CN106248829A - A kind of detection method of succinum love song Ge Lieting chiral purity - Google Patents
A kind of detection method of succinum love song Ge Lieting chiral purity Download PDFInfo
- Publication number
- CN106248829A CN106248829A CN201610708617.8A CN201610708617A CN106248829A CN 106248829 A CN106248829 A CN 106248829A CN 201610708617 A CN201610708617 A CN 201610708617A CN 106248829 A CN106248829 A CN 106248829A
- Authority
- CN
- China
- Prior art keywords
- lieting
- detection method
- love song
- need testing
- succinum love
- 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.)
- Pending
Links
Classifications
-
- 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
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analysing Biological Materials (AREA)
Abstract
The invention discloses the detection method of a kind of succinum love song Ge Lieting chiral purity, step includes: (1) takes succinum love song Ge Lieting, adds flowing phased soln and dilution makes the solution of every 0.8 1.2mg/mL, as need testing solution；(2) using normal hexane: dehydrated alcohol (4:6) adds 0.1% diethylamine as flowing phase；(3) parameter of chromatograph of liquid is set to flow velocity is 0.5ml/min, and detection wavelength is 276nm；(4) need testing solution injects chromatograph of liquid, records chromatogram, such as chiral isomer peak in the chromatogram of need testing solution, calculates by area normalization method, cannot be greater than 0.5%.Ee value is not less than 99.0%.It is an advantage of the current invention that this detection method deft design, operation is relatively easy to, and flowing mutually and fixing arranges relatively reasonable mutually, can improve the precision detected, and generally speaking using effect is preferable.
Description
Technical field
The present invention relates to the detection method of a kind of succinum love song Ge Lieting chiral purity, belong to the technology neck of medicine detection
Territory.
Background technology
Trelagliptin (bent Ge Lieting) is a kind of weekly DPP IV (DPP-4) inhibitor, passes through
Selectivity, persistence suppression DPP-4, controls blood sugar level.DPP-4 is a kind of enzyme, it is possible to cause incretin (pancreas hyperglycemia
Element sample peptide-1 (GLP-1) and glucose-dependent-insulinotropic polypeptide (GIP)) inactivation, and these 2 kinds of intestinal drop insulins at blood glucose
Regulation plays an important role.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..
Summary of the invention
The technical problem to be solved in the present invention is to provide the detection method of a kind of succinum love song Ge Lieting chiral purity.
The present invention is achieved through the following technical solutions.
A kind of detection method of succinum love song Ge Lieting chiral purity, step includes:
(1) take succinum love song Ge Lieting, add flowing phased soln and dilution makes the solution of every 0.8-1.2mg/mL, as confession
Test sample solution；
(2) using normal hexane: dehydrated alcohol (4:6) adds 0.1% diethylamine as flowing phase；
(3) parameter of chromatograph of liquid is set to flow velocity is 0.5ml/min, and detection wavelength is 276nm；
(4) need testing solution injects chromatograph of liquid, records chromatogram, such as chiral photo-isomerisation in the chromatogram of need testing solution
Body peak, is calculated by area normalization method, cannot be greater than 0.5%.Ee value is not less than 99.0%.
Further, use AD-H type chiral column as fixing phase.
Beneficial effects of the present invention:
This detection method deft design, operation is relatively easy to, and flowing mutually and fixing arranges relatively reasonable mutually, can improve inspection
The precision surveyed, generally speaking using effect is preferable.
Detailed description of the invention
Below according to embodiment, the present invention is described in further detail.
The detection method of a kind of succinum love song Ge Lieting chiral purity, takes succinum love song Ge Lieting appropriate, adds flowing and mix
Solve and dilute the solution made in every 1ml containing about 0.1mg, as need testing solution.It is 276nm at detection wavelength, uses AD-H type
Chiral column (250 × 4.6mm) is fixing phase；With normal hexane: dehydrated alcohol (4:6) add 0.1% diethylamine for flowing phase, flow velocity is
0.5ml/min；Precision measures need testing solution 5 μ l, injects chromatograph of liquid, records chromatogram.The chromatogram of need testing solution
In such as chiral isomer peak, calculate by area normalization method, cannot be greater than 0.5%.Ee value is not less than 99.0%.
The present invention, the detection method of a kind of succinum love song Ge Lieting chiral purity, deft design, operation is relatively easy to, stream
Dynamic mutually and fixing arrange relatively reasonable mutually can improve the precision detected, generally speaking using effect is preferable.
Above-described embodiment only for technology design and the feature of the present invention are described, its object is to allow and is familiar with this art
Personage will appreciate that present invention and is carried out, and can not limit the scope of the invention with this.All according to the present invention
The equivalence that spirit is made changes or modifies, and all should contain within the scope of the present invention.
Claims (2)
1. the detection method of a succinum love song Ge Lieting chiral purity, it is characterised in that step includes:
(1) take succinum love song Ge Lieting, add flowing phased soln and dilution makes the solution of every 0.8-1.2mg/mL, as test sample
Solution；
(2) using normal hexane: dehydrated alcohol (4:6) adds 0.1% diethylamine as flowing phase；
(3) parameter of chromatograph of liquid is set to flow velocity is 0.5ml/min, and detection wavelength is 276nm；
(4) need testing solution injects chromatograph of liquid, records chromatogram, such as chiral isomer in the chromatogram of need testing solution
Peak, is calculated by area normalization method, cannot be greater than 0.5%.Ee value is not less than 99.0%.
The detection method of succinum love song Ge Lieting chiral purity the most according to claim 1, it is characterised in that use AD-H
Type chiral column is as fixing phase.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610708617.8A CN106248829A (en) | 2016-08-23 | 2016-08-23 | A kind of detection method of succinum love song Ge Lieting chiral purity |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610708617.8A CN106248829A (en) | 2016-08-23 | 2016-08-23 | A kind of detection method of succinum love song Ge Lieting chiral purity |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106248829A true CN106248829A (en) | 2016-12-21 |
Family
ID=57595860
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610708617.8A Pending CN106248829A (en) | 2016-08-23 | 2016-08-23 | A kind of detection method of succinum love song Ge Lieting chiral purity |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106248829A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106770855A (en) * | 2016-12-30 | 2017-05-31 | 江苏开元医药化工有限公司 | A kind of method for separating and detecting of Sha Kubi song intermediates and its optical isomer based on high performance liquid chromatography |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105675733A (en) * | 2014-11-17 | 2016-06-15 | 重庆医药工业研究院有限责任公司 | Method for using liquid chromatography method for separation and determination of trelagliptin succinate and trelagliptin succinate optical isomers |
-
2016
- 2016-08-23 CN CN201610708617.8A patent/CN106248829A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105675733A (en) * | 2014-11-17 | 2016-06-15 | 重庆医药工业研究院有限责任公司 | Method for using liquid chromatography method for separation and determination of trelagliptin succinate and trelagliptin succinate optical isomers |
Non-Patent Citations (4)
| Title |
|---|
| PRADIP JADAV 等: "Design, synthesis and biological evaluation of novel aminomethyl-piperidones based DPP-IV inhibitors", 《BIOORGANIC & MEDICINAL CHEMISTRY LETTERS》 * |
| 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》 * |
| 邓思思 等: "RP-HPLC法测定琥珀酸曲格列汀的油光物质及酸降解杂质的LC-MS/MS分析", 《中国新药杂志》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106770855A (en) * | 2016-12-30 | 2017-05-31 | 江苏开元医药化工有限公司 | A kind of method for separating and detecting of Sha Kubi song intermediates and its optical isomer based on high performance liquid chromatography |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104237421B (en) | A kind of relevant substance detecting method of succinum love song Ge Lieting and preparation thereof | |
| Hu et al. | Platelets express activated P2Y12 receptor in patients with diabetes mellitus | |
| Hirata et al. | Mechanisms of adrenomedullin-induced vasodilation in the rat kidney | |
| Ganz et al. | The hepcidin-ferroportin system as a therapeutic target in anemias and iron overload disorders | |
| Lee et al. | Euthyroid sick syndrome | |
| Hamel et al. | G-protein–coupled receptor 91 and succinate are key contributors in neonatal postcerebral hypoxia-ischemia recovery | |
| Iyer et al. | Vasodepressor actions of angiotensin-(1–7) unmasked during combined treatment with lisinopril and losartan | |
| Ishikura et al. | Effects of sildenafil citrate (Viagra) combined with nitrate on the heart | |
| Jin et al. | Mitochondrial dynamics and hypothalamic regulation of metabolism | |
| Wu et al. | GLP-1, exendin-4 and C-peptide regulate pancreatic islet microcirculation, insulin secretion and glucose tolerance in rats | |
| CN102138892B (en) | Choline alfoscerate injection preparation as well as preparation method and detection method thereof | |
| Guo et al. | Characterization of interaction property of multicomponents in Chinese Herb with protein by microdialysis combined with HPLC | |
| Zhang et al. | Effects of Angiotensin‐(1‐7) and Angiotensin II on Acetylcholine‐Induced Vascular Relaxation in Spontaneously Hypertensive Rats | |
| CN106248829A (en) | A kind of detection method of succinum love song Ge Lieting chiral purity | |
| Gevaert et al. | Blood-brain barrier transport kinetics of the neuromedin peptides NMU, NMN, NMB and NT | |
| Fudim et al. | Ultrafiltration in acute heart failure: implications of ejection fraction and early response to treatment from CARRESS‐HF | |
| Guo et al. | Effects of testosterone on erythropoiesis in a female mouse model of anemia of inflammation | |
| Tian et al. | Novel 14S, 21‐dihydroxy‐docosahexaenoic acid rescues wound healing and associated angiogenesis impaired by acute ethanol intoxication/exposure | |
| CN105929084B (en) | The method that high performance liquid chromatography splits alogliptin benzoate and its enantiomter | |
| Miseta et al. | Hepcidin and its potential clinical utility | |
| CN104764815A (en) | Method for detecting aldehyde and higher alcohol compounds in brandy | |
| CN106074422A (en) | A kind of succinum love song Ge Lieting oral solid formulation and preparation method thereof | |
| CN103760286A (en) | Method for measuring optical purity of solifenacin succinate intermediate by high-performance liquid chromatography | |
| Rademaker et al. | Haemodynamic, endocrine and renal actions of adrenomedullin 5 in an ovine model of heart failure | |
| CN105461604B (en) | A kind of preparation method of high purity allicin |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20161221 |