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A kind of analytical detection method of ivabradine intermediate

A technology of ivabradine and detection method, applied in the field of high performance liquid chromatography analysis, can solve problems such as affecting the quality of final products, and achieve the effects of stable and reliable results, ensuring stability and simple operation

Active Publication Date: 2015-12-02
LUNAN PHARMA GROUP CORPORATION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] So far, USP, EP, BP, JP and Chinese Pharmacopoeia and literature do not record the analysis and detection methods of ivabradine intermediates, but the analysis and detection of ivabradine intermediates plays an important role in reaction control and yield improvement. It also directly affects the quality of the final product, so it is necessary to establish a stable and effective analytical method for quality control of ivabradine intermediates

Method used

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  • A kind of analytical detection method of ivabradine intermediate
  • A kind of analytical detection method of ivabradine intermediate
  • A kind of analytical detection method of ivabradine intermediate

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Experimental program
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Effect test

Embodiment 1

[0028] Instruments and conditions: Waterse2695 liquid chromatography system, Waters2489 UV / visible light detector, chromatographic column: WelchUltimateXB-C18 (4.6×250mm, 5μm); detection wavelength: 220nm; column temperature: 25°C; flow rate: 1.0mL / min; acetonitrile and 0.01mol / L sodium octane sulfonate solution (1mL phosphoric acid was added to 1L solution) was used as the mobile phase at a volume ratio of 40:60.

[0029] Experimental procedure: Dissolve the ivabradine intermediate with the mobile phase and quantitatively dilute it to make a solution containing 1.0 mg of the ivabradine intermediate per 1 mL, as the test solution; accurately measure 5 μL of the test solution for injection Phase chromatograph, carry out high performance liquid chromatography analysis according to above-mentioned conditions, record chromatogram, the result sees attached figure 1 .

[0030] attached figure 1 It shows that under the chromatographic conditions, the main peak of ivabradine interme...

Embodiment 2

[0032] Instruments and conditions: Waterse2695 liquid chromatography system, Waters2489 UV / visible light detector, chromatographic column: WelchUltimateXB-C18 (4.6×250mm, 5μm); detection wavelength: 220nm; column temperature: 25°C; flow rate: 0.7mL / min; acetonitrile and 0.02mol / L sodium octane sulfonate solution (1mL phosphoric acid was added to 1L solution) was used as the mobile phase at a volume ratio of 30:70.

[0033] Experimental procedure: Dissolve the ivabradine intermediate with the mobile phase and quantitatively dilute it to make a solution containing 1.0 mg of the ivabradine intermediate per 1 mL, as the test solution; accurately measure 5 μL of the test solution for injection Phase chromatograph, carry out high performance liquid chromatography analysis according to above-mentioned conditions, record chromatogram, the result sees attached figure 2 .

[0034] attached figure 2 It shows that under the chromatographic conditions, the main peak of ivabradine inter...

Embodiment 3

[0036] Instruments and conditions: Waterse2695 liquid chromatography system, Waters2489 UV / visible light detector, chromatographic column: WelchUltimateXB-C18 (4.6×250mm, 5μm); detection wavelength: 220nm; column temperature: 25°C; flow rate: 1.2mL / min; acetonitrile and 0.03mol / L sodium octane sulfonate solution (1mL of phosphoric acid was added to 1L solution) was used as the mobile phase at a volume ratio of 50:50.

[0037] Experimental procedure: Dissolve the ivabradine intermediate with the mobile phase and quantitatively dilute it to make a solution containing 1.0 mg of the ivabradine intermediate per 1 mL, as the test solution; accurately measure 5 μL of the test solution for injection Phase chromatograph, carry out high performance liquid chromatography analysis according to above-mentioned conditions, record chromatogram, the result sees attached image 3 .

[0038] attached image 3 It shows that under the chromatographic conditions, the main peak of ivabradine inte...

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Abstract

The invention relates to a method for analyzing and detecting an ivabradine intermediate. The method is used for quality control of the ivabradine intermediate. According to the method, octadecylsilane chemically bonded silica serves as a chromatographic column of packing (C18, 4.6*250mm, 5 micrometers), a solution system of acetonitrile and sodium 1-octanesulfonate-phosphoric acid serves as a mobile phase, the detection wavelength is 215-225nm, and high performance liquid chromatography is performed for analysis and detection. The analysis and detection method has the advantages of high separation degree, simple and convenient operation, high repeatability and durability and stable and reliable result.

Description

technical field [0001] The invention relates to a high-performance liquid chromatography analysis method, in particular to an analysis and detection method of an ivabradine intermediate. Background technique [0002] Ivabradine is a drug with a new mechanism for the treatment of angina pectoris. It has no effect on electrocardiographic conduction, myocardial contractility and ventricular repolarization. Its simple effect of slowing down the heart rate is the most important progress in the treatment of stable angina pectoris in recent years. [0003] 3-{3-[((7S)-3,4-Dimethoxy-8-bicyclo[4.2.0]oct-1,3,5-triene)methyl-methylamino]propyl}-7 ,8-dimethoxy-1,3,4,5-tetrahydro-2H-3-benzazepine-4-en-2-one is an important intermediate for the synthesis of ivabradine, and its molecular formula is C 27 h 34 N 2 o 5 , the molecular weight is 466.58, and the structural formula is as follows: [0004] [0005] So far, USP, EP, BP, JP and Chinese Pharmacopoeia and literature do not r...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
Inventor 赵志全赵亮亮
Owner LUNAN PHARMA GROUP CORPORATION