CN103558326A - 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
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- CN103558326A CN103558326A CN201310556108.4A CN201310556108A CN103558326A CN 103558326 A CN103558326 A CN 103558326A CN 201310556108 A CN201310556108 A CN 201310556108A CN 103558326 A CN103558326 A CN 103558326A
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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 (3)
1. the method for razaxaban content in high effective liquid chromatography for measuring razaxaban sheet, is characterized in that, it comprises the steps:
(1) preparation of reference substance solution: take razaxaban reference substance, add methyl alcohol: water (4:1) is made every 1ml containing the razaxaban solution of 0.5mg;
(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, and column temperature is 40~50 ℃, draws 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 effective liquid chromatography for measuring 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.
3. according to the method for razaxaban content in the high effective liquid chromatography for measuring razaxaban sheet described in claim 1, it is characterized in that: the volume ratio of described methyl alcohol, 0.01% phosphoric acid is 30:70.
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Cited By (6)
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CN103822997A (en) * | 2014-03-20 | 2014-05-28 | 山东新时代药业有限公司 | Analysis and detection method for rivaroxaban intermediate |
CN104730165A (en) * | 2015-03-23 | 2015-06-24 | 成都百裕科技制药有限公司 | High performance liquid chromatography (HPLC) detection method of Rivaroxaban |
CN104931595A (en) * | 2014-03-20 | 2015-09-23 | 山东新时代药业有限公司 | Method using high performance liquid chromatography (HPLC) to measure Rivaroxaban intermediate content |
CN105738489A (en) * | 2014-12-09 | 2016-07-06 | 重庆医药工业研究院有限责任公司 | Method for determining rivaroxaban and impurities thereof through adopting liquid chromatography |
CN106896164A (en) * | 2015-12-18 | 2017-06-27 | 重庆植恩药业有限公司 | A kind of razaxaban and the assay method about material |
CN115469038A (en) * | 2022-10-26 | 2022-12-13 | 苏州中化药品工业有限公司 | Method for extracting and detecting insoluble drug in jam and insoluble drug mixture |
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Cited By (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103822997A (en) * | 2014-03-20 | 2014-05-28 | 山东新时代药业有限公司 | Analysis and detection method for rivaroxaban intermediate |
CN104931595A (en) * | 2014-03-20 | 2015-09-23 | 山东新时代药业有限公司 | Method using high performance liquid chromatography (HPLC) to measure Rivaroxaban intermediate content |
CN105738489A (en) * | 2014-12-09 | 2016-07-06 | 重庆医药工业研究院有限责任公司 | Method for determining rivaroxaban and impurities thereof through adopting liquid chromatography |
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 |
CN104730165A (en) * | 2015-03-23 | 2015-06-24 | 成都百裕科技制药有限公司 | High performance liquid chromatography (HPLC) detection method of Rivaroxaban |
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 |
CN106896164A (en) * | 2015-12-18 | 2017-06-27 | 重庆植恩药业有限公司 | A kind of razaxaban and the assay method about material |
CN115469038A (en) * | 2022-10-26 | 2022-12-13 | 苏州中化药品工业有限公司 | Method for extracting and detecting insoluble drug in jam and insoluble drug mixture |
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 |
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