CN106370742A - Detection method of purity of trelagliptin succinate - Google Patents
Detection method of purity of trelagliptin succinate Download PDFInfo
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- CN106370742A CN106370742A CN201610708642.6A CN201610708642A CN106370742A CN 106370742 A CN106370742 A CN 106370742A CN 201610708642 A CN201610708642 A CN 201610708642A CN 106370742 A CN106370742 A CN 106370742A
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- mobile phase
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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
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- Life Sciences & Earth Sciences (AREA)
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Abstract
The invention discloses a detection method of purity of trelagliptin succinate. The method includes the steps of: 1) dissolving trelagliptin succinate in a methanol solution and diluting the trelagliptin succinate solution into 0.1 mg/ml to form a sample solution; 2) employing octadecyl bonded silica as filler; 3) setting the parameters of a liquid chromatographic instrument as follows: flow rate is 0.8-1.2 ml/min, detection wavelength is 276 nm, a mobile phase A is methanol-acetonitrile being 1:4 in ratio, and a mobile phase B is a 0.1% triethylamine solution; 4) metering 15-25 [mu]l of the sample solution and injecting the sample solution into the liquid chromatographic instrument, and if there are impurity peaks in the chromatogram map of the sample solution, performing calculation according to area normalization method, wherein individual impurity should be not more than 1.0% and total impurity should be not more than 0.2%. The detection method is improved in detection precision and has a totally excellent use effect.
Description
Technical field
The present invention relates to a kind of detection method of succinum love song Ge Lieting purity, it is mainly used in the technology neck of medicine detection
Domain.
Background technology
Trelagliptin (bent Ge Lieting) is a kind of weekly dipeptidyl peptidase iv (dpp-4) inhibitor, passes through
Selectivity, persistence suppression dpp-4, control blood sugar level.Dpp-4 is a kind of enzyme, can cause incretin (pancreas hyperglycemia
Plain sample peptide -1 (glp-1) and glucose-dependent-insulinotropic polypeptide (gip)) inactivation, and this 2 kinds of intestinal fall insulin is in blood glucose
Play an important role in regulation.Suppression dpp-4, by increasing capacitance it is possible to increase blood sugar level dependency insulin secretion, thus control blood glucose
Level.For this medicine, the purity of its main component is the deciding factor of medicine drug effect, is therefore preparing this medicine
Subsequent detection is highly important.
Content of the invention
The technical problem to be solved in the present invention is to provide a kind of detection method of succinum love song Ge Lieting purity.
The present invention is achieved through the following technical solutions.
A kind of detection method of succinum love song Ge Lieting purity, step includes:
(1) take succinum love song Ge Lieting, plus methanol solution dissolves and dilutes the solution making 0.1mg/ml, as test sample
Solution；
(2) octadecyl silane is used as filler；
(3) parameter of chromatograph of liquid is set to: flow velocity is 0.8-1.2ml/min, and Detection wavelength is 276nm, mobile phase a
For methanol-acetonitrile=1:4, mobile phase b is 0.1% triethylamine solution；
(4) measure need testing solution 15-25 μ l, inject chromatograph of liquid, if any impurity in the chromatogram of need testing solution
Peak, is calculated by area normalization method, and single miscellaneous no more than 1.0%, always miscellaneous no more than 0.2%.
Further, the methanol solution that (1) methanol solution is 50% for concentration.
Further, the gradient mode of (3) mobile phase a and mobile phase b is:
During 0min mobile phase a be 10%, mobile phase b be 90%；
During 20min mobile phase a be 30%, mobile phase b be 70%；
During 50min mobile phase a be 50%, mobile phase b be 50%；
Hereafter concentration keeps constant.
Further, (4) triethylamine solution uses acetic acid to adjust ph2.9.
Beneficial effects of the present invention:
This detection method deft design, operation is relatively easy to, and the gradient mode of mobile phase a and mobile phase b is reasonable in design, energy
Improve the precision of detection, generally speaking using effect is preferable.
Specific embodiment
Below according to embodiment, the present invention is described in further detail.
The detection method of succinum love song Ge Lieting purity, takes succinum love song Ge Lieting appropriate, plus 50% methanol solution is ultrasonic
Dissolve and dilute and make the solution containing about 0.1mg in every 1ml, as need testing solution.With octadecyl silane (250 ×
4.6mm) it is filler；Flow velocity is 1.0ml/min；Detection wavelength is 276nm, and mobile phase a is methanol-acetonitrile=1:4, mobile phase
B is 0.1% triethylamine solution (ph2.9 adjusted by acetic acid), and gradient mode is as follows:
| Time | A% | B% |
| 0 | 10 | 90 |
| 20 | 30 | 70 |
| 50 | 50 | 50 |
| 120 | 50 | 50 |
Precision measures need testing solution 20 μ l, injects chromatograph of liquid.If any impurity peaks in the chromatogram of need testing solution,
Calculate by area normalization method, single miscellaneous no more than 1.0%, always miscellaneous no more than 0.2%.
The present invention, the detection method of succinum love song Ge Lieting purity, this detection method deft design, operation is relatively easy to,
The gradient mode of mobile phase a and mobile phase b is reasonable in design, can improve the precision of detection, generally speaking using effect is preferable.
Above-described embodiment only technology design to illustrate the invention and feature, its object is to allow and is familiar with this art
Personage will appreciate that present invention and is carried out, and can not be limited the scope of the invention with this.All according to the present invention
Equivalence changes or modification that spirit is made, all should cover within the scope of the present invention.
Claims (4)
1. a kind of detection method of succinum love song Ge Lieting purity is it is characterised in that step includes:
(1) take succinum love song Ge Lieting, plus methanol solution dissolves and dilute the solution making 0.1mg/ml, molten as test sample
Liquid；
(2) octadecyl silane is used as filler；
(3) parameter of chromatograph of liquid is set to: flow velocity is 0.8-1.2ml/min, and Detection wavelength is 276nm, and mobile phase a is first
Alcohol-acetonitrile=1:4, mobile phase b is 0.1% triethylamine solution；
(4) measure need testing solution 15-25 μ l, inject chromatograph of liquid, if any impurity peaks in the chromatogram of need testing solution, press
Area normalization method calculates, and single miscellaneous no more than 1.0%, always miscellaneous no more than 0.2%.
2. the detection method of succinum love song Ge Lieting purity according to claim 1 is it is characterised in that (1) methanol solution
The methanol solution being 50% for concentration.
3. succinum love song Ge Lieting purity according to claim 1 detection method it is characterised in that (3) mobile phase a and
The gradient mode of mobile phase b is:
During 0min mobile phase a be 10%, mobile phase b be 90%；
During 20min mobile phase a be 30%, mobile phase b be 70%；
During 50min mobile phase a be 50%, mobile phase b be 50%；
Hereafter concentration keeps constant.
4. the detection method of succinum love song Ge Lieting purity according to claim 1 is it is characterised in that (4) triethylamine is molten
Liquid uses acetic acid to adjust ph2.9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610708642.6A CN106370742A (en) | 2016-08-23 | 2016-08-23 | Detection method of purity of trelagliptin succinate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610708642.6A CN106370742A (en) | 2016-08-23 | 2016-08-23 | Detection method of purity of trelagliptin succinate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106370742A true CN106370742A (en) | 2017-02-01 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610708642.6A Pending CN106370742A (en) | 2016-08-23 | 2016-08-23 | Detection method of purity of trelagliptin succinate |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104237421A (en) * | 2014-10-15 | 2014-12-24 | 济南春和景明医药技术有限公司 | Related substance detection method for trelagliptin succinate and preparation thereof |
| CN105699547A (en) * | 2016-04-22 | 2016-06-22 | 中山万汉医药科技有限公司 | Method for measuring related substances in succinic acid Trelagliptin raw materials |
| CN105738517A (en) * | 2016-02-24 | 2016-07-06 | 中山万汉医药科技有限公司 | Method for determining related substances in Trelagliptin tablets |
-
2016
- 2016-08-23 CN CN201610708642.6A patent/CN106370742A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104237421A (en) * | 2014-10-15 | 2014-12-24 | 济南春和景明医药技术有限公司 | Related substance detection method for trelagliptin succinate and preparation thereof |
| CN105738517A (en) * | 2016-02-24 | 2016-07-06 | 中山万汉医药科技有限公司 | Method for determining related substances in Trelagliptin tablets |
| CN105699547A (en) * | 2016-04-22 | 2016-06-22 | 中山万汉医药科技有限公司 | Method for measuring related substances in succinic acid Trelagliptin raw materials |
Non-Patent Citations (3)
| Title |
|---|
| HUI ZHANG 等: "Identification, characterization and HPLC quantification of process-related impurities in Trelagliptin succinate bulk drug: Six identified as new compounds", 《JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS》 * |
| QI WANG等: "Determination of the Enantiomeric Purity of Trelagliptin by Pre‑Column Derivatization and Liquid Chromatography on a Chiral Stationary Phase", 《CHROMATOGRAPHIA》 * |
| 李广禄: "高效液相色谱法测定琥珀酸曲格列汀片的含量", 《海峡药学》 * |
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Application publication date: 20170201 |