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Method of measuring content of related substance in dexmedetomidine hydrochloride active ingredient

A technology for dexmedetomidine hydrochloride and related substances, which is applied in the field of drug analysis and can solve problems to be improved and the like

Inactive Publication Date: 2017-11-28
YICHANG HUMANWELL PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, the method for determining the content of related substances in dexmedetomidine hydrochloride bulk drug still needs to be improved

Method used

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  • Method of measuring content of related substance in dexmedetomidine hydrochloride active ingredient
  • Method of measuring content of related substance in dexmedetomidine hydrochloride active ingredient
  • Method of measuring content of related substance in dexmedetomidine hydrochloride active ingredient

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] The selection of embodiment 1 chromatographic conditions

[0058] wavelength selection

[0059] Starting material 1, intermediate 2, intermediate 3, and impurity B in the dexmedetomidine hydrochloride crude drug are mixed and dissolved in water to form a mixed solution containing 0.5 mg / ml of each substance, sample injection, and use DAD (diode array detection device, which can also be expressed as PDA) for full-wavelength scanning, the chromatogram results are as follows figure 1 shown. figure 1 The results show that scanning the PDA chromatogram of each substance finds that all substances have terminal absorption peaks, and then select a wavelength with relatively large main peaks and impurity peaks, so the inventor selects a lower wavelength of 214nm.

[0060] pH selection

[0061] In the present invention, the inventor uses 0.03mol / L dipotassium hydrogen phosphate solution (phosphoric acid adjusts pH to 7.0) and 0.05mol / L potassium dihydrogen phosphate solution (...

Embodiment 2

[0084] Embodiment 2 specificity experiment

[0085] The verification process of the specificity experiment is as follows:

[0086] ① The finished product and each starting material and intermediate are injected separately to obtain a chromatogram; and after mixing, inject a sample to obtain a chromatogram;

[0087] ② Degrade the finished product under severe conditions such as acid, alkali, oxidation, pyrolysis, and light;

[0088] The acceptable detection criteria for the verification results of the specificity experiment are as follows:

[0089] ① The existence of each starting material and intermediate does not interfere with the detection of the main component;

[0090] ②The separation between the main peak and the impurity peak should be greater than 1.5, and the minimum separation between the impurity peaks should be greater than 1.5;

[0091] ③ The purity angle value of the main peak and the main impurities should be less than the purity threshold value (use PDA to s...

Embodiment 3

[0104] Embodiment 3 durability experiment

[0105] Verification process of durability test

[0106] Investigate mobile phase flow rate variation ± 10%, column temperature variation ± 5 ℃, mobile phase pH value variation and the variation of chromatographic column, to measure need testing solution (concentration of need testing solution is 0.5mg / ml, injection volume is 20ul) chromatographic changes in chromatographic behavior.

[0107] Acceptable criteria for the results of the durability test are as follows:

[0108] (1) The main peak tailing factor should be ≤ 2.0,

[0109] (2) The impurity peak and other component peaks must achieve baseline separation,

[0110] (3) The RSD of impurity content data under each condition should be ≤10.0%,

[0111] (4) The absolute value of the impurity content is within 0.1%.

[0112] The test results of the durability test are shown in Table 3-1.

[0113] Table 3-1:

[0114]

[0115] As can be seen from Table 3-1, the tailing factor...

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PUM

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Abstract

The invention provides a method of measuring the content of related substance in dexmedetomidine hydrochloride active ingredient. The method comprises the following steps: analyzing the dexmedetomidine hydrochloride active ingredient by means of liquid chromatography to obtain a chromatogram conveniently; and determining the content of related substance in the dexmedetomidine hydrochloride active ingredient based on the chromatogram. The method can effectively measure impurities, initial materials and intermediates probably introduced in a synthetic process of dexmedetomidine hydrochloride and effectively control the quality of a dexmedetomidine hydrochloride drug. The method has the characteristics of effectiveness, sensitivity, specificity and accuracy.

Description

technical field [0001] The invention relates to the technical field of drug analysis, in particular, the invention relates to a method for determining the content of related substances in dexmedetomidine hydrochloride crude drug. Background technique [0002] Dexmedetomidine hydrochloride is an α2-adrenoceptor agonist, its chemical name is: (+)-4-(S)-[1-(2,3-dimethylphenyl)ethyl]-1H - imidazole hydrochloride. It can be used for sedation during endotracheal intubation and mechanical ventilation of surgical patients undergoing general anesthesia. The structural formula of dexmedetomidine hydrochloride is shown below. [0003] [0004] However, the method for determining the content of related substances in dexmedetomidine hydrochloride crude drug still needs to be improved. Contents of the invention [0005] The present invention aims to solve one of the technical problems in the related art at least to a certain extent. [0006] The present invention has been accompli...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/027
Inventor 王学海潘思敬许勇罗勇乐洋刘城铭胡虹黄璐江曦肖强于静
Owner YICHANG HUMANWELL PHARMA
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