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Separation and preparation method of trace impurities D in gabapentin bulk drug

A technology of trace impurities and gabapentin, which is applied in organic chemistry and other fields, can solve the problem of undiscovered countercurrent chromatography two-phase solvent system

Pending Publication Date: 2021-04-20
ZHEJIANG CHIRAL MEDICINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The reason why this method has not been used for the separation and preparation of trace impurity D in gabapentin bulk drug is that no countercurrent chromatography two-phase solvent system capable of effectively separating trace impurity D has been found.

Method used

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  • Separation and preparation method of trace impurities D in gabapentin bulk drug
  • Separation and preparation method of trace impurities D in gabapentin bulk drug

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Embodiment 1

[0035] Embodiment 1. A method for separating and preparing impurity D from gabapentin bulk drug, using a countercurrent chromatograph to perform the following steps in sequence:

[0036] 1), n-butanol, methanol and 0.2% formic acid aqueous solution are prepared as a two-phase solvent in a volume ratio of 5:1:5, and the layers are left to stand in a liquid separation container to separate the upper and lower phases; that is, the upper and lower phases are obtained respectively And next phase.

[0037] 2) Dissolving 600 mg of gabapentin bulk drug in 5 ml of the upper phase and 5 ml of the lower phase to form a sample solution (gabapentin bulk drug solution); the internal diameter of the countercurrent chromatographic column is 2.6 mm, and the column volume is 310 ml. The above phase is used as the stationary phase, and the lower phase is the mobile phase. After the separation column of the countercurrent chromatograph is filled with the stationary phase, the sample solution is i...

Embodiment 2-1

[0045] Embodiment 2-1, a kind of method for separating and preparing impurity D from gabapentin crude drug:

[0046] The injection flow rate of the mobile phase in step 2) of Example 1 was changed from 5.0 ml / min to 6.0 ml / min, and the rest were identical to those of Example 1. The final obtained impurity D has a purity of 96.2% and a recovery rate of 87.4%.

Embodiment 2-2

[0047] Embodiment 2-2, a kind of method for separating and preparing impurity D from gabapentin crude drug:

[0048] The injection flow rate of the mobile phase in step 2) of Example 1 was changed from 5.0 ml / min to 4.0 ml / min, and the rest were identical to those of Example 1. The final obtained impurity D has a purity of 96.5% and a recovery rate of 85.9%.

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Abstract

The invention discloses a method for separating and preparing a trace impurity D in a gabapentin bulk drug, the molecular formula of the trace impurity D is C18H29NO3, and the trace impurity D in the gabapentin bulk drug is separated and prepared by adopting a counter-current chromatography. According to a counter-current chromatography method, n-butyl alcohol, methanol and 0.2% formic acid aqueous solution are used as a solvent system for separation and preparation; through online monitoring of an ultraviolet detector, target fractions are collected and combined according to a map and subjected to rotary evaporation to be dry, and an impurity D is obtained. By adopting the method disclosed by the invention, the quality of gabapentin series products can be conveniently controlled.

Description

technical field [0001] The invention belongs to the technical field of drug impurity research, and specifically relates to a method for separating and preparing trace impurity D in gabapentin bulk medicine, in particular to a method for separating and preparing trace impurity D from gabapentin bulk medicine by high-speed countercurrent chromatography. Background technique [0002] Drugs will introduce some impurities during the production process, often due to the impurity of raw materials or incomplete reactions, the existence of intermediate products and reaction by-products, and related impurities caused by the influence of external conditions during the storage process of drugs, such as temperature and humidity. Under the influence and action of factors such as microorganisms, time, etc., changes such as hydrolysis, oxidation, decomposition, isomerization, and mildew will occur in the drug, and related impurities will be produced in the drug. In addition, the contact wit...

Claims

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Application Information

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IPC IPC(8): C07D209/54
Inventor 何匡朱银龙沈丽洒夏鑫佳彭家荣
Owner ZHEJIANG CHIRAL MEDICINE CHEM