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Preparation method of impurity compound in ramelteon and prepared standard substance

A technology of ramelteon and compound, applied in preparation method and prepared standard, in the field of quality analysis and inspection of medicine ramelteon, and can solve the problem that there is no compound of formula (I) and/or formula (II), There are no problems such as preparation and sales of standard compounds of formula (I) and/or formula (II), and the effects of easy availability of raw materials, low cost and suitable yield are achieved

Active Publication Date: 2017-02-08
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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Patent Type & Authority Patents(China)
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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