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Preparation method of impurity compound in ramelteon and prepared standard substance

A technology of ramelteon and compound, applied in the field of pharmacy, can solve the problem that there is no formula (I) and/or formula (II) compound standard preparation and sales, no formula (I) and/or formula (II) ) compounds, etc., to achieve the effects of easy availability of raw materials, low cost and suitable yield

Active Publication Date: 2015-03-11
ZHUHAI UNITED LAB
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] But do not have any record and report of the preparation separation method of formula (I) and / or formula (II) compound at present, more do not have the preparation of formula (I) and / or formula (II) compound standard substance used as analysis control and sales

Method used

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  • Preparation method of impurity compound in ramelteon and prepared standard substance
  • Preparation method of impurity compound in ramelteon and prepared standard substance
  • Preparation method of impurity compound in ramelteon and prepared standard substance

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0080] Step 1, preparation of ramelteon damage sample

[0081] Take 20 grams of ramelteon raw material (manufactured by Zhuhai United Laboratories Co., Ltd., batch number 140218), and place it at 160° C. for 2 hours to generate the impurities.

[0082] Step 2, HPLC Determination of Ramelteon Destruction Sample

[0083] High performance liquid chromatography: Shimadzu 20A HPLC (equipped with DAD detector);

[0084] Chromatographic column: Hypersil GOLD 5μ250×4.6mm;

[0085] Mobile phase A: 0.1% formic acid solution; Mobile phase B: acetonitrile;

[0086] Gradient: 0min (A: 90%, B: 10%), 5min (A: 90%, B: 10%), 45min (A: 40%, B: 60%), 50min (A: 10%, B: 90%), 51min (A: 90%, B: 10%), 60min (A: 90%, B: 10%);

[0087] Flow rate: 0.8ml / min;

[0088] Injection volume: 20μL;

[0089] Detection wavelength: 288nm.

[0090] Get above-mentioned destruction sample appropriate amount, be mixed with the solution that contains ramelteon about 2mg / ml with 50% acetonitrile-water, sample in...

Embodiment 2

[0116] Step 1, preparation of ramelteon damage sample

[0117] Take 10 grams of ramelteon raw material (manufactured by Zhuhai United Laboratories Co., Ltd., batch number 140218), and place it at 180° C. for 3 hours to generate the impurities.

[0118] Step 2, HPLC Determination of Ramelteon Destruction Sample

[0119] High performance liquid chromatography: Shimadzu 20A HPLC (equipped with DAD detector);

[0120] Chromatographic column: Hypersil GOLD 5μ250×4.6mm;

[0121] Mobile phase A: 0.1% formic acid solution; Mobile phase B: acetonitrile;

[0122] Gradient: 0min (A: 90%, B: 10%), 5min (A: 90%, B: 10%), 45min (A: 40%, B: 60%), 50min (A: 10%, B: 90%), 51min (A: 90%, B: 10%), 60min (A: 90%, B: 10%);

[0123] Flow rate: 0.8ml / min;

[0124] Injection volume: 20μL;

[0125] Detection wavelength: 288nm.

[0126] Get above-mentioned destruction sample appropriate amount, be mixed with the solution that contains ramelteon about 2mg / ml with 50% acetonitrile-water, sample in...

Embodiment 3

[0145] Step 1, preparation of ramelteon damage sample

[0146] Take 10 grams of ramelteon raw material (manufactured by Zhuhai United Laboratories Co., Ltd., batch number 140218), and place it at 140° C. for 1.5 hours to generate the impurities.

[0147] Step 2, HPLC Determination of Ramelteon Destruction Sample

[0148] High performance liquid chromatography: Shimadzu 20A HPLC (equipped with DAD detector);

[0149] Chromatographic column: Hypersil GOLD 5μ250×4.6mm;

[0150] Mobile phase A: 0.1% formic acid solution; Mobile phase B: acetonitrile;

[0151] Gradient: 0min (A: 90%, B: 10%), 5min (A: 90%, B: 10%), 45min (A: 40%, B: 60%), 50min (A: 10%, B: 90%), 51min (A: 90%, B: 10%), 60min (A: 90%, B: 10%);

[0152] Flow rate: 0.8ml / min;

[0153] Injection volume: 20μL;

[0154] Detection wavelength: 288nm.

[0155]Get above-mentioned destruction sample appropriate amount, be mixed with the solution that contains ramelteon about 2mg / ml with 50% acetonitrile-water, sample i...

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Abstract

The invention relates to the pharmaceutical field, and in particular provides a preparation method of an impurity compound type shown as formula (I) or / and formula (II) in ramelteon raw material and the prepared standard substance containing the compound shown as formula (I) or / and (II). The methods includes the steps of: 1) preparing the ramelteon material containing the compounds shown as formula (I) and / or (II) by using a preparative chromatography method, wherein the chromatographic conditions are chromatographic column of kromasil C18 10 mu 21.2*250 mm, a mobile phase of acetonitrile-water (45:55), flow rate of 30ml / min, and detection wavelength of 225nm; and respectively collecting the peaks of the compounds shown as formula (I) (relative retention time of 0.5) and formula (II) (relative retention time of 1.5).

Description

technical field [0001] The invention relates to the field of pharmacy, in particular to a method for preparing an impurity compound of ramelteon and a prepared standard product, which are used for quality analysis and inspection of the drug ramelteon. Background technique [0002] Ramelteon (Ramelteon), chemical name: N-[2-[(8S)-1,6,7,8-tetrahydro-2H-indeno[5,4-b]furan-8-yl] Ethyl] propionamide) is a new molecular drug developed by Japan's Takeda Corporation (TAKEDA) for the treatment of insomnia, chronic insomnia, and short-term insomnia. It was launched in the United States and Japan in 2005 and 2008, respectively. The drug is a melatonin receptor agonist, which can simulate the physiological effects of melatonin secreted by the pineal gland, which helps to regulate the sleep cycle and improve sleep quality. It has a strong affinity for melatonin receptors, but has no affinity for GABA receptors and opioid receptors, so it will not produce drug dependence; it has a defini...

Claims

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Application Information

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IPC IPC(8): C07D307/77
CPCC07D307/77
Inventor 马萍钟雅妮程玉宝熊渊刘俊华杜青波朱美容
Owner ZHUHAI UNITED LAB
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