CN103558326B - Method for determining content of rivaroxaban in rivaroxaban tablet by high performance liquid chromatography - Google Patents
Method for determining content of rivaroxaban in rivaroxaban tablet by high performance liquid chromatography Download PDFInfo
- Publication number
- CN103558326B CN103558326B CN201310556108.4A CN201310556108A CN103558326B CN 103558326 B CN103558326 B CN 103558326B CN 201310556108 A CN201310556108 A CN 201310556108A CN 103558326 B CN103558326 B CN 103558326B
- Authority
- CN
- China
- Prior art keywords
- razaxaban
- performance liquid
- solution
- rivaroxaban
- high performance
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a method for determining the content of rivaroxaban in a rivaroxaban tablet by a high performance liquid chromatography. The method comprises the following steps: preparing a comparison product solution; preparing a testing product solution and determining, wherein a fixed phase of a high performance liquid chromatograph is octadecyl silane bonded silica gel and a mobile phase of the high performance liquid chromatograph is a mixed solution of methanol and 0.01% of phosphoric acid; the column temperature is 40-50 DEG C; and respectively absorbing 10 microliters of the comparison product solution and 10 microliters of the testing product solution; and injecting the solutions into a liquid chromatograph and reading data. According to the method, the content of the rivaroxaban in the rivaroxaban tablet is determined by adopting the high performance liquid chromatography; the method is high in separation efficiency, rapid in analyzing speed and high in detection sensitivity; the content of the rivaroxaban in the rivaroxaban tablet is determined so that the quality of the rivaroxaban tablet can be controlled and the stability of a product is controlled.
Description
Technical field
The present invention relates to high-efficient liquid phase chromatogram technology field, be specifically related to the method for razaxaban content in a kind of high effective liquid chromatography for measuring razaxaban sheet.
Background technology
Razaxaban sheet is a kind of antithrombotic reagent, and it does not need antithrombin Ⅲ to participate in, and directly antagonism dissociates and the Xa factor of combination.Razaxaban is main active in razaxaban sheet, by measuring razaxaban content, can well reflect the quality of razaxaban sheet.Therefore set up a method of measuring razaxaban content in razaxaban sheet, can better control the quality of razaxaban tablet, better control the stability of product.
Summary of the invention
The object of the invention is to set up a method of measuring razaxaban content in razaxaban sheet, can better control the quality of razaxaban sheet, better control the stability of product.
Technical scheme of the present invention is: the method for razaxaban content in high effective liquid chromatography for measuring razaxaban sheet, it comprises the steps:
(1) preparation of reference substance solution: take razaxaban reference substance, add methyl alcohol and make every 1ml methyl alcohol containing the solution of 0.5mg razaxaban;
(2) preparation of need testing solution: get razaxaban tablet and add methyl alcohol and make every 1ml methyl alcohol containing the solution of 0.5mg razaxaban;
(3) measure: the fixing of high efficiency liquid phase chromatography is octadecylsilane chemically bonded silica mutually, mobile phase is the mixed solution of first alcohol and water, and column temperature is 40～50 ℃, draws respectively each 5 μ l of reference substance solution and need testing solution, inject high performance liquid chromatograph, reading out data.
The detecting device of described high performance liquid chromatograph is ultraviolet absorption detector, and detection wavelength is 240nm.
Described methyl alcohol and 0.01% phosphoric acid volume ratio are 30:70.
The invention has the beneficial effects as follows: razaxaban content in the present invention's application high effective liquid chromatography for measuring razaxaban sheet, separation efficiency is high, analysis speed is fast, detection sensitivity is high, by detecting the content of razaxaban in razaxaban sheet, control in every razaxaban sheet containing razaxaban 10 ± 0.5mg, can control the quality of razaxaban sheet, better control the stability of product.
Form is described in further detail content of the present invention more by the following examples, but should not be interpreted as in the above-mentioned subject area of the present invention at this point and only limit to following examples.Do not departing under the above-mentioned technology prerequisite of the present invention, the corresponding replacement of making according to ordinary skill knowledge and customary means or the modification of change, include within the scope of the invention
.
Embodiment 1
The method of razaxaban content in high effective liquid chromatography for measuring razaxaban sheet, it comprises the steps:
(1) preparation of reference substance solution: take razaxaban reference substance, add methyl alcohol and make every 1ml methyl alcohol containing the solution of 0.5mg razaxaban;
(2) preparation of need testing solution: get razaxaban tablet powder and add methyl alcohol and make every 1ml methyl alcohol containing the solution of 4.25mg powder;
(3) measure: the fixing of high performance liquid chromatograph is octadecylsilane chemically bonded silica mutually, mobile phase is the mixed solution of methyl alcohol and 0.01% phosphoric acid, and column temperature is 40 ℃, draws respectively each 10 μ l of reference substance solution and need testing solution, inject high performance liquid chromatograph, reading out data.
Embodiment 2
The method of razaxaban content in high effective liquid chromatography for measuring razaxaban sheet, it comprises the steps:
(1) preparation of reference substance solution: take razaxaban reference substance, add methyl alcohol and make every 1ml methyl alcohol containing the solution of 0.5mg razaxaban;
(2) preparation of need testing solution: get razaxaban sheet powder and add methyl alcohol and make every 1ml methyl alcohol containing the solution of 4.25mg razaxaban;
(3) measure: the fixing of high performance liquid chromatograph is octadecylsilane chemically bonded silica mutually, mobile phase is the mixed solution of methyl alcohol and 0.01% phosphoric acid, and column temperature is 45 ℃, draws respectively each 10 μ l of reference substance solution and need testing solution, inject high performance liquid chromatograph, reading out data.
Embodiment 3
The method of razaxaban content in high effective liquid chromatography for measuring razaxaban sheet, it comprises the steps:
(1) preparation of reference substance solution: take razaxaban reference substance, add methyl alcohol and make every 1ml methyl alcohol containing the solution of 0.5mg razaxaban;
(2) preparation of need testing solution: get razaxaban sheet powder and add methyl alcohol and make every 1ml methyl alcohol containing the solution of 4.25mg razaxaban powder;
(3) measure: the fixing of high performance liquid chromatograph is octadecylsilane chemically bonded silica mutually, mobile phase is the mixed solution of methyl alcohol and 0.01% phosphoric acid, and column temperature is 50 ℃, draws respectively each 10 μ l of reference substance solution and need testing solution, inject high performance liquid chromatograph, reading out data.
In above-described embodiment, the detecting device of high performance liquid chromatograph is ultraviolet absorption detector, and detection wavelength is 240nm.The volume ratio of mobile phase methanol and 0.01% phosphoric acid is 30:70.
In above-described embodiment, razaxaban reference substance is purchased from Cato Research Chemicals Inc., and razaxaban sheet is produced purchased from Bayer Schering Pharma AG.
Claims (2)
1. the method for razaxaban content in high-performance liquid chromatogram determination razaxaban sheet, is characterized in that, it comprises the steps:
(1) preparation of reference substance solution: take razaxaban reference substance, add 80% methanol aqueous solution and make every 1ml containing the solution of 0.5mg razaxaban;
(2) preparation of need testing solution: get razaxaban sheet powder and add methyl alcohol and make every 1ml methyl alcohol containing the solution of 4.25mg powder;
(3) measure: the fixing of high performance liquid chromatograph is octadecylsilane chemically bonded silica mutually, mobile phase is the mixed solution of methyl alcohol, 0.01% phosphoric acid, its volume ratio is 30:70, column temperature is 40～50 ℃, draw respectively each 10 μ l of reference substance solution and need testing solution, inject high performance liquid chromatograph, reading out data.
2. according to the method for razaxaban content in the high-performance liquid chromatogram determination razaxaban sheet described in claim 1, it is characterized in that: the detecting device of described high performance liquid chromatograph is ultraviolet absorption detector, detection wavelength is 240nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310556108.4A CN103558326B (en) | 2013-11-12 | 2013-11-12 | Method for determining content of rivaroxaban in rivaroxaban tablet by high performance liquid chromatography |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310556108.4A CN103558326B (en) | 2013-11-12 | 2013-11-12 | Method for determining content of rivaroxaban in rivaroxaban tablet by high performance liquid chromatography |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103558326A CN103558326A (en) | 2014-02-05 |
| CN103558326B true CN103558326B (en) | 2014-10-15 |
Family
ID=50012634
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310556108.4A Active CN103558326B (en) | 2013-11-12 | 2013-11-12 | Method for determining content of rivaroxaban in rivaroxaban tablet by high performance liquid chromatography |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103558326B (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104931595B (en) * | 2014-03-20 | 2019-01-18 | 鲁南制药集团股份有限公司 | A method of with high effective liquid chromatography for measuring Rivaroxaban intermediate content |
| CN103822997B (en) * | 2014-03-20 | 2018-12-04 | 山东新时代药业有限公司 | A kind of analyzing detecting method of Rivaroxaban intermediate |
| CN105738489B (en) * | 2014-12-09 | 2020-01-31 | 重庆医药工业研究院有限责任公司 | method for determining rivaroxaban and impurities thereof by adopting liquid chromatography |
| CN104730165B (en) * | 2015-03-23 | 2016-05-25 | 成都百裕科技制药有限公司 | A kind of high-efficiency liquid chromatography method for detecting of razaxaban |
| CN105651871A (en) * | 2015-12-18 | 2016-06-08 | 重庆植恩药业有限公司 | Determination method of rivaroxaban and related substances |
| CN115469038B (en) * | 2022-10-26 | 2024-04-30 | 苏州中化药品工业有限公司 | Extraction and detection method of insoluble drugs in jam and insoluble drug mixture |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101821260A (en) * | 2007-08-14 | 2010-09-01 | 康塞特医药品有限公司 | Substituted oxazolidinone derivatives |
| CN102822167A (en) * | 2010-01-04 | 2012-12-12 | 埃南蒂亚有限公司 | Process for the preparation of rivaroxaban and intermediates thereof |
| CN103145698A (en) * | 2013-03-01 | 2013-06-12 | 江西同和药业有限责任公司 | Preparation method of Rivaroxaban midbody and novel synthetic method of Rivaroxaban |
| CN103217492A (en) * | 2013-03-26 | 2013-07-24 | 上海应用技术学院 | Separation determination method of rivaroxaban optical isomer |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AU2012378913B2 (en) * | 2012-05-02 | 2017-04-13 | Symed Labs Limited | Improved process for preparing rivaroxaban using novel intermediates |
-
2013
- 2013-11-12 CN CN201310556108.4A patent/CN103558326B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101821260A (en) * | 2007-08-14 | 2010-09-01 | 康塞特医药品有限公司 | Substituted oxazolidinone derivatives |
| CN102822167A (en) * | 2010-01-04 | 2012-12-12 | 埃南蒂亚有限公司 | Process for the preparation of rivaroxaban and intermediates thereof |
| CN103145698A (en) * | 2013-03-01 | 2013-06-12 | 江西同和药业有限责任公司 | Preparation method of Rivaroxaban midbody and novel synthetic method of Rivaroxaban |
| CN103217492A (en) * | 2013-03-26 | 2013-07-24 | 上海应用技术学院 | Separation determination method of rivaroxaban optical isomer |
Non-Patent Citations (16)
| Title |
|---|
| Ccedil * |
| Determination of rivaroxaban – a novel, oral, direct Factor Xa inhibitor–in human plasma by high-performance liquid chromatography–tandem mass spectrometry;G. Rohde;《Journal of Chromatography B》;20080901;第872卷(第1-2期);第43-50页 * |
| elebier et al.RP-HPLC method development and validation for estimation of rivaroxaban in pharmaceutical dosage forms.《Brazilian Journal of Pharmaceutical Sciences》.2013,第49卷(第2期), * |
| Fast, simultaneous quantification of three novel cardiac drugs in human urine by MEPS–UHPLC–MS/MS for therapeutic drug monitoring;Sylwia Magiera;《Journal of Chromatography B》;20131101;第938卷;第86-95页 * |
| G. Rohde.Determination of rivaroxaban – a novel, oral, direct Factor Xa inhibitor–in human plasma by high-performance liquid chromatography–tandem mass spectrometry.《Journal of Chromatography B》.2008,第872卷(第1-2期), |
| Joanne E. Adaway et al.Therapeutic drug monitoring and LC–MS/MS.《Journal of Chromatography B》.2012,第883-884卷 |
| Mustafa & * |
| Mustafa Ç |
| SylwiaMagiera.Fast simultaneous quantification of three novel cardiac drugs in human urine by MEPS–UHPLC–MS/MS for therapeutic drug monitoring.《Journal of Chromatography B》.2013 |
| Therapeutic drug monitoring and LC–MS/MS;Joanne E. Adaway et al;《Journal of Chromatography B》;20120201;第883-884卷;第33-49页 * |
| 利伐沙班合成工艺改进;苻坚 等;《安徽医药》;20130610;第17卷(第6期);第917-918页 * |
| 利伐沙班的合成;袁静 等;《中国新药杂志》;20101215;第19卷(第23期);第2185-2187页 * |
| 利伐沙班的合成工艺改进;杨银萍 等;《中国药物化学杂志》;20130220;第23卷(第1期);第26-29页 * |
| 杨银萍 等.利伐沙班的合成工艺改进.《中国药物化学杂志》.2013,第23卷(第1期), |
| 苻坚 等.利伐沙班合成工艺改进.《安徽医药》.2013,第17卷(第6期), |
| 袁静 等.利伐沙班的合成.《中国新药杂志》.2010,第19卷(第23期), |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103558326A (en) | 2014-02-05 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103558326B (en) | Method for determining content of rivaroxaban in rivaroxaban tablet by high performance liquid chromatography | |
| CN104237421A (en) | Related substance detection method for trelagliptin succinate and preparation thereof | |
| CN102507805B (en) | Method for detecting trichothecene compound in grain and solid phase extraction column for detection | |
| CN105486791A (en) | Fe3O4@SiO2@G magnetic adsorbent and method for detecting 16 anti-staling agents in vegetable by using same | |
| Han et al. | Analysis of some β-Lactam antibiotics using ionic liquids as mobile phase additives by RP-HPLC | |
| CN103743844B (en) | The assay method of ethanol content in methyl alcohol | |
| CN104297357B (en) | The content assaying method of methyl p-hydroxybenzoate and Sodium Benzoate in a kind of solution | |
| CN106198832A (en) | A kind of quality of production control method of intensified loquet distillate | |
| CN103954705A (en) | Method for measuring content of allantoin contained in Chinese traditional medicine rhizoma dioscoreae and rhizoma dioscoreae-containing preparation | |
| CN104198605B (en) | A kind of assay method of cigarette hot melt adhesive phenol antioxidant content | |
| Satheesh et al. | UPLC separation and quantification of related substances of varenicline tartrate tablet | |
| CN103063794B (en) | Content detecting and control method of epalrestat tablets | |
| CN101390984B (en) | Detection method of Lanhuayao | |
| Liang et al. | Direct preparation of a graphene oxide modified monolith in a glass syringe as a solid‐phase extraction cartridge for the extraction of quaternary ammonium alkaloids from Chinese patent medicine | |
| CN103063795B (en) | Methods for determining the content of imidafenacin and detecting related substances | |
| CN103513000A (en) | Method for carrying out identification and content measurement on nymphaea candida presl | |
| CN103728392A (en) | Method for separating and measuring prucalopride succinate related substances by liquid chromatography | |
| CN103454355A (en) | Method for analyzing and detecting content of monomer in polyacrylic resin latex solution (enteric type) product | |
| CN103487532A (en) | Method for separating and determining vilazodone hydrochloride raw materials and preparations thereof by liquid chromatography | |
| CN103713064B (en) | Method for determining related substances of bismuthyl ecabet by using high performance liquid chromatography | |
| CN103675187A (en) | Content determination method of sodium taurochenodeoxycholate in bile | |
| CN104655736A (en) | Analysis and detection method of L-thiazolidinyl-4-carboxylic acid | |
| CN104569213A (en) | Method for measuring content of (S)-(+)-N-(2,3-ethyoxyl propyl) phthalimide by adopting high performance liquid chromatography | |
| CN103163227A (en) | Method for determining related substances of Febuxostat and preparation thereof | |
| CN104267114A (en) | Detection method of nymphaea candida presl |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |