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Method for detecting mosapride citrate and five key impurities in preparation of mosapride citrate

A mosapride citrate and a key technology are applied in the detection field of mosapride citrate related substances, and can solve the problems of long analysis time, influence on the detection accuracy of impurities, baseline fluctuation and the like, and achieve good separation. , The effect of stable baseline and effective control

Active Publication Date: 2020-08-07
南京百思福医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The study found that the above gradient elution method not only takes a long time to analyze, but also has a large baseline fluctuation, which affects the accuracy of impurity detection

Method used

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  • Method for detecting mosapride citrate and five key impurities in preparation of mosapride citrate
  • Method for detecting mosapride citrate and five key impurities in preparation of mosapride citrate
  • Method for detecting mosapride citrate and five key impurities in preparation of mosapride citrate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0066] The screening of embodiment 1 high performance liquid chromatography conditions

[0067] Preparation of system suitability solution: Weigh 10mg each of mosapride citrate related substances A~E, put them in five 20ml measuring bottles, add methanol to dissolve and dilute to the mark, shake well; then take 1ml each and place in the same 100ml To a measuring bottle, add 10 mg of mosapride citrate, add methanol to dissolve and dilute to the mark, shake well to obtain. (Containing mosapride citrate 1mg / ml, each impurity 5μg / ml).

[0068] HPLC conditions: mobile phase: 50mmol / L citric acid solution (adjust pH to 4.0 with sodium hydroxide solution)-acetonitrile (65:35), flow rate 1ml / min, detection wavelength 274nm, column temperature 40°C, sample injection Volume 10 μl.

[0069] Take the system suitability solution and inject it for testing, the results are as follows: figure 1 As shown, impurity B and impurity E cannot be separated.

Embodiment 2

[0070] The screening of embodiment 2 high performance liquid chromatography conditions

[0071] HPLC conditions: mobile phase: 50mmol / L citric acid solution (adjust pH to 4.0 with sodium hydroxide solution)-methanol-acetonitrile (55:35:10), flow rate 1ml / min, detection wavelength 274nm, column temperature 40 ℃, the injection volume is 10 μl.

[0072] Prepare the system suitability solution according to the method in embodiment 1, sample injection detection, the result is as follows figure 2 As shown, all known impurities were detected, the baseline was stable, and the separation between impurities and main peaks and between impurities was good.

Embodiment 3

[0073] Example 3 Baseline comparison between this method and the gradient elution method

[0074] (1) Gradient elution method (Japanese Pharmacopoeia method):

[0075] HPLC conditions: mobile phase A: 0.03mol / L sodium citrate buffer (take 8.82g of trisodium citrate dihydrate, dissolve in 800ml of water, adjust the pH to 4.0 with dilute hydrochloric acid, add water to dilute to 1000ml obtained), mobile phase B: acetonitrile; column temperature 40°C, flow rate 1ml / min; detection wavelength 274nm, gradient elution as shown in the table below.

[0076]

[0077] (2) The patent method

[0078] HPLC conditions: mobile phase: 50mmol / L citric acid solution (adjust pH to 4.0 with sodium hydroxide solution)-methanol-acetonitrile (55:35:10), column temperature 40°C, flow rate 1ml / min, detection wavelength 274nm.

[0079] Prepare blank solution according to the method in embodiment 1, sample injection detects, and the result is as follows image 3 As shown, in the gradient method of...

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Abstract

The invention discloses a method for detecting mosapride citrate and five key impurities in a preparation of the mosapride citrate, and belongs to the technical field of medicine quality detection methods, and particularly relates to the method for detecting mosapride citrate and five key impurities in the preparation of the mosapride citrate by adopting high performance liquid chromatography. According to the detection method, the test solution is prepared, the isocratic elution is carried out by adopting the high performance liquid chromatography, and the related substances in a drug and thepreparation of the drug are detected. The detection method is good in separation degree, high in sensitivity on the related substances, stable in baseline and short in analysis time, and is simple and convenient to operate.

Description

technical field [0001] The invention relates to the field of drug detection, in particular to a method for detecting related substances of mosapride citrate. [0002] technical background [0003] Mosapride citrate is a potent and selective 5-HT4 receptor agonist that stimulates the release of acetylcholine and enhances gastric and duodenal motility. It is a new type of safe and effective digestive tract motility drug. Mosapride citrate tablets (trade name: Gasqing) were developed by Sumitomo Pharmaceutical Co., Ltd., and were first launched in Japan in October 1998. Chinese chemical name 4-amino-5-chloro-2-ethoxy-N-{[4-(4-fluorobenzyl)-2-morpholinyl]methyl}benzamide citrate; molecular formula: C 21 h 25 ClFN 3 o 3 ·C 6 h 8 o 7 2H 2 O, molecular weight: 650.05, its structural formula is: [0004] [0005] The synthetic route of mosapride citrate crude drug is as follows. During the synthesis process, process impurities will be introduced from the starting materi...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/86
CPCG01N30/02G01N30/06G01N30/8675
Inventor 王栋李学明王永禄孙红李杨陈卫孙小虎黄凯宇
Owner 南京百思福医药科技有限公司
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