Esomeprazole magnesium related substance analysis method based on impurity spectrum

A technology for esomeprazole magnesium and related substances is applied in the field of related substance analysis of novel esomeprazole magnesium, and can solve problems such as poor sample stability and the like

Inactive Publication Date: 2020-04-10
SHANDONG DYNE MARINE BIOTECHCAL PHARM HLDG CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the stability of the sample is not good, and it needs to be prepared and delivered now

Method used

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  • Esomeprazole magnesium related substance analysis method based on impurity spectrum
  • Esomeprazole magnesium related substance analysis method based on impurity spectrum
  • Esomeprazole magnesium related substance analysis method based on impurity spectrum

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Example 1: Detection according to the final scheme

[0043] According to the final scheme of the present invention, the related substances of esomeprazole magnesium are analyzed by HPLC based on the impurity spectrum:

[0044] The chromatographic analysis conditions are as follows:

[0045] Chromatographic column: C8 column (250mm×4.6mm, 5μm)

[0046] Detector: UV detector

[0047] Detection wavelength: 280nm

[0048] Column temperature: 25℃

[0049] Mobile phase flow rate: 1.5mL / min

[0050] Injection volume: 20μl

[0051] Its mobile phase uses:

[0052] (1) Ammonium acetate buffer solution: Weigh 0.7708 g of ammonium acetate solid into 1 L of purified water, mix well, and filter through a membrane to obtain it.

[0053] (2) Mobile phase A: acetonitrile: ammonium acetate = 1:3, ammonia water to adjust pH = 7.65;

[0054] (3) Mobile phase B: acetonitrile: ammonium acetate = 6:4, ammonia water to adjust pH = 7.65.

[0055] The above mobile phase is a gradient,...

Embodiment 2

[0061] Example 2: Investigating the choice of dissolved phase

[0062] The type of mobile phase will affect the peak shape of impurity B, so we use mobile phase A and B as the dissolved phase respectively, and investigate the chromatographic conditions. The test results are as follows: figure 2 .

[0063] Conclusion: When mobile phase B is used as the dissolving phase, due to the large amount of acetonitrile and strong solubility, impurity B will have solvent effect, the number of theoretical plates is low, and the peak is split; after changing to mobile phase A, the solvent effect disappeared and the column efficiency increased.

Embodiment 3

[0064] Embodiment 3: investigate the influence of different pH values ​​on the separation of impurity D and main peak (adjust pH first and add acetonitrile)

[0065] Different pH values ​​will affect the separation of impurity D and the main peak. At the same time, the sequence of adding acetonitrile and adjusting pH will also affect the separation. In order to determine the most suitable method, we first adjust the pH and then add acetonitrile. The effect of pH on the separation results in image 3 .

[0066] Conclusion: Between 7.95 and 8.10, the higher the pH, the closer the impurity D is to the main peak, the worse the resolution, and the poor repeatability of the final pH value of the prepared mobile phase, resulting in impurities after the main peak sometimes detectable, sometimes not. .

[0067] Then we investigated the effect of different pH on the separation of impurity D and the main peak when acetonitrile was added and the pH was adjusted again. The results are as...

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Abstract

The invention provides a method for effectively separating known and potential impurities in esomeprazole magnesium based on an esomeprazole magnesium impurity spectrum. The retention time of the esomeprazole main peak is about 15 minutes, the resolution between impurity peaks is greater than 1.5, the number N of theoretical plates of the main peak is greater than or equal to 3000, the main peak tailing factor T is greater than or equal to 0.8 and less than or equal to 1.2, and the peak pattern is good. According to the method, a C8 chromatographic column (250 mm * 4.6 nm, 5 microns) and a UVdetector are mainly adopted, the detection wavelength is 280 nm, the column temperature is 25 DEG C, the flow velocity of a mobile phase is 1.5 mL/min, and the sample introduction volume is 20 microliters; a mobile phase A: the ratio of acetonitrile to ammonium acetate is 1: 3, and the pH value is adjusted to 7.5 by ammonia water; and a mobile phase B: the ratio of acetonitrile: ammonium acetate is 6: 4, and the pH value is adjusted to 7.5 by ammonia water. Experiments prove that the method can effectively and successfully separate 12 impurities and main peaks in an impurity spectrum, realizeseffective detection, and can be used for quality monitoring in the production process of the esomeprazole magnesium bulk drug.

Description

technical field [0001] The invention relates to a novel related substance analysis method of esomeprazole magnesium based on impurity profile. Background technique [0002] Gastroesophageal reflux refers to the reflux of gastric contents into the esophagus, which can be divided into physiological and pathological, including alkaline reflux, that is, bile salts and pancreatic enzymes refluxed from the duodenum into the stomach into the esophagus. When GER is accompanied by symptoms or complications, it is called gastroesophageal reflux disease. Clinically, it can be manifested as vomiting, weight loss, dysphagia, retrosternal pain, esophagitis, and respiratory symptoms. Esomeprazole is the S-type optical isomer of omeprazole. Due to its pharmacokinetic characteristics, it is superior to several existing PPIs in the treatment of GERD and the eradication of Helicobacter pylori in combination with antibiotics. The pharmacokinetics of esomeprazole magnesium is characterized by ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/34G01N30/36G01N30/74G01N30/86
CPCG01N30/02G01N30/06G01N30/34G01N30/36G01N30/74G01N30/8679G01N2030/027
Inventor 赵忠熙段洪东何淑旺吴晓东杨琳解春文
Owner SHANDONG DYNE MARINE BIOTECHCAL PHARM HLDG CO LTD
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