CN108680658A - A kind of detection method of sirolimus - Google Patents
A kind of detection method of sirolimus Download PDFInfo
- Publication number
- CN108680658A CN108680658A CN201810258009.0A CN201810258009A CN108680658A CN 108680658 A CN108680658 A CN 108680658A CN 201810258009 A CN201810258009 A CN 201810258009A CN 108680658 A CN108680658 A CN 108680658A
- Authority
- CN
- China
- Prior art keywords
- sirolimus
- antioxidant
- acetonitrile solution
- acetonitrile
- solution
- 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.)
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
Abstract
A kind of detection method of claimed sirolimus comprising following steps：Prepare the most stable of phosphate buffer of sirolimus；Prepare the acetonitrile solution containing antioxidant；Sample to be tested is dissolved in containing in antioxidant acetonitrile solution again, obtains the acetonitrile solution of sirolimus, sample to be tested is dissolved in containing in antioxidant acetonitrile, phosphate buffer constant volume；Sirolimus standard items contain in antioxidant acetonitrile solution, phosphate buffer constant volume simultaneously dilutes, and sample introduction standard items and testing sample solution to high performance liquid chromatography, are mapped with standard solution test result respectively, regression equation is calculated, equation calculation concentration is brought into sample tests.The detection method of the sirolimus of the present invention dissolves sirolimus using more stable solvent, and sirolimus solution and sirolimus standard items to be measured is made more to stablize, and reduces sirolimus and degrades over time the influence to test.
Description
Technical field
The present invention relates to field of medical technology, and in particular to a kind of detection method of sirolimus.
Background technology
Sirolimus (Sirolimus) belongs to macrolide antibiotics, has immunosuppressive action, penetrates cell membrane
It can be combined with FKBP-12 (FK506 binding protein) and generate Sirolimus-FKBP-12 compounds, inhibit the work of mTOR kinases
Property, to play the role of inhibiting cell Proliferation.The detection generally use high performance liquid chromatography of micro sirolimus is with acetonitrile
The mixture of solution, acetonitrile and water is detected for mobile phase, and sirolimus is sensitive to soda acid, and the unstable of solution be easy to cause
Sirolimus is degraded.
Invention content
The present invention is directed to current sirolimus problem of easy degradation, and the more stable solvent of use and antioxidant are to western sieve
Department is not dissolved, and is reduced sirolimus and is degraded over time the influence to test.
The purpose of the present invention is what is be achieved through the following technical solutions：A kind of detection method of sirolimus comprising such as
Lower step：
(1) prepare the most stable of phosphate buffer of sirolimus prevents the change of pH value for preparing sirolimus solution
Change causes sirolimus to degrade；
(2) appropriate antioxidant is added in acetonitrile, the acetonitrile solution containing antioxidant is made, prevents sirolimus from existing
Oxidative degradation in solution；
(3) A. by sample to be tested be dissolved in step (2) containing in antioxidant acetonitrile solution, obtain the acetonitrile of sirolimus
Solution,
B. take known weight sirolimus standard items be dissolved in step (2) containing obtaining western sieve in antioxidant acetonitrile solution
The acetonitrile solution of standard items is not taken charge of；
(4) phosphate buffer and constant volume of step (1) is added in the acetonitrile solution of A. sirolimus, obtains prepare liquid,
B. the phosphate buffer and constant volume of step (1) is added in the acetonitrile solution of sirolimus standard items, is diluted to respectively
A plurality of various concentrations are prepared as titer for standard curve；
(5) it is detected in sample introduction prepare liquid and titer to high performance liquid chromatography respectively, with a plurality of various concentrations
Titer measurement result does figure, obtains regression equation, and prepare liquid sirolimus concentration is calculated.
In currently preferred technical solution, in step (5), done with the titer measurement result of 3-10 various concentration
Figure, obtains regression equation.
The detection method of the sirolimus of the present invention is directed to current sirolimus problem of easy degradation, what use was more stablized
Solvent dissolves sirolimus, so that sirolimus solution and sirolimus standard items to be measured is more stablized, reduces western sieve
Department does not degrade over time the influence to test.
Description of the drawings
Fig. 1 is one embodiment flow chart of detection method for preparing the sirolimus of the present invention.
Specific implementation mode
To further understand the present invention, preferred embodiment of the present invention is described with reference to specific embodiment, but answered
Work as understanding, these descriptions are only the feature and advantage further illustrated the present invention, rather than to the limit of the claims in the present invention
System.
Said program is described further below in conjunction with specific embodiment.The implementation condition used in embodiment can root
Further adjustment is done according to the condition of specific producer, the implementation condition being not specified is usually the condition in routine experiment.
Embodiment 1
A kind of detection method of sirolimus comprising following steps：
(1) according to previous experiments data and documents and materials, the phosphate buffer of sirolimus most stable pH value is prepared,
For preparing sirolimus solution, prevent the variation of pH value from sirolimus being caused to degrade；
(2) appropriate antioxidant is added in acetonitrile, the acetonitrile solution containing antioxidant is made, prevents sirolimus from existing
Oxidative degradation in solution；
(3) sample to be tested is dissolved in a certain amount of acetonitrile solution containing antioxidant by A., obtains the acetonitrile of sirolimus
Solution,
B. it takes known weight sirolimus standard items to be dissolved in a certain amount of acetonitrile solution containing antioxidant and obtains western sieve
The acetonitrile solution of standard items is not taken charge of；
(4) phosphate buffer and constant volume are added in the acetonitrile solution of A. sirolimus, obtains prepare liquid,
B. phosphate buffer and constant volume are added in the acetonitrile solution of sirolimus standard items, it is different in being diluted to 5 respectively
Concentration is prepared as titer for standard curve.
(5) it is detected in sample introduction prepare liquid and titer to high performance liquid chromatography respectively, with the standard of 5 various concentrations
Liquid measurement result does figure, obtains regression equation, and prepare liquid sirolimus concentration is calculated.
Sirolimus can be significantly kept with the solution of the acetonitrile containing antioxidant and phosphate buffered saline
Stability slows down the decomposition rate of sirolimus, reduces the detection error that degradation is brought.
The technology contents and technical characteristic of the present invention have revealed that as above, however those skilled in the art still may base
Make various replacements and modification without departing substantially from spirit of that invention, therefore, the scope of the present invention in teachings of the present invention and announcement
It should be not limited to the revealed content of embodiment, and should include various replacements and modification without departing substantially from the present invention, and be this patent Shen
Please claim covered.
Claims (2)
1. a kind of detection method of sirolimus comprising following steps：
(1) the most stable of phosphate buffer of sirolimus is prepared；
(2) appropriate antioxidant is added in acetonitrile, the acetonitrile solution containing antioxidant is made；
(3) A. by sample to be tested be dissolved in step (2) containing in antioxidant acetonitrile solution, the acetonitrile for obtaining sirolimus is molten
Liquid,
B. take known weight sirolimus standard items be dissolved in step (2) containing obtaining sirolimus in antioxidant acetonitrile solution
The acetonitrile solution of standard items；
(4) phosphate buffer and constant volume of step (1) is added in the acetonitrile solution of A. sirolimus, obtains prepare liquid,
B. the phosphate buffer and constant volume of step (1) is added in the acetonitrile solution of sirolimus standard items, is diluted to plural number respectively
A various concentration is prepared as titer for standard curve；
(5) it is detected in sample introduction prepare liquid and titer to high performance liquid chromatography respectively, with the standard of a plurality of various concentrations
Liquid measurement result does figure, obtains regression equation, and prepare liquid sirolimus concentration is calculated.
2. detection method according to claim 1, which is characterized in that in step (5), with the standard of 3-10 various concentration
Liquid measurement result does figure, obtains regression equation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810258009.0A CN108680658A (en) | 2018-03-27 | 2018-03-27 | A kind of detection method of sirolimus |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810258009.0A CN108680658A (en) | 2018-03-27 | 2018-03-27 | A kind of detection method of sirolimus |
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| CN108680658A true CN108680658A (en) | 2018-10-19 |
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| CN201810258009.0A Pending CN108680658A (en) | 2018-03-27 | 2018-03-27 | A kind of detection method of sirolimus |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114137120A (en) * | 2021-11-29 | 2022-03-04 | 赛诺神畅医疗科技有限公司 | Method for detecting related substances in rapamycin drug stent |
Citations (7)
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| US20050288481A1 (en) * | 2004-04-30 | 2005-12-29 | Desnoyer Jessica R | Design of poly(ester amides) for the control of agent-release from polymeric compositions |
| CN101129361A (en) * | 2007-07-17 | 2008-02-27 | 山东华诺生物科技有限公司 | Sirolimus lipidosome freeze-dried acanthopanax powder and technique of preparing the same |
| CN101273967A (en) * | 2007-11-22 | 2008-10-01 | 山东蓝金生物工程有限公司 | Anticancer sustained-release injection containing neovascularization inhibitor |
| CN101522690A (en) * | 2006-07-25 | 2009-09-02 | 艾博特公司 | Crystalline forms of rapamycin analogs |
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2018
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| CN101522690A (en) * | 2006-07-25 | 2009-09-02 | 艾博特公司 | Crystalline forms of rapamycin analogs |
| CN101129361A (en) * | 2007-07-17 | 2008-02-27 | 山东华诺生物科技有限公司 | Sirolimus lipidosome freeze-dried acanthopanax powder and technique of preparing the same |
| CN101273967A (en) * | 2007-11-22 | 2008-10-01 | 山东蓝金生物工程有限公司 | Anticancer sustained-release injection containing neovascularization inhibitor |
| CN106153756A (en) * | 2015-04-25 | 2016-11-23 | 山东新时代药业有限公司 | A kind of detect the high performance liquid chromatography of rapamycin in everolimus |
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| 徐文俊 等: "西罗莫司及其药物支架体内释放度的HPLC法测定", 《中国医药工业杂质》 * |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114137120A (en) * | 2021-11-29 | 2022-03-04 | 赛诺神畅医疗科技有限公司 | Method for detecting related substances in rapamycin drug stent |
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Application publication date: 20181019 |
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