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Method for detecting residual solvents in pantoprazole sodium sesquihydrate

A technology of sesquihydrate and pantoprazole sodium is applied in the field of detection of residual solvent in pantoprazole sodium sesquihydrate, and can solve problems such as limited types of residual solvents and the like

Pending Publication Date: 2020-10-23
武汉九州钰民医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The present invention is in order to solve the problem that the type of residual solvent in the detection pantoprazole sodium sesquihydrate is limited in the prior art, thereby provides a kind of detection method of residual solvent in the pantoprazole sodium sesquihydrate

Method used

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  • Method for detecting residual solvents in pantoprazole sodium sesquihydrate
  • Method for detecting residual solvents in pantoprazole sodium sesquihydrate
  • Method for detecting residual solvents in pantoprazole sodium sesquihydrate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] (1) prepare need testing solution: get pantoprazole sodium sesquihydrate 0.5g, accurately weighed, put in the headspace bottle, add solvent [dimethylsulfoxide-water (80-20)] 5ml and make it dissolve , Sealed, that is, the test solution.

[0057] (2) Preparation of reference solution: Accurately weigh 300mg of methanol, 60mg of dichloromethane, 500mg of ethanol, and 41mg of acetonitrile, place them in a 100ml measuring bottle with 10ml of solvent, add solvent to dilute to the mark, and shake well to obtain the first reserve solution; accurately weigh 40 mg of benzene and place it in a 100 ml measuring bottle with 10 ml of solvent, add solvent to dilute to the mark, and shake well to obtain the benzene intermediate stock solution; then precisely pipette 0.5 ml of benzene intermediate stock solution and place it in the existing 2 -In a 100ml measuring bottle with 5ml of solvent, add solvent to dilute to the mark, and shake well to obtain the second stock solution; precisel...

Embodiment 2

[0085] Limit of detection and limit of quantification: The limit of detection (LOD) and limit of quantitation (LOQ) are determined according to the signal-to-noise ratio method. The tested signal is compared with the baseline noise, and the lowest concentration or percentage that can be reliably detected is calculated. Dilute each residual solvent stock solution of known concentration to a low concentration and measure according to the law, requiring detection limit signal-to-noise ratio S / N≥3; quantification limit signal-to-noise ratio S / N≥10, and connected to 6 needles of LOQ solution peak area RSD≤15%.

[0086] Solution preparation

[0087] Blank solution: accurately pipette 5ml of diluent, put it in a headspace bottle, seal it, and get it.

[0088] Quantitative limit solution: Precisely pipette 0.2ml of methanol positioning solution, 0.2ml of dichloromethane positioning solution, 0.125ml of ethanol positioning solution, 0.5ml of acetonitrile positioning solution, 2.5ml of...

Embodiment 3

[0097] Linearity: From the limit of quantification to 150% concentration of each residual solvent limit, uniformly select 6 concentration levels to prepare the solution, measure according to the law, take the main peak concentration as the abscissa, and take the peak area as the ordinate, fit the curve and perform linear regression Y=aX+b, requiring correlation coefficient r≥0.99; Y-axis intercept / limit concentration peak area should be ≤25%.

[0098] Solution preparation

[0099] Blank solution: Accurately pipette 5ml of diluent and put it in a headspace bottle, seal it, and get it.

[0100] Methanol positioning solution: Accurately weigh 304.0mg of methanol, put it in a 100ml measuring bottle with 10ml of diluent, add diluent to make up to the mark, shake well, and it is marked as ID-MeOH.

[0101] Dichloromethane positioning solution: Accurately weigh 62.1mg of dichloromethane, put it in a 100ml measuring bottle with 10ml of diluent, add diluent to make up to the mark, sha...

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Abstract

The invention provides a method for detecting residual solvents in pantoprazole sodium sesquihydrate. The method comprises the following steps: (1) preparing a test solution which comprises pantoprazole sodium sesquihydrate and a solvent, wherein the solvent comprises dimethyl sulfoxide and / or water; (2) preparing a reference substance solution, wherein the reference substance solution comprises methanol, dichloromethane, ethanol, acetonitrile and benzene, wherein a solvent is the same as the solvent in step (1); and (3) performing headspace gas chromatography test by using a medium-polarity capillary column and adopting temperature programming, wherein the sequence of the step (1) and step (2) is not sequential. The method can be used for simultaneously detecting the residual quantity ofmethanol, dichloromethane, ethanol, acetonitrile and benzene in the pantoprazole sodium sesquihydrate. The method has good specificity, system adaptability, extremely low detection limit and quantification limit, good linearity, good accuracy and durability.

Description

technical field [0001] The invention relates to the technical field of drug analysis, in particular to a method for detecting residual solvents in pantoprazole sodium sesquihydrate. Background technique [0002] Pantoprazole sodium (pantoprazole sodium), chemical name 5-difluoromethoxy-2-[(3,4-dimethoxy-2-pyridyl)-methyl]sulfinyl-1H-benzo Imidazole sodium salt, is a H + , K + -ATPase inhibitor, which can inhibit the secretion of gastric acid stimulated by various factors such as histamine, gastrin and acetylcholine, and is used for the treatment of diseases related to gastric acid secretion disorders, with high cure rate, rapid onset, and small adverse reactions Etc. Pantoprazole sodium is usually monohydrate or sesquihydrate. [0003] The manufacturer of pantoprazole sodium sesquihydrate is Jinzhou Jiutai Pharmaceutical Co., Ltd., which is the first manufacturer in China to develop sesquihydrate API. According to the synthetic route of analysis bulk drug, in the operat...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/047
Inventor 姚萍刘松林范昭泽陈龙张璐龚丹凤余艳平顿伟许勇
Owner 武汉九州钰民医药科技有限公司
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