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Method using high performance liquid chromatography (HPLC) to measure Rivaroxaban intermediate content

A technology of high performance liquid chromatography and rivaroxaban, which is applied in the field of high performance liquid chromatography to determine the content of rivaroxaban intermediates, can solve problems affecting the quality of the final product rivaroxaban, and achieve stable, reliable and repeatable results Good performance and durability, easy operation

Active Publication Date: 2015-09-23
LUNAN PHARMA GROUP CORPORATION
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AI Technical Summary

Problems solved by technology

[0005] So far, the content determination method of this intermediate has not been recorded in the literature, but the content determination of this intermediate has an important effect on reaction control and yield improvement, and also directly affects the quality of the final product rivaroxaban, so It is very necessary to establish a stable and effective assay method for quality control of this intermediate

Method used

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  • Method using high performance liquid chromatography (HPLC) to measure Rivaroxaban intermediate content
  • Method using high performance liquid chromatography (HPLC) to measure Rivaroxaban intermediate content
  • Method using high performance liquid chromatography (HPLC) to measure Rivaroxaban intermediate content

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Effect test

Embodiment 1

[0025] Instrument and conditions: Agilent1200 liquid chromatography system, chromatographic column: Agilent SB-C18 (4.6×150mm, 5μm), detection wavelength 241nm, column temperature 25°C, flow rate 1.0ml / min, the volume ratio of 0.1% phosphoric acid aqueous solution to acetonitrile is 70:30.

[0026] Experimental procedure: Dissolve the rivaroxaban intermediate with 30% (volume ratio) acetonitrile aqueous solution and quantitatively dilute to make a solution containing 0.3 mg of rivaroxaban intermediate per 1 ml, as the test solution, and accurately measure the 20 μ l of the test solution was injected into the liquid chromatograph, and the high-performance liquid chromatography was analyzed according to the above conditions, and the chromatogram was recorded. The results are shown in the attached figure 1 .

[0027] attached figure 1 It shows that under the chromatographic conditions, the rivaroxaban intermediate peak and the impurity peak can be completely separated, the reso...

Embodiment 2

[0029] Instrument and conditions: Agilent1200 liquid chromatography system, chromatographic column: Agilent SB-C18 (4.6×150mm, 5μm), detection wavelength 241nm, column temperature 25°C, flow rate 1.1ml / min, the volume ratio of 0.1% phosphoric acid aqueous solution to acetonitrile is 80:20.

[0030] Experimental procedure: Dissolve the rivaroxaban intermediate with 30% (volume ratio) acetonitrile aqueous solution and quantitatively dilute to make a solution containing 0.3 mg of rivaroxaban intermediate per 1 ml, as the test solution, and accurately measure the 20 μ l of the test solution was injected into the liquid chromatograph, and the high-performance liquid chromatography was analyzed according to the above conditions, and the chromatogram was recorded. The results are shown in the attached figure 2 .

[0031] attached figure 2 It shows that under the chromatographic conditions, the rivaroxaban intermediate peak and the impurity peak can be completely separated, the re...

Embodiment 3

[0033] Instrument and conditions: Agilent1200 liquid chromatography system, chromatographic column: Agilent SB-C18 (4.6×150mm, 5μm), detection wavelength 241nm, column temperature 25°C, flow rate 0.7ml / min, the volume ratio of 0.1% phosphoric acid aqueous solution to acetonitrile is 60:40.

[0034] Experimental procedure: Dissolve the rivaroxaban intermediate with 30% (volume ratio) acetonitrile aqueous solution and quantitatively dilute to make a solution containing 0.3 mg of rivaroxaban intermediate per 1 ml, as the test solution, and accurately measure the 20 μ l of the test solution was injected into the liquid chromatograph, and the high-performance liquid chromatography was analyzed according to the above conditions, and the chromatogram was recorded. The results are shown in the attached image 3 .

[0035] attached image 3 It shows that under the chromatographic conditions, the rivaroxaban intermediate peak and the impurity peak can be completely separated, the reso...

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Abstract

The invention relates to a method using high performance liquid chromatography (HPLC) to measure the Rivaroxaban intermediate content. The method is used to control the quality of Rivaroxaban intermediate. In HPLC, a chromatography column (4.6*150 mm, 5[mu]m) is filled with octadecyl silane bonded silica gel, and an acidic water solution and an organic modifier are taken as the mobile phase. The provided method can effectively separate Rivaroxaban intermediate from other impurities, and has the advantages of high separation degree and sensitivity, good repeatability and durability, short analysis time, simple operation, and reliable and stable results.

Description

technical field [0001] The invention relates to a high performance liquid chromatography analysis method, in particular to a method for measuring the content of rivaroxaban intermediates by high performance liquid chromatography. Background technique [0002] Rivaroxaban, known in English as Rivaroxban, is an oral direct inhibitor of factor Xa jointly developed by Bayer and Johnson & Johnson. It was first launched in Canada in 2008. Rivaroxaban is mainly used to prevent hip or knee replacements After the formation of deep vein thrombosis and pulmonary embolism in patients, it can also be used to prevent stroke and non-central nervous system embolism in patients with non-valvular atrial fibrillation, and reduce the risk of coronary artery syndrome recurrence. [0003] (S)-2-({2-oxo-3-[4-(3-oxo-4-morpholinyl)phenyl]-1,3-oxazolidin-5-yl}methyl)- 1H-isoindole-1,3-dione is an important intermediate in the synthesis of rivaroxaban, and its chemical formula is C 22 h 19 N 3 o ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 赵志全杨欣茹徐勤娟
Owner LUNAN PHARMA GROUP CORPORATION
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