Analysis and detection method for rivaroxaban intermediate

A detection method, the technology of rivaroxaban, which is applied in the field of high-performance liquid chromatography analysis, can solve the problems affecting the quality of the final product rivaroxaban, and achieve stable and reliable results, good repeatability and durability, and short analysis time Effect

Active Publication Date: 2014-05-28
SHANDONG NEWTIME PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] So far, the analysis and detection method of this intermediate has not been recorded in the literature, but the analysis and detection 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 analytical detection method for quality control of this intermediate

Method used

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  • Analysis and detection method for rivaroxaban intermediate
  • Analysis and detection method for rivaroxaban intermediate
  • Analysis and detection method for rivaroxaban intermediate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Instrument and conditions: Agilent1200 liquid chromatography system, chromatographic column: Agilent SB-C18 (4.6×150mm, 5μm), detection wavelength 245nm, column temperature 35°C, flow rate 1.0ml / min, mobile phase A is adjusted pH with triethylamine =3 of 0.5% perchloric acid aqueous solution, the mobile phase B is methanol, and the gradient elution settings are as follows:

[0026]

[0027] Experimental procedure: Dissolve the rivaroxaban intermediate in 40% (volume ratio) methanol aqueous solution and quantitatively dilute it to make a solution containing 1.0mg of rivaroxaban intermediate per 1ml, as the test solution, and accurately measure the 5 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 .

[0028] attached figure 1 It shows that under the chromatographic conditi...

Embodiment 2

[0030] Instrument and conditions: Agilent1200 liquid chromatography system, chromatographic column: Agilent SB-C18 (4.6×150mm, 5μm), detection wavelength 245nm, column temperature 35°C, flow rate 1.1ml / min, mobile phase A is adjusted pH with triethylamine =3.5 of 0.6% perchloric acid aqueous solution, the mobile phase B is methanol, and the gradient elution settings are as follows:

[0031]

[0032]

[0033] Experimental procedure: Dissolve the rivaroxaban intermediate in 40% (volume ratio) methanol aqueous solution and quantitatively dilute it to make a solution containing 1.0mg of rivaroxaban intermediate per 1ml, as the test solution, and accurately measure the 5 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 .

[0034] attached figure 2 It shows that under the chromat...

Embodiment 3

[0036] Instrument and conditions: Agilent1200 liquid chromatography system, chromatographic column: Agilent SB-C18 (4.6×150mm, 5μm), detection wavelength 245nm, column temperature 35°C, flow rate 0.7ml / min, mobile phase A is adjusted pH with triethylamine =2.5 of 0.4% perchloric acid aqueous solution, the mobile phase B is methanol, and the gradient elution settings are as follows:

[0037]

[0038] Experimental procedure: Dissolve the rivaroxaban intermediate in 40% (volume ratio) methanol aqueous solution and quantitatively dilute it to make a solution containing 1.0mg of rivaroxaban intermediate per 1ml, as the test solution, and accurately measure the 5 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 .

[0039] attached image 3 It shows that under the chromatographic condi...

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Abstract

The invention relates to an analysis and detection method for a rivaroxaban intermediate, which is particularly used for mass control on the rivaroxaban intermediate. A chromatographic column (C18, 4.6mm*150mm, 5 microns) which takes octadecyl silane bonded silica gel as a packing and a perchloric acid solution and methanol as flow phases are adopted for gradient elution, and analysis and detection are performed by a high performance liquid chromatography method under the conditions that the detection wavelength is 240nm-250nm, the column temperature is 30-40 DEG C and the velocity is 0.7-1.1 ml/min. By adopting the analysis and detection method provided by the invention, the rivaroxaban intermediate can be effectively separated from impurities of the rivaroxaban intermediate, and moreover, the method has the advantages of high separation degree and sensitivity, good repeatability and durability, short analysis time, simplicity in operation 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 for an intermediate of rivaroxaban. 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] 4-{4-[(5(s)-5-aminomethyl)-2-oxo-1,3-oxazolidin-3-yl]phenyl}morpholin-3-one hydrochloride is a synthetic An important intermediate of varoxaban, its chemical formula is C 14 h 18 ClN 3 o 4 , the structural formula is as follows: [0004] ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 李铁健郭玉
Owner SHANDONG NEWTIME PHARMA
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