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Method for determining rivaroxaban and related substances thereof

A technology of related substances and determination methods, applied in the field of medicinal chemical analysis, can solve the problems of poor separation of impurity peaks and impurity peaks near the main peak, and achieve the effects of good column efficiency, reduced baseline interference, and improved time efficiency.

Active Publication Date: 2021-03-26
JIANGSU SINOBIOPHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The object of the present invention is to provide a kind of rivaroxaban and its related substances that do not contain ion pairs, use core-shell type chromatographic column, can separate more impurities and solve the impurity peak separation problem near the main peak and the main peak. test methods

Method used

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  • Method for determining rivaroxaban and related substances thereof
  • Method for determining rivaroxaban and related substances thereof
  • Method for determining rivaroxaban and related substances thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] The method for separating and measuring rivaroxaban and its impurities specifically includes the following contents:

[0056] 1) Instruments and conditions

[0057] Instrument: high performance liquid chromatography; chromatographic column: core-shell chromatographic column with octadecylsilane bonded silica gel as filler, model is Agilent Poroshell 120EC-C18, 150×4.6mm, 2.7μm or equivalent Chromatographic column; detector detection wavelength: 250nm; mobile phase flow rate: 1.2ml / min; mobile phase A: with 10mmol / mL potassium dihydrogen phosphate buffer solution (1.36g potassium dihydrogen phosphate adds water 1000ml, adds 200 μ l phosphoric acid)-methanol ( 95:5) is mobile phase A; mobile phase B: acetonitrile-methanol-water (50:30:20) is mobile phase B; diluent: acetonitrile-water (70:30); column temperature is 50 ° C; The elution gradient is shown in Table 2 below:

[0058]

[0059] Table 2

[0060] Injection volume: 5 μl.

[0061] 2) Experimental steps

[00...

Embodiment 2

[0072] 1) on the basis of embodiment 1, adjust the flow rate to be 1.0ml / min

[0073] 2) The experimental results are shown in Table 4 below:

[0074]

[0075]

[0076] Table 4

[0077] Result: Baseline separation can be achieved between each component, which meets the separation requirements of the Pharmacopoeia, and the blank solvent does not interfere with the detection of each component (such as Figure 5-6 and Table 4).

Embodiment 3

[0079] 1) on the basis of embodiment 1, adjust the flow rate to be 1.4ml / min

[0080] 2) The experimental results are shown in Table 5 below:

[0081]

[0082] table 5

[0083] Results: The baseline separation of each component can be achieved, which meets the separation requirements of the Pharmacopoeia, and the blank solvent does not interfere with the detection of each component. (Such as Figure 7-8 and shown in Table 5).

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Abstract

The invention provides a method for determining rivaroxaban and related substances thereof, which comprises the following steps: performing determining by high performance liquid chromatography, dissolving rivaroxaban in a diluent to obtain a sample solution, and injecting the sample solution into a high performance liquid chromatograph with a core-shell chromatographic column as a stationary phase, carrying out gradient elution on the sample solution by adopting a flowing phase without an ion pair reagent, performing separating to obtain an eluent, and injecting the eluent into a detector fordetermination. According to the method, a core-shell chromatographic column is adopted, the column efficiency is good, and good peak pattern and separation can be brought; meanwhile, a mobile phase does not contain an ion pair reagent, so that various ghost peaks generated in an analysis process are avoided, the interference of a baseline is effectively reduced, the sensitivity of impurity detection is greatly improved, various processes and degradation impurities in rivaroxaban can be separated at the same time, and the method has important significance in impurity control and product safetyprocedures in rivaroxaban bulk drugs.

Description

technical field [0001] The invention relates to a method for determining rivaroxaban and related substances thereof, and belongs to the technical field of medical chemical analysis. Background technique [0002] Rivaroxaban is an oral anticoagulant that directly inhibits coagulation factor Xa with high selectivity, and its molecular formula is C19H 18 ClN 3 o 5 S, chemical name: 5-chloro-N-({(5S)-2-oxo-3-[4-(3-oxo-4-morpholinyl)-phenyl]-1,3-oxo Oxazolidine-5-yl}-methyl)-2-thiophene-carboxamide, its structural formula is: [0003] [0004] During the chemical synthesis of rivaroxaban, due to the residual intermediates of starting materials and the occurrence of side reactions in chemical reactions, various intermediates, side reaction impurities and degradation products are inevitably contained in the raw materials. In order to ensure the quality of rivaroxaban API, scientific analysis methods are required to detect and control various impurities in it. [0005] The r...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 张晓飞黄乐群
Owner JIANGSU SINOBIOPHARMA
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