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Method for detecting related substances of 3-amino-6-methoxypyridazine

A methoxypyridazine and detection method technology, which is applied in the field of medicine, can solve the problems of no relevant literature reports on the detection method of process impurities, etc., and achieve the effects of good linear correlation, strong specificity and high sensitivity

Pending Publication Date: 2022-07-15
南京方生和医药科技有限公司 +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, there are many reports about the preparation method of this compound, and various process impurities are often introduced in the process of the existing synthesis process, such as 3-amino-6-chloropyridazine (impurity A), 3-amino-6-hydroxyl Pyridazine (impurity B), 3-chloro-6-hydroxypyridazine (impurity C), 3,3-dichloropyridazine (impurity D), 3,6-dimethoxypyridazine (impurity E), 3 - 7 kinds of amino-6-methoxypyridazine (impurity F), 3-aminopyridazine (impurity G), etc., but there are no relevant literatures reporting the detection methods of these process impurities

Method used

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  • Method for detecting related substances of 3-amino-6-methoxypyridazine
  • Method for detecting related substances of 3-amino-6-methoxypyridazine
  • Method for detecting related substances of 3-amino-6-methoxypyridazine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Example 1 System suitability test

[0046] Preparation of system suitability solution: take about 25 mg of 3-amino-6-methoxypyridazine test product, accurately weigh it, put it in a 50 ml volumetric flask, add water and ultrasonic to dissolve, cool to room temperature, and then add 7.5 μg / 5ml of each impurity stock solution of ml, diluted with water to the mark, shaken up to prepare a system suitability solution of each impurity 0.75μg / ml and 3-amino-6-methoxypyridazine 0.5mg / ml. Sample injection test, detection conditions are as follows: chromatographic column: Atlantis T3 column; mobile phase: use 20mmol / L potassium hexafluorophosphate buffer (adjust pH to 3.0 with phosphoric acid) as mobile phase A, use acetonitrile as mobile phase B, gradient wash flow rate: 1.0ml / min; column temperature: 35°C; detection wavelength: 215nm; injection volume 5μl. Record the results as in Table 1 and figure 1 shown.

[0047] Table 1 System suitability test results

[0048] ...

Embodiment 2

[0050] Example 2 Specificity test

[0051] 2.1 Interference test

[0052] Blank solvent: water

[0053] Preparation of the test solution: Precisely weigh about 25 mg of the 3-amino-6-methoxypyridazine test product, put it in a 50ml measuring bottle, add water to ultrasonically make the solution, cool to room temperature, then dilute with water to the mark, shake well .

[0054]The blank solvent and the test solution were injected separately, and the detection conditions were as follows: chromatographic column: Atlantis T3 column; mobile phase: 20mmol / L potassium hexafluorophosphate buffer (adjusted to pH 3.0 with phosphoric acid) as mobile phase A, with Acetonitrile is mobile phase B, gradient elution; flow rate: 1.0 ml / min; column temperature: 35°C; detection wavelength: 215 nm; injection volume 5 μl. Record the results, the spectra are as follows figure 2 and image 3 shown. The results showed that the blank solvent did not interfere with the detection of the test pro...

Embodiment 3

[0075] Example 3 Detection limit and quantification limit

[0076] Preparation of 3-amino-6-methoxypyridazine reference substance stock solution: Precisely weigh about 25 mg of 3-amino-6-methoxypyridazine reference substance, put it in a 50ml volumetric flask, add water to sonicate to dissolve, and cool to room temperature , and then dilute with water to the mark, shake well.

[0077] Preparation of quantitative limit stock solution: Precisely measure 1.5ml of 3-amino-6-methoxypyridazine reference stock solution and 5ml of other impurity stock solutions in the same 100ml measuring bottle, add water to dilute to the mark, and shake well.

[0078] Preparation of the limit of quantification solution: Precisely measure 1ml of the limit of quantification stock solution, put it in a 50ml volumetric flask, add water to dilute to the mark, and shake well.

[0079] Preparation of detection limit solution: Precisely measure 3ml of quantitation limit solution and put it in a 10ml volume...

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Abstract

The invention discloses a method for detecting related substances of 3-amino-6-methoxypyridazine. The method comprises the following steps: (1) preparing a test solution and a contrast solution; (2) detecting and recording: detecting the test solution and the contrast solution by adopting a liquid chromatography and recording a spectrogram; wherein the chromatographic conditions of the liquid chromatography are as follows: a chromatographic column is a water-resistant octadecyl bonded silica gel column; mobile phase: a potassium hexafluorophosphate buffer solution (the pH is adjusted to 2.8-3.2 by phosphoric acid) is used as a mobile phase A, acetonitrile is used as a mobile phase B, and gradient elution is performed; the flow rate is 0.9 to 1.1 ml / min; the column temperature is 33 to 37 DEG C; the detection wavelength is 213 to 217 nm. The detection method can be used for rapidly and accurately detecting related substances in 3-amino-6-methoxypyridazine, and is good in accuracy, precision, reproducibility and stability.

Description

technical field [0001] The invention belongs to the technical field of medicine, and relates to a method for detecting related substances in a pharmaceutical intermediate 3-amino-6-methoxypyridazine. Background technique [0002] 3-Amino-6-methoxypyridazine (English name: 3-amino-6-methoxydazine) is an important pharmaceutical intermediate, which can be used for pyridopyrimidine compounds or drugs with significant biological activity, such as Relugolix, a cancer drug, can be used to treat pain caused by endometriosis, uterine fibroids, and advanced prostate cancer. [0003] At present, there are many reports on the preparation method of this compound, and various process impurities are often introduced in the process of the existing synthesis process, such as 3-amino-6-chloropyridazine (impurity A), 3-amino-6-hydroxyl Pyridazine (impurity B), 3-chloro-6-hydroxypyridazine (impurity C), 3,3-dichloropyridazine (impurity D), 3,6-dimethoxypyridazine (impurity E), 3 - 7 kinds of...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/027
Inventor 牟丽丽李双花贾佳王敏王然李慧敏郑雪涛
Owner 南京方生和医药科技有限公司
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