification method of unknown impurities of amikacin sulfate injection
  • Preparation and structure identification method of unknown impurities of amikacin sulfate injection

Examples

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Embodiment 1

[0049] Separation and purification of unknown impurities in amikacin sulfate injection by the following steps:

[0050] Heat and stir 80ml of Amikacin Sulfate Injection until saturated, cool and crystallize and filter, the resulting filtrate is crystallization mother liquor, concentrate to dryness under reduced pressure to obtain a solid sample containing about 2% of the unknown impurity, then add 10ml Dissolve dichloromethane, add 8g of 200 mesh silica gel, concentrate to dryness under reduced pressure, then use dry method to prepare sample, put it on silica gel column, and use petroleum ether-ethyl acetate with volume ratio of 20:1, 10:1, 0:1 to mix successively The volume of each solution was 500mL, eluted and washed into the column, and the components with Rf of 0.5 were collected, concentrated to dryness under reduced pressure to obtain 200mg of 10% crude product of the unknown impurity, dissolved in 10ml of purified water, prepared into a solution, and carried out gradien...

Embodiment 2

[0059] Separation and purification of this unknown impurity in amikacin sulfate injection by the following steps: measure amikacin sulfate injection 40ml until saturated under heating and stirring conditions, suction filtration after cooling and crystallization carries out solid-liquid separation, and the gained filtrate is The crystallized mother liquor was concentrated to dryness under reduced pressure to obtain a solid sample containing about 2% of the unknown impurity, then added 10ml of dichloromethane to dissolve it, added 8g of 200 mesh silica gel, concentrated to dryness under reduced pressure, and then prepared the sample by dry method and put it on a silica gel column , followed by volume ratios of 20:1, 10:1, 0:1 petroleum ether - ethyl acetate mixed solution volume 250mL elution washed column, collected components with Rf 0.5, concentrated to dryness under reduced pressure to obtain 10% 100 mg of the crude unknown impurity was dissolved in 5 ml of purified water to ...

Embodiment 3

[0062] The structure of the obtained unknown impurity was analyzed by the following steps:

[0063] Molecular weight determination: Weigh about 2.00mg of unknown impurity sample into a 5ml volumetric flask, dissolve with purified water and dilute to the mark to prepare unknown impurity mother liquor. Remove 1ml of the unknown impurity mother solution, place it in a 10ml volumetric flask, dilute to the mark with purified water, and prepare an unknown impurity solution. LC-MS analysis conditions are preferably Agilent 1200-Themo-LTQ ORBITRAPXL, chromatographic column: Unisil 10-120 C18 Aq 10μm 4.6*250mm, mobile phase: A phase 0.1% formic acid solution, B phase acetonitrile solution, gradient elution (0 -4min, 100%A; 4-8min, 100%A→90%A; 8-10min, 90%A; 10-10.010, 90%A→100%A; 10.010-14min, 100%A), column temperature : 30°C, UV detector wavelength: 220nm, column flow rate: 0.8ml / min, injection volume: 100μl, run time 14min, ion source: ACPI, positive ion mode, fragmentation voltage...

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Abstract

The invention belongs to the field of medicine technology analysis, and particularly relates to a preparation method and a structure identification method of unknown impurities in amikacin sulfate injection. The method comprises the following steps: crystallizing the amikacin sulfate injection, carrying out preliminary separation by silica gel, carrying out gradient separation by preparative liquid chromatography to obtain an unknown impurity with the content of more than 80%, carrying out structural identification on the unknown impurity by LC-MS and HPLC analysis means, determining the molecular structure of the unknown impurity in the amikacin sulfate injection, and analyzing the generation reason of the unknown impurity. And the impurity limit in the amikacin sulfate injection is set to be not more than 0.30%. The confirmation of the impurity enables the impurity research of the amikacin sulfate injection product to be more comprehensive, and the product quality research to be more perfect.

Description

technical field [0001] The invention belongs to the field of technical analysis of medicines, and in particular relates to a preparation and structure identification method of unknown impurities in amikacin sulfate injection. Background technique [0002] The chemical name of amikacin sulfate is O-3-amino-3-deoxy-α-D-glucopyranosyl-(1→4)-O-[6-amino-6-deoxy-α-Dglucosyl Pyranosyl-(l→6)]-N3-(4-amino-2-hydroxy-1-oxobutyl)-2-deoxy-L-streptamine sulfate, produced by the fermentation product Kanamyces It is obtained by synthesis of aminohydroxybutyryl chains in the streptomycin part of the kanamycin A molecule. Its physical, chemical, pharmacological and pharmacokinetic characteristics are similar to those of other aminoglycoside antibiotics. The site of action is bacterial ribose The 30S subunit of the body inhibits the synthesis of bacterial proteins and produces a bactericidal effect. The characteristic of amikacin sulfate is that it is stable to aminoglycoside inactivating en...

Claims

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Application Information

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IPC IPC(8): C07H15/224C07H1/06G01N30/04G01N30/06G01N30/72
CPCC07H15/224C07H1/06G01N30/04G01N30/06G01N30/72G01N2030/027
Inventor 陈轶嘉徐兵勇董燕华陈渊李元飞黄燕斌李艳韩上上范东东庹皓
Owner 杭州沐源生物医药科技有限公司
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