CN103822996A - Measuring method of content of perindopril tert-butylamine salt - Google Patents
Measuring method of content of perindopril tert-butylamine salt Download PDFInfo
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- CN103822996A CN103822996A CN201410104469.XA CN201410104469A CN103822996A CN 103822996 A CN103822996 A CN 103822996A CN 201410104469 A CN201410104469 A CN 201410104469A CN 103822996 A CN103822996 A CN 103822996A
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- butylamine salt
- perindopril tert
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- perindopril
- tert
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Abstract
The invention discloses a measuring method of the content of a perindopril tert-butylamine salt. The measuring method comprises the following steps: testing system suitability; selecting a filling agent and a flowing phase; dissolving a proper amount of perindopril tert-butylamine salt and a proper amount of perindopril tert-butylamine salt reference substance by adding the flowing phase, diluting and evenly shaking so as to prepare a solution; weighing a proper amount of the solution and injecting into a liquid chromatograph; recording a chromatogram and measuring a peak area or a peak height; and finally, calculating the content of the perindopril tert-butylamine salt according to an external standard method. As the method is used, the defect of low measuring accuracy of the potentiometric titration method in the prior art is overcome; and the measuring accuracy and the measuring precision of the content of the perindopril tert-butylamine salt are effectively improved.
Description
Technical field
The invention belongs to pharmaceutical technology field, be specifically related to a kind of assay method of perindopril tert-butylamine salt content.
Background technology
In prior art, the mensuration of perindopril tert-butylamine salt content generally adopts potentiometric determination, concrete mensuration process is: get the about 0.16g of perindopril tert-butylamine salt sample, accurately weighed, add glacial acetic acid 50ml, aceticanhydride 5ml, ultrasonic making dissolved, according to potentiometric titration, with perchloric acid titration liquid (0.1mol/L) titration, and the result of titration is proofreaied and correct with blank test, this content assaying method accuracy, precision are all poor.
Summary of the invention
Goal of the invention: the object of the invention is, in order to solve deficiency of the prior art, provides a kind of assay method of perindopril tert-butylamine salt content.
Technical scheme: the assay method of a kind of perindopril tert-butylamine salt content of the present invention, comprises the following steps:
(1) system suitability: the number of theoretical plate to chromatographic column, degree of separation, repeatability, tailing factor are tested respectively;
(2) selection of filling agent and mobile phase: employing octadecylsilane chemically bonded silica is filling agent, take methyl alcohol-phosphate buffer (55:45) as mobile phase, detection wavelength is 210-215nm; Column temperature 40-42 ℃;
(3) get perindopril tert-butylamine salt sample appropriate, accurately weighed, add the mutual-assistance of flowing and dissolves and dilute and shake up, make the solution that approximately contains 0.4mg in every 1ml, precision measures 20 μ l, and injection liquid chromatography, records chromatogram; And measure peak area or peak height;
(4) separately get perindopril tert-butylamine salt reference substance appropriate, accurately weighed, add mobile phase and dissolve and dilute and make in every 1ml the approximately solution containing 0.4mg, precision measures 20 μ l, and injection liquid chromatography, records chromatogram; And measure peak area or peak height;
(5) according in step (3) and (4) the data of surveying calculate the content of perindopril tert-butylamine salt according to external standard method.
As preferably, described in step (2), phosphate buffer is by 2-3g potassium dihydrogen phosphate, 3-5ml phosphoric acid, and 3-5ml triethylamine is dissolved in water and is diluted to 1000ml.
Beneficial effect: assay method of the present invention has solved the not high shortcoming of potentiometric titration accuracy of measurement in prior art, has effectively improved accuracy, the precision of perindopril tert-butylamine salt assay.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described:
Embodiment 1
An assay method for perindopril tert-butylamine salt content, comprises the following steps:
(1) system suitability: the number of theoretical plate to chromatographic column, degree of separation, repeatability, tailing factor are tested respectively;
(2) selection of filling agent and mobile phase: employing octadecylsilane chemically bonded silica is filling agent, take methyl alcohol-phosphate buffer (55:45) as mobile phase, wherein phosphate buffer is by 2g potassium dihydrogen phosphate, 3ml phosphoric acid, 3ml triethylamine is dissolved in water and is diluted to 1000ml, and detection wavelength is 210nm; 40 ℃ of column temperatures;
(3) get perindopril tert-butylamine salt sample appropriate, accurately weighed, add the mutual-assistance of flowing and dissolves and dilute and shake up, make the solution that approximately contains 0.4mg in every 1ml, precision measures 20 μ l, and injection liquid chromatography, records chromatogram; And measure peak area or peak height;
(4) separately get perindopril tert-butylamine salt reference substance appropriate, accurately weighed, add mobile phase and dissolve and dilute and make in every 1ml the approximately solution containing 0.4mg, precision measures 20 μ l, and injection liquid chromatography, records chromatogram; And measure peak area or peak height;
(5) according in step (3) and (4) the data of surveying calculate the content of perindopril tert-butylamine salt according to external standard method.
Embodiment 2
An assay method for perindopril tert-butylamine salt content, comprises the following steps:
(1) system suitability: the number of theoretical plate to chromatographic column, degree of separation, repeatability, tailing factor are tested respectively;
(2) selection of filling agent and mobile phase: employing octadecylsilane chemically bonded silica is filling agent, take methyl alcohol-phosphate buffer (55:45) as mobile phase, wherein phosphate buffer is by 3g potassium dihydrogen phosphate, 5ml phosphoric acid, 5ml triethylamine is dissolved in water and is diluted to 1000ml, and detection wavelength is 215nm; 42 ℃ of column temperatures;
(3) get perindopril tert-butylamine salt sample appropriate, accurately weighed, add the mutual-assistance of flowing and dissolves and dilute and shake up, make the solution that approximately contains 0.4mg in every 1ml, precision measures 20 μ l, and injection liquid chromatography, records chromatogram; And measure peak area or peak height;
(4) separately get perindopril tert-butylamine salt reference substance appropriate, accurately weighed, add mobile phase and dissolve and dilute and make in every 1ml the approximately solution containing 0.4mg, precision measures 20 μ l, and injection liquid chromatography, records chromatogram; And measure peak area or peak height;
(5) according in step (3) and (4) the data of surveying calculate the content of perindopril tert-butylamine salt according to external standard method.
Embodiment 3
An assay method for perindopril tert-butylamine salt content, comprises the following steps:
(1) system suitability: the number of theoretical plate to chromatographic column, degree of separation, repeatability, tailing factor are tested respectively;
(2) selection of filling agent and mobile phase: employing octadecylsilane chemically bonded silica is filling agent, take methyl alcohol-phosphate buffer (55:45) as mobile phase, wherein phosphate buffer is by 2.5g potassium dihydrogen phosphate, 4ml phosphoric acid, 4ml triethylamine is dissolved in water and is diluted to 1000ml, and detection wavelength is 213nm; 41 ℃ of column temperatures;
(3) get perindopril tert-butylamine salt sample appropriate, accurately weighed, add the mutual-assistance of flowing and dissolves and dilute and shake up, make the solution that approximately contains 0.4mg in every 1ml, precision measures 20 μ l, and injection liquid chromatography, records chromatogram; And measure peak area or peak height;
(4) separately get perindopril tert-butylamine salt reference substance appropriate, accurately weighed, add mobile phase and dissolve and dilute and make in every 1ml the approximately solution containing 0.4mg, precision measures 20 μ l, and injection liquid chromatography, records chromatogram; And measure peak area or peak height;
(5) according in step (3) and (4) the data of surveying calculate the content of perindopril tert-butylamine salt according to external standard method.
Claims (2)
1. an assay method for perindopril tert-butylamine salt content, is characterized in that: comprise the following steps:
(1) system suitability: the number of theoretical plate to chromatographic column, degree of separation, repeatability, tailing factor are tested respectively;
(2) selection of filling agent and mobile phase: employing octadecylsilane chemically bonded silica is filling agent, take methyl alcohol-phosphate buffer (55:45) as mobile phase, detection wavelength is 210-215nm; Column temperature 40-42 ℃;
(3) get perindopril tert-butylamine salt sample appropriate, accurately weighed, add the mutual-assistance of flowing and dissolves and dilute and shake up, make the solution that approximately contains 0.4mg in every 1ml, precision measures 20 μ l, and injection liquid chromatography, records chromatogram; And measure peak area or peak height;
(4) separately get perindopril tert-butylamine salt reference substance appropriate, accurately weighed, add mobile phase and dissolve and dilute and make in every 1ml the approximately solution containing 0.4mg, precision measures 20 μ l, and injection liquid chromatography, records chromatogram; And measure peak area or peak height;
(5) according in step (3) and (4) the data of surveying calculate the content of perindopril tert-butylamine salt according to external standard method.
2. the assay method of a kind of perindopril tert-butylamine salt content according to claim 1, is characterized in that: described in step (2), phosphate buffer is by 2-3g potassium dihydrogen phosphate, 3-5ml phosphoric acid, and 3-5ml triethylamine is dissolved in water and is diluted to 1000ml.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410104469.XA CN103822996A (en) | 2014-03-20 | 2014-03-20 | Measuring method of content of perindopril tert-butylamine salt |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410104469.XA CN103822996A (en) | 2014-03-20 | 2014-03-20 | Measuring method of content of perindopril tert-butylamine salt |
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| CN103822996A true CN103822996A (en) | 2014-05-28 |
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| CN201410104469.XA Pending CN103822996A (en) | 2014-03-20 | 2014-03-20 | Measuring method of content of perindopril tert-butylamine salt |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2001087835A1 (en) * | 2000-07-06 | 2001-11-22 | Les Laboratoires Servier | Α crystalline form of perindopril tert-butylamine salt |
| WO2008050185A2 (en) * | 2006-10-26 | 2008-05-02 | Glenmark Pharmaceuticals Limited | Novel polymorphs of perindopril erbumine |
| CN101228179A (en) * | 2005-08-12 | 2008-07-23 | 力奇制药公司 | A process for the preparation of perindopril erbumine |
| CN101332191A (en) * | 2008-07-10 | 2008-12-31 | 沈阳药科大学 | Stable perindopril tert-butylamine salt tablets and preparation method thereof |
| CN101766598A (en) * | 2008-12-31 | 2010-07-07 | 东英（江苏）药业有限公司 | Drug combination containing perindopril |
-
2014
- 2014-03-20 CN CN201410104469.XA patent/CN103822996A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2001087835A1 (en) * | 2000-07-06 | 2001-11-22 | Les Laboratoires Servier | Α crystalline form of perindopril tert-butylamine salt |
| CN101228179A (en) * | 2005-08-12 | 2008-07-23 | 力奇制药公司 | A process for the preparation of perindopril erbumine |
| WO2008050185A2 (en) * | 2006-10-26 | 2008-05-02 | Glenmark Pharmaceuticals Limited | Novel polymorphs of perindopril erbumine |
| CN101332191A (en) * | 2008-07-10 | 2008-12-31 | 沈阳药科大学 | Stable perindopril tert-butylamine salt tablets and preparation method thereof |
| CN101766598A (en) * | 2008-12-31 | 2010-07-07 | 东英（江苏）药业有限公司 | Drug combination containing perindopril |
Non-Patent Citations (2)
| Title |
|---|
| M. MEDENICA ETAL: "Evaluation of impurities level of perindopril tert-butylamine in tablets", 《JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS》 * |
| 张永强 等: "辅料对培哚普利叔丁胺盐稳定性影响的考察", 《中国药剂学杂志》 * |
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Application publication date: 20140528 |