CN106153804A - A kind of detection method of Li Gelieting raw material - Google Patents
A kind of detection method of Li Gelieting raw material Download PDFInfo
- Publication number
- CN106153804A CN106153804A CN201610612507.1A CN201610612507A CN106153804A CN 106153804 A CN106153804 A CN 106153804A CN 201610612507 A CN201610612507 A CN 201610612507A CN 106153804 A CN106153804 A CN 106153804A
- Authority
- CN
- China
- Prior art keywords
- solution
- gelieting
- detection method
- high performance
- performance liquid
- 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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
-
- 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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
- G01N2030/884—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample organic compounds
Abstract
A kind of detection method of Li Gelieting raw material.The method uses high performance liquid chromatography to carry out, and comprises the steps: that (1) prepares Li Gelieting sample solution；(2) step (1) gained solution is injected high performance liquid chromatograph, and record chromatogram；Wherein, the chromatographic column fixed phase filler octadecylsilane chemically bonded silica of described high performance liquid chromatography is filler；The preparation of flowing phase: mobile phase A is pH2.5 phosphate buffer；Mobile phase B is methanol acetonitrile 1: 1.The detection method of the present invention measures the related substance that has in Li Gelieting raw material under same liquid-phase condition, and described detection method is easy and simple to handle, separating degree is high, assay method specificity is strong, testing result is the most credible.
Description
Technical field
The present invention relates to drug measurement techniques field, be specifically related to the detection method of a kind of Li Gelieting raw material.
Background technology
Li Gelieting (Linagliptin Tablets), Li Gelieting are a kind of dipeptidyl peptidase-4 (DPP-4) suppression
Agent, can improve the different blood glucose levels of type 2 diabetes mellitus (T2DM) adult patients on the basis of diet control and physical training.?
Preparation process can be used a lot of raw material, but the detection method operation currently to raw material is responsible for, separating degree is low, testing result is accurate
Really property is low.
Summary of the invention
The technical problem to be solved in the present invention is the defect overcoming prior art, it is provided that a kind of Li Gelieting raw material
Detection method.
In order to solve above-mentioned technical problem, the invention provides following technical scheme: a kind of Li Gelieting raw material
Detection method, its scheme is as follows:
1) preparation Li Gelieting sample solution, described Li Gelieting sample solution include system suitability solution, need testing solution,
Reference substance solution；
(2) step (1) gained sample solution is injected high performance liquid chromatograph, carry out eluting mutually with flowing, and record chromatogram；
Wherein, it is appropriate that the preparation method of described need testing solution comprises the steps: to take this product, dissolves with acetonitrile-water 70: 30 and quantitative
Every 1ml solution containing about 2mg is made in dilution, as need testing solution, separately takes Li Gelieting reference substance appropriate, with acetonitrile-water 70:
30 dissolve and quantitatively dilute the solution making every 1ml containing 2 μ g, as reference substance solution, test according to high performance liquid chromatography, with ten
Eight alkyl silane bonded silica gels are filler, with pH2.5 phosphate buffer as mobile phase A；Methanol-acetonitrile 1: 1 is flowing phase
B, carries out gradient elution according to following table, and flow velocity is 1.0ml per minute, and detection wavelength is 218nm, and column temperature 55 DEG C takes Li Gelieting miscellaneous
Matter M, impurity X, impurity Z, the most about 2mg, put in 10ml measuring bottle, adds acetonitrile-water 70: 30 and dissolves and be diluted to scale, and precision measures
1ml, adds in the 5ml measuring bottle being placed with Li Gelieting system suitability reference substance 10mg in advance, with acetonitrile-water 70: 30
Being diluted to scale, take 2 μ l and inject chromatograph of liquid, record chromatogram, the chromatographic column fixed phase of described high performance liquid chromatography is filled out
Filling agent octadecylsilane chemically bonded silica is filler.
Preferably, the preparation of described flowing phase: mobile phase A is pH2.5 phosphate buffer；Mobile phase B is methanol-acetonitrile
1∶1。
Preferably, described phosphate buffered solution takes potassium dihydrogen phosphate 3.0g, is dissolved in 1000ml water, uses phosphorus acid for adjusting pH
To 2.5.
Preferably, the chromatographic column of described high performance liquid chromatography, column temperature is 55 DEG C, and detection wavelength is 218nm.
Preferably, in high performance liquid chromatography detecting step (2), take reference substance solution 2 μ l and inject chromatograph of liquid, adjust
Joint detection sensitivity, makes the peak height of main constituent chromatographic peak be about the 20% of full scale；It is molten with reference substance that precision measures need testing solution
The each 2 μ l of liquid, are injected separately into chromatograph of liquid, record chromatogram；Preferably, the amount of sample solution in chromatograph of liquid of injecting is
2μl。
The detection method of the present invention measures the related substance that has in Li Gelieting raw material, described detection under same liquid-phase condition
Method is easy and simple to handle, separating degree is high, assay method specificity is strong, testing result is the most credible.
Embodiment
Embodiment 1
The method uses high performance liquid chromatography to carry out, and comprises the steps:
(1) preparation Li Gelieting sample solution, described Li Gelieting sample solution includes that system suitability solution, test sample are molten
Liquid, reference substance solution
(2) step (1) gained sample solution is injected high performance liquid chromatograph, carry out eluting mutually with flowing, and record chromatogram；
Wherein, it is appropriate that the preparation method of described need testing solution comprises the steps: to take this product, dissolves with acetonitrile-water 70: 30 and quantitative
Dilution makes every 1ml solution containing about 2mg, as need testing solution.Separately take Li Gelieting reference substance appropriate, with acetonitrile-water 70:
30 dissolve and quantitatively dilute the solution making every 1ml containing 2 μ g, as reference substance solution.According to high performance liquid chromatography (Chinese Pharmacopoeia
Two annex of version in 2010D) test.It is filler with octadecylsilane chemically bonded silica, particle diameter 5 μm, 15cm × 4.6mm,
Intertsil ODS-2, with pH2.5 phosphate buffer as mobile phase A, phosphate buffer potassium dihydrogen phosphate 3.0g, molten
In 1000ml water, with phosphorus acid for adjusting pH to 2.5；Methanol-acetonitrile 1: 1 is Mobile phase B, carries out gradient elution, flow velocity according to following table
For 1.0ml per minute, detection wavelength is 218nm, column temperature 55 DEG C.Take Li Gelieting impurity M, impurity X, impurity Z, the most about 2mg, put
In 10ml measuring bottle, adding acetonitrile-water 70: 30 and dissolve and be diluted to scale, precision measures 1ml, adds and is placed with Li Gelieting system in advance
System employment and suitability test (E & ST), with in the 5ml measuring bottle of reference substance 10mg, is diluted to scale with acetonitrile-water 70: 30, takes 2 μ l and injects liquid phase color
Spectrometer, records chromatogram.The chromatographic column fixed phase filler octadecylsilane chemically bonded silica of described high performance liquid chromatography
For filler, particle diameter 5 μm, 15cm × 4.6mm, Intertsil ODS-2 is the most applicable.
Claims (5)
1. the detection method of Yi Zhong Li Gelieting raw material, it is characterised in that step is as follows:
1) preparation Li Gelieting sample solution, described Li Gelieting sample solution include system suitability solution, need testing solution,
Reference substance solution；
(2) step (1) gained sample solution is injected high performance liquid chromatograph, carry out eluting mutually with flowing, and record chromatogram；
Wherein, it is appropriate that the preparation method of described need testing solution comprises the steps: to take this product, dissolves with acetonitrile-water 70: 30 and quantitative
Every 1ml solution containing about 2mg is made in dilution, as need testing solution, separately takes Li Gelieting reference substance appropriate, with acetonitrile-water 70:
30 dissolve and quantitatively dilute the solution making every 1ml containing 2 μ g, as reference substance solution, test according to high performance liquid chromatography, with ten
Eight alkyl silane bonded silica gels are filler, with pH2.5 phosphate buffer as mobile phase A；Methanol-acetonitrile 1: 1 is flowing phase
B, carries out gradient elution according to following table, and flow velocity is 1.0ml per minute, and detection wavelength is 218nm, and column temperature 55 DEG C takes Li Gelieting miscellaneous
Matter M, impurity X, impurity Z, the most about 2mg, put in 10ml measuring bottle, adds acetonitrile-water 70: 30 and dissolves and be diluted to scale, and precision measures
1ml, adds in the 5ml measuring bottle being placed with Li Gelieting system suitability reference substance 10mg in advance, with acetonitrile-water 70: 30
Being diluted to scale, take 2 μ l and inject chromatograph of liquid, record chromatogram, the chromatographic column fixed phase of described high performance liquid chromatography is filled out
Filling agent octadecylsilane chemically bonded silica is filler.
2. according to the detection method described in claim 1, it is characterised in that the preparation of described flowing phase: mobile phase A is pH2.5
Phosphate buffer；Mobile phase B is methanol-acetonitrile 1: 1.
Detection method the most according to claim 1, it is characterised in that described phosphate buffered solution takes potassium dihydrogen phosphate
3.0g, is dissolved in 1000ml water, with phosphorus acid for adjusting pH to 2.5.
Detection method the most according to claim 1, it is characterised in that the chromatographic column of described high performance liquid chromatography, column temperature
Being 55 DEG C, detection wavelength is 218nm.
Detection method the most according to claim 1, it is characterised in that in high performance liquid chromatography detecting step (2), take
Reference substance solution 2 μ l injects chromatograph of liquid, regulates detection sensitivity, makes the peak height of main constituent chromatographic peak be about full scale
20%；Precision measures need testing solution and each 2 μ l of reference substance solution, is injected separately into chromatograph of liquid, records chromatogram；Preferably,
The amount of sample solution in chromatograph of liquid of injecting is 2 μ l.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610612507.1A CN106153804A (en) | 2016-07-31 | 2016-07-31 | A kind of detection method of Li Gelieting raw material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610612507.1A CN106153804A (en) | 2016-07-31 | 2016-07-31 | A kind of detection method of Li Gelieting raw material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106153804A true CN106153804A (en) | 2016-11-23 |
Family
ID=57327636
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610612507.1A Pending CN106153804A (en) | 2016-07-31 | 2016-07-31 | A kind of detection method of Li Gelieting raw material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106153804A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108132313A (en) * | 2018-01-18 | 2018-06-08 | 上海药明康德新药开发有限公司 | The high-efficiency liquid chromatography method for detecting of BI 1356 |
| CN110240599A (en) * | 2018-03-07 | 2019-09-17 | 齐鲁制药有限公司 | A kind of Li Gelieting impurity and its preparation method and application |
| CN114527200A (en) * | 2020-11-23 | 2022-05-24 | 成都倍特药业股份有限公司 | Method for detecting related substances of linagliptin |
-
2016
- 2016-07-31 CN CN201610612507.1A patent/CN106153804A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108132313A (en) * | 2018-01-18 | 2018-06-08 | 上海药明康德新药开发有限公司 | The high-efficiency liquid chromatography method for detecting of BI 1356 |
| CN110240599A (en) * | 2018-03-07 | 2019-09-17 | 齐鲁制药有限公司 | A kind of Li Gelieting impurity and its preparation method and application |
| CN114527200A (en) * | 2020-11-23 | 2022-05-24 | 成都倍特药业股份有限公司 | Method for detecting related substances of linagliptin |
| CN114527200B (en) * | 2020-11-23 | 2023-08-11 | 成都倍特药业股份有限公司 | Detection method of linagliptin related substances |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104237421B (en) | A kind of relevant substance detecting method of succinum love song Ge Lieting and preparation thereof | |
| CN106153804A (en) | A kind of detection method of Li Gelieting raw material | |
| CN105301159B (en) | High performance liquid chromatography analysis method of sirolimus | |
| CN106918676B (en) | Method for separating and measuring contents of two drugs in tazarotene betamethasone cream and related substances | |
| CN107238672A (en) | The content assaying method of impurity in a kind of isoniazid or its pharmaceutical composition | |
| CN106950290A (en) | About the detection method of material in Clindamycin Phosphate Gel | |
| CN109387587B (en) | Detection method of L-2-amino-5-guanidino valeric acid enantiomer | |
| CN111024831B (en) | Method for separating moxifloxacin hydrochloride and impurities thereof by high performance liquid chromatography | |
| CN108593818B (en) | High performance liquid chromatography method for measuring related substances of nicergoline | |
| CN103353492A (en) | Method of separating and measuring solifenacin succinate raw material and preparation thereof by using liquid chromatography | |
| CN106706769B (en) | Separation and determination method of empagliflozin and optical isomer thereof | |
| CN102384946B (en) | By the method for high efficiency liquid chromatography for separating and determining Entecavir and diastereo-isomerism thereof | |
| CN104764840B (en) | The separation of palonosetron Hcl and impurity and detection method | |
| CN107328874B (en) | Resolution reagent and separation detection method for palonosetron hydrochloride optical isomer | |
| CN110095538A (en) | A kind of detection method of the Anisodamine in relation to substance | |
| CN110412164B (en) | Method for detecting related substances of mexiletine hydrochloride | |
| CN104897832A (en) | High performance liquid chromatography method for detecting free amino acid content in transfer factor solution and preparation thereof | |
| CN110824074A (en) | Method for detecting related substances of ticagrelor by using high performance liquid chromatography | |
| CN101929988A (en) | Method for detecting febuxostat-associated matters by using high performance liquid chromatography | |
| CN106290621A (en) | A kind of detection method of Li Gelieting isomer | |
| CN103837626B (en) | The content assaying method of trifluoroacetic acid in a kind of bivalirudin | |
| CN108169379A (en) | A kind of high efficient liquid phase analysis method of times Ta Siding and its preparation | |
| CN111351866A (en) | Method for detecting hyodeoxycholic acid in Xihuang capsules | |
| CN116678982B (en) | Detection method of paliperidone palmitate impurity SM1-G | |
| CN116297889A (en) | Detection method of related substances of amoxicillin bulk drug |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20161123 |
|
| WD01 | Invention patent application deemed withdrawn after publication |