RT-HPLC detection method for related substances of doxylamine succinate

A technology of RT-HPLC and doxylamine succinate, applied in the field of drug analysis, can solve the problem of inability to separate the characteristic peaks of doxylamine succinate and related substances, achieve simple sample pretreatment, less sample dosage, and ensure the quality effect

Active Publication Date: 2016-04-20
NANJING GRITPHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] In order to solve the problem that the prior art cannot separate the characteristic peaks of doxylamine succinate and related s...

Method used

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  • RT-HPLC detection method for related substances of doxylamine succinate
  • RT-HPLC detection method for related substances of doxylamine succinate
  • RT-HPLC detection method for related substances of doxylamine succinate

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Experimental program
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Effect test

Embodiment 1

[0030] (1) Instrument and chromatographic conditions

[0031] High performance liquid chromatography: Agilent1260 high performance liquid chromatography system and workstation;

[0032] Chromatographic column: Agilent C8 250mm×4.6mm, 5μm;

[0033] Preparation of mobile phase: Take 3.4g of potassium dihydrogen phosphate, 1.5g of triethylamine hydrochloride, 1.5g of sodium dodecylsulfonate, add 650ml of water, stir to fully dissolve, add 300ml of acetonitrile, add 50ml of methanol, stir to make the solution Clarify, filter, and take the filtrate as the mobile phase; the flow rate is 1.0ml per minute, the detection wavelength is 262nm, and the column temperature is 40°C.

[0034] (2) Experimental steps

[0035] Take doxylamine succinate, impurity A (introduction of starting material), impurity B (intermediate impurity), impurity C (demethylation impurity), impurity D (starting material), impurity E (monooxidation impurity) respectively Appropriate amount, put in a 10ml measuri...

Embodiment 2

[0038] (1) Instrument and chromatographic conditions

[0039] High performance liquid chromatography: Agilent1260 high performance liquid chromatography system and workstation;

[0040] Chromatographic column: Agilent C8 250mm×4.6mm, 5μm;

[0041] Prepare mobile phase: potassium dihydrogen phosphate 3.4g, triethylamine hydrochloride 1.5g, sodium dodecylsulfonate 1.5g, add water 700ml, stir to fully dissolve, add acetonitrile 295ml, add methanol 55ml, stir to clarify the solution , filtered, and the filtrate was taken as the mobile phase; the flow rate was 1.0ml per minute, the detection wavelength was 262nm, and the column temperature was 40°C.

[0042] (2) Experimental steps

[0043] Take doxylamine succinate, impurity A (introduction of starting material), impurity B (intermediate impurity), impurity C (demethylation impurity), impurity D (starting material), impurity E (monooxidation impurity) respectively Appropriate amount, put in a 10ml measuring bottle, add 0.1M HCl ...

Embodiment 3

[0046] (1) Instrument and chromatographic conditions

[0047] High performance liquid chromatography: Agilent1260 high performance liquid chromatography system and workstation;

[0048] Chromatographic column: Agilent C8 250mm×4.6mm, 5μm;

[0049]Prepare potassium dihydrogen phosphate 3.4g, triethylamine hydrochloride 1.5g, sodium dodecylsulfonate 1.5g, add water 600ml, stir to dissolve fully, add acetonitrile 305ml, add methanol 45ml, stir to clarify the solution, filter, Take the filtrate as the mobile phase; the flow rate is 1.0ml per minute, the detection wavelength is 262nm, and the column temperature is 40°C.

[0050] (2) Experimental steps

[0051] Take doxylamine succinate, impurity A (introduction of starting material), impurity B (intermediate impurity), impurity C (demethylation impurity), impurity D (starting material), impurity E (monooxidation impurity) respectively Appropriate amount, put in a 10ml measuring bottle, add 0.1M HCl to dissolve and dilute to the ...

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Abstract

The invention relates to the technical field of pharmaceutical analysis, in particular to a reversed-phase high-performance liquid chromatography detection method for related substances of doxylamine succinate and discloses an RT-HPLC detection method for the related substances of doxylamine succinate. The RT-HPLC detection method comprises the following steps of preparing an analyzing solution, setting chromatographic conditions and carrying out measurement on a machine. By means of the RT-HPLC detection method, various related impurities in a doxylamine succinate solution can be effectively measured, and separation of doxylamine succinate characteristic peaks and the related impurities in a spectrogram is especially achieved. Thus, it is ensured that the quality of products is controllable.

Description

technical field [0001] The invention relates to the technical field of drug analysis, in particular to a reversed-phase high-performance liquid chromatography detection method for related substances of doxylamine succinate. Background technique [0002] "Related substances" in drug analysis refer to substances such as starting materials, reagents, intermediates, by-products and isomers brought in during the production of raw materials And special impurities such as degradation products, polymers or crystal transformations generated during transportation. The type of related substances is closely related to the synthesis route and preparation process of the drug. Any change in any factor in the process of drug synthesis and preparation may lead to different types of related substances. Therefore, the detection and control process of related substances is relatively complicated. The detection of related substances is an important indicator for controlling the quality of drugs...

Claims

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Application Information

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IPC IPC(8): G01N30/89
CPCG01N30/89
Inventor 霍立茹张慧卢翔周杰张元元赵卿李战
Owner NANJING GRITPHARMA CO LTD
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