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Method for determining ramelteon and impurities thereof through high-performance liquid chromatography separation

A technology of high performance liquid chromatography and ramelteon, applied in the field of separation and determination of ramelteon and its impurities by high performance liquid chromatography, to achieve the effect of ensuring quality controllability

Active Publication Date: 2016-01-27
NANJING CHANGAO PHARMA SCI & TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] There is no bibliographical report about the separation and determination method of ramelteon and the above-mentioned eight impurities at present, and finding a method that can separate and measure ramelteon and the eight impurities is useful for controlling the quality of ramelteon and improving the curative effect of drugs , It is imminent to reduce the toxic and side effects

Method used

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  • Method for determining ramelteon and impurities thereof through high-performance liquid chromatography separation
  • Method for determining ramelteon and impurities thereof through high-performance liquid chromatography separation
  • Method for determining ramelteon and impurities thereof through high-performance liquid chromatography separation

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Experimental program
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Effect test

Embodiment 1

[0045] Instrument: Diana U3000PDA high performance liquid chromatograph;

[0046] Chromatographic column: Agilent ZORBAXSB-AQC18 chromatographic column (4.6mm×250mm, 5μm);

[0047] Mobile phase: mobile phase A is 0.1% triethylamine solution (adjust pH 6.0 with phosphoric acid), mobile phase B is acetonitrile, carry out gradient elution according to the following table:

[0048]

[0049] Column temperature: 30°C;

[0050] Flow rate: 1.0ml / min;

[0051] Detection wavelength: 230nm.

[0052] Preparation of positioning solution: take appropriate amount of LM-1, S-IBU, impurity 1, impurity 2, impurity 3, impurity 4, impurity 5, impurity 6, ramelteon reference substance, respectively add 50% acetonitrile solution to dissolve and dilute Prepare a solution containing 1mg per 1ml as a positioning solution.

[0053]The preparation of ramelteon and impurity mixed solution: get about 10mg of ramelteon test sample, accurately weighed, put in 10ml measuring bottle, add precisely 0.1m...

Embodiment 2

[0060] Instrument: Diana U3000 high performance liquid chromatography;

[0061] Chromatographic column: DikmaC18 chromatographic column (4.6mm×250mm, 5μm);

[0062] Mobile phase: mobile phase A is 0.1% triethylamine solution (adjust pH 3.0 with phosphoric acid), mobile phase B is acetonitrile, carry out gradient elution according to the following table:

[0063]

[0064] Column temperature: 30°C;

[0065] Flow rate: 1.0ml / min;

[0066] Detection wavelength: 230nm.

[0067] Solution preparation method and assay method are carried out according to embodiment 1, the collection of illustrative plates of ramelteon system suitability solution, ramelteon need testing solution, ramelteon sheet solution, ramelteon sheet blank excipient solution see respectively Figure 5 , 6 , 7, 8.

Embodiment 3

[0069] Instrument: Agilent1200HPLC;

[0070] Chromatographic column: Phenomenexluna-C18 chromatographic column (4.6mm×250mm, 5μm);

[0071] Mobile phase: mobile phase A is 0.1% triethylamine solution (adjust pH 7.5 with phosphoric acid), mobile phase B is acetonitrile, carry out gradient elution according to the following table:

[0072]

[0073]

[0074] Column temperature: 30°C;

[0075] Flow rate: 1.5ml / min;

[0076] Detection wavelength: 230nm.

[0077] Solution preparation method and assay method are carried out according to embodiment 1, the collection of illustrative plates of ramelteon system suitability solution, ramelteon need testing solution, ramelteon tablet powder solution, ramelteon tablet blank excipient solution see respectively Figure 9 , 10 , 11, 12.

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Abstract

The present invention discloses a method for determining ramelteon and impurities thereof through high-performance liquid chromatography separation. The technical scheme comprises that: the chromatographic conditions comprise that octadecylsilane bonded silica gel is adopted as a filler, 0.1% triethylamine solution-acetonitrile is adopted as a mobile phase, the detection wavelength is 210-310 nm, the column temperature is 20-45 DEG C, the mobile phase velocity is 0.5-2.0 ml / min, and the triethylamine solution is formed by adjusting the pH value of triethylamine with a volume fraction of 1% to 3.0-7.5 with phosphoric acid; the sample solution preparation comprises using a polar solvent to respectively prepare solutions respectively containing 0.01-2.0 mg / ml of ramelteon and 0.01-2.0 mg / ml of impurities; and the determination comprises: injecting the solution into a high-performance liquid chromatograph, recording the chromatogram, and analyzing. With the method of the present invention, the quantitative analysis can be performed on the related substances of the bulk drug ramelteon and the preparation thereof so as to ensure the quality controllability of the ramelteon and the preparation thereof.

Description

technical field [0001] The invention belongs to the field of drug analysis, in particular to a method for separating and measuring ramelteon and its impurities through high-performance liquid chromatography. Background technique [0002] Ramelteon (Ramelteon) is a new molecular drug developed by Japan's Takeda Corporation (TAKEDA) for the treatment of insomnia, chronic insomnia and short-term insomnia. Hormone receptor agonist, also has definite curative effect on chronic insomnia and short-term insomnia. Because this product has no dependence and drug abuse tendency, FDA lists it as an unregulated hypnotic drug. Ramelteon was launched in the U.S. in 2005, under the trade name: ROZEREM, and in Japan in 2008, under the trade name: ロゼレム [0003] The chemical name of ramelteon is (S)-N-[2-(1,6,7,8-tetrahydro-2H-indeno-[5,4-b]furan-8-yl)ethyl] Propionamide, molecular formula: C 16 h 21 NO 2 , the structural formula is as follows: [0004] [0005] Common adverse reac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 朱丽君崔金凤李纬范婧黄海燕李战
Owner NANJING CHANGAO PHARMA SCI & TECH CO LTD
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