Method for detecting content of dyclonine hydrochloride mucilage or related substances through high performance liquid chromatography

A technology of high performance liquid phase and related substances, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of shortened life, no detection method of dyclonine hydrochloride mucilage, large column damage, etc.

Pending Publication Date: 2020-04-28
TIANJIN PHARMA GROUP XINZHENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0015] In the above methods for detecting the content of dyclonine hydrochloride mucilage, the mobile phase mostly uses a mixed solution of buffer salt and methanol or acetonitrile with different volume ratios. The buffer salt will cause greater damage to the column, resulting in increased column pressure and shortened life. And the obtained dyclonine hydrochloride chromatographic peak tailing phenomenon is serious; In addition, dyclonine hydrochloride i

Method used

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  • Method for detecting content of dyclonine hydrochloride mucilage or related substances through high performance liquid chromatography
  • Method for detecting content of dyclonine hydrochloride mucilage or related substances through high performance liquid chromatography
  • Method for detecting content of dyclonine hydrochloride mucilage or related substances through high performance liquid chromatography

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Effect test

Embodiment 1

[0063] A method for detecting the content of dyclonine hydrochloride mucilage by high performance liquid phase, the chromatographic conditions are as follows:

[0064] Chromatographic column: octadecylsilane bonded silica gel column (4.6mm×150mm, 5μm);

[0065] Mobile phase: 0.5v% triethylamine (phosphoric acid to adjust pH to 4.0): methanol = 60:40; 0.5v% triethylamine is prepared with water as solvent, the same below;

[0066] Flow rate: 1.0ml / min;

[0067] Column temperature: 25°C;

[0068] Solvent: 0.5% triethylamine (phosphoric acid to adjust pH to 4.0): methanol = 50:50;

[0069] Theoretical plate number: not less than 2000 calculated according to the peak of dyclonine hydrochloride;

[0070] Implementation steps:

[0071] Preparation of the test solution: Take 10 sticks of this product, shake them well, mix them with ultrasonic waves, pour them into a beaker, stir them mechanically, mix them evenly, take 1ml to a 100ml measuring bottle precisely with an internal vol...

Embodiment 2

[0075] A method for detecting the content of dyclonine hydrochloride mucilage by high performance liquid phase, the chromatographic conditions are as follows:

[0076] Chromatographic column: octadecylsilane bonded silica gel column;

[0077] Mobile phase: 0.015mol / L KH 2 PO 4 (glacial acetic acid adjusts pH to 3.5): acetonitrile=55:45;

[0078] Flow rate: 1.0ml / min;

[0079] Column temperature: 35°C;

[0080] Solvent: 0.015mol / L KH 2 PO 4 (glacial acetic acid to adjust the pH to 3.5): acetonitrile=60:40;

[0081] Theoretical plate number: not less than 2000 calculated according to the peak of dyclonine hydrochloride;

[0082] Implementation steps:

[0083] Preparation of the test solution: Take 10 sticks of this product, shake them well, mix them with ultrasonic waves, pour them into a beaker, stir them mechanically, mix them evenly, take 1ml to a 100ml measuring bottle precisely with an internal volume pipette, and use Wash the inner wall of the pipette with 30ml of...

Embodiment 3

[0087] A method for detecting the content of dyclonine hydrochloride mucilage by high performance liquid phase, the chromatographic conditions are as follows:

[0088] Chromatographic column: octadecylsilane bonded silica gel column;

[0089] Mobile phase: 0.015mol / L anhydrous sodium acetate (adjust the pH to 3.0 with trifluoroacetic acid): ethanol = 70:30;

[0090] Flow rate: 1.0ml / min;

[0091] Column temperature: 40°C;

[0092] Solvent: 0.015mol / L anhydrous sodium acetate (adjust pH to 3.0 with trifluoroacetic acid): ethanol = 70:30;

[0093] Theoretical plate number: not less than 2000 calculated according to the peak of dyclonine hydrochloride;

[0094] Implementation steps:

[0095] Preparation of the test solution: Take 10 sticks of this product, shake them well, mix them with ultrasonic waves, pour them into a beaker, stir them mechanically, mix them evenly, take 1ml to a 100ml measuring bottle precisely with an internal volume pipette, and use Wash the inner wall...

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Abstract

The application discloses a method for detecting the content of dyclonine hydrochloride mucilage or related substances through a high performance liquid chromatography. According to the method, when the content of the dyclonine hydrochloride mucilage is detected, a linear correlation coefficient R2 between the concentration and a peak area in a concentration range equivalent to 10-200% of the concentration of a test sample is greater than 0.9990, the repeatability is good, the quantification limit of the dyclonine hydrochloride is 0.0510 microgram/ml, the average recovery rate is 98-101%, andthe RSD is less than 2.0%. During detection of related impurities, the separation degree between the impurity I and the dyclonine hydrochloride peak is 29.6, the quantitative limit concentration of the impurity I is 1.734 microgram/ml; the linear equation of the impurity I is as follows: A=2*10<7> C-220161, the correlation coefficient is 0.9993, the peak area RSD of the impurity I is 0.6%, the average recovery rate is 97.9%, the RSD is 3.5%, and the detection limit is 0.0041 microgram/ml.

Description

technical field [0001] The invention belongs to the field of drug analysis, in particular to a method for detecting the content of dyclonine hydrochloride mucilage or related substances by high-performance liquid phase. Background technique [0002] Dyclonine hydrochloride is a local anesthetic that has been reported to significantly reduce discomfort in patients undergoing upper gastrointestinal endoscopy. Its structural formula is: [0003] The chemical name is 4-butoxy-β-piperidinylpropiophenone hydrochloride, and the molecular formula is C 18 h 27 NO 2 HCl, in the process of synthesizing this compound, can produce by-product, i.e. impurity I, its structural formula is: [0004] [0005] The chemical name is 1-(4-butoxyphenyl)-2-propen-1-one, and the molecular formula is C 13 h 16 o 2 , the molecular weight is 204.26. [0006] According to literature reports, the methods for measuring the content of dyclonine hydrochloride mucilage include: [0007] Song Hon...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/86
CPCG01N30/02G01N30/06G01N30/8679G01N2030/047
Inventor 李淑云周红建李俊霞白艳鹤李强王丽
Owner TIANJIN PHARMA GROUP XINZHENG
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