CN107677751A - A kind of method of high performance liquid chromatography detection Amlodipine Besylate Tablet and its impurity - Google Patents
A kind of method of high performance liquid chromatography detection Amlodipine Besylate Tablet and its impurity Download PDFInfo
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- CN107677751A CN107677751A CN201711069238.XA CN201711069238A CN107677751A CN 107677751 A CN107677751 A CN 107677751A CN 201711069238 A CN201711069238 A CN 201711069238A CN 107677751 A CN107677751 A CN 107677751A
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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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- 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
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/065—Preparation using different phases to separate parts of sample
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Abstract
The invention belongs to Pharmaceutical Analysis technical field, is related to a kind of method of high performance liquid chromatography detection Amlodipine Besylate Tablet and its impurity.The method for separating and detecting of the present invention uses high performance liquid chromatograph, and chromatographic column is C18 posts, and specification is 4.6 × 250mm, 5 μm；Mobile phase A methanol：Acetonitrile：Triethylamine solution=35:（20~25）:（40~45）(v:v:V) with Mobile phase B methanol, gradient elution is carried out.Amlodipine Besylate Tablet and its side reaction product and catabolite can simply, be quickly and accurately effectively separated by this method, are easy to the preparation process of Amlodipine Besylate Tablet and the quality control of finished product.
Description
Technical field
The invention belongs to Pharmaceutical Analysis technical field, and in particular to a kind of high performance liquid chromatography detection Amlodipine Besylate Tablet
And its method for impurity.
Background technology
Amlodipine Besylate Tablet is a kind of cardiovascular drug with a chiral centre, is clinically mainly used in treating high blood
Pressure and angina pectoris, are third generation dihydrogen pyridine derivative calcium channel blockers, cardioselective is stronger.Promoting coronary blood flow
While can reduce blood pressure, can be the drug of first choice of current Hypertension with diastole coronary vasodilator and system vascular.
Amlodipine Besylate Tablet molecular formula is C20H25ClN2O5•C6H6O3S, chemistry are entitled（±）-2-[（2- amino ethoxies）First
Base] -4-（2- chlorphenyls）- Isosorbide-5-Nitrae-dihydro -6- methyl -3,5- pyridinedicarboxylic acid -5- methyl esters, 3- ethyl ester benzene sulfonates, structural formula
For：
The molecule has side reaction in building-up process, and the product of side reaction is likely to remain in molecule.And the compound
Also easily degraded produces impurity under the conditions of high temperature, illumination etc., and impurity caused by side reaction product and degraded shares 7, respectively
A, B, D, E, F, G and H are named as, structural formula sees below formula.These impurity can be remained in medicine, influence the quality and safety of medicine
Property.Therefore, the content of each impurity in Amlodipine Besylate Tablet is controlled, the quality to improving Amlodipine Besylate Tablet, is ensured vast
The security of patient medication is of great importance.
AB
DE
FG
H
For the impurity in Amlodipine Besylate Tablet, need to carry out quality control during pharmaceutical synthesis.It is however, secondary anti-
The separation for answering multiple impurity similar to principal component structure such as product, catabolite is always matter in pharmaceutical synthesis and production process
The difficult point of control is measured, by literature search, finds European Pharmacopoeia/British Pharmacopoeia（EP/BP）Above-mentioned impurity is controlled, but I
Carried out it is corresponding research find, principal component and each impurity can be effectively separated by EP/BP methods, but this method is resistance to
Poor with property, the C18 post separation Detection results of different brands differ greatly, and the retention time of impurity A is by mobile phase pH, organic
Situations such as Phase Proportion, chromatographic column, has a great influence, easily front and rear miscellaneous inseparable with it.
A kind of detection method of Levamlodipine beaylate tablets about material, this method are disclosed in CN105301164
Each impurity of P-TOLUENE SULFO ACID 99's Amlodipine is not positioned or identified, it is impossible to multiple known impurities and unknown miscellaneous are completely secured
Mass-energy, which reaches, to be efficiently separated；And impurity and main peak caused by degraded and not up to baseline separation after main peak in the patent；Impurity with
Separating degree between impurity does not reach requirement yet.
The content of the invention
For the above situation, the present invention is intended to provide a kind of separation of Amlodipine Besylate Tablet and its impurity based on HPLC
Detection method.Analysis Amlodipine Besylate Tablet and its impurity can simply, quickly and accurately be separated by this method, can be used for
The preparation process of Amlodipine Besylate Tablet and finished product quality control.
Specifically, the present invention adopts the following technical scheme that：
Step（1）The preparation of reference substance solution：It is each that precision weighs reference substance Amlodipine Besylate Tablet, impurity A, B, D, E, F, G and H
In right amount, add flowing phased soln, be made every milliliter of 1mg containing Amlodipine Besylate Tablet, impurity A, each 0.1mg of B, D, E, F, G and H it is molten
Liquid, as system suitability solution；
Step（2）The preparation of need testing solution：Precision weighs test sample Amlodipine Besylate Tablet, adds flowing phased soln, is made every 1
Ml 0.8 ~ 1.2mg Han Amlodipine Besylate Tablet sample solution；
Wherein step is poly-（1）Gather with step（2）The mobile phase of middle dissolving reference substance and test sample is mobile phase A, three second in mobile phase A
Amine aqueous solution is the aqueous solution that percent by volume is 0.3 ~ 0.8%, and the Preparation Method of matching somebody with somebody of triethylamine solution is the triethylamine for taking 3 ~ 8ml, is added
Water dilutes, and is quantified solution to 1000ml with after phosphorus acid for adjusting pH value to 3.5 ~ 4.5.
Step（3）High-efficient liquid phase chromatogram condition：Chromatographic column is Cl8 posts（4.6 × 250mm, 5 μm）；Mobile phase A is methanol：
Acetonitrile：Triethylamine solution=35:（20~25）:（40~45）(v:v:V), Mobile phase B is methanol, carries out gradient elution；Ultraviolet detection
Device, Detection wavelength 237nm；Flow velocity is 0.8 ~ 1.2ml/min, and 30 ~ 35 DEG C of column temperature, sample size is 5 ~ 20 μ l；
Gradient elution program is as follows：
Time：0 ~ 15min, mobile phase A 95% ~ 80%, Mobile phase B 5% ~ 20%;
Time：15 ~ 30min, mobile phase A 80% ~ 20%, Mobile phase B 20% ~ 80%;
Time：After 30min, mobile phase A is with Mobile phase B with volume ratio 80：20 operation 5min;
Step（4）Take step（1）The reference substance solution of middle preparation, high performance liquid chromatograph is injected, record chromatogram, take step
（2）The need testing solution of middle preparation, high performance liquid chromatograph is injected, record chromatogram, calculated using area normalization method for examination
Amlodipine Besylate Tablet, impurity A, the content of each material of B, D, E, F, G and H in product, Amlodipine Besylate Tablet and its front and rear impurity
Between separating degree should >=2.0, separating degree between other each peaks should >=1.5, complete separation detection process.
The present invention method can simply, quickly and accurately separate analysis Amlodipine Besylate Tablet and its side reaction product and
Catabolite impurity.Chromatographic column Phenomenex Gemini of the present invention using octadecylsilane chemically bonded silica as filler
Cl8 posts（4.6mm × 250mm, 5 μm）, using methanol-acetonitrile-triethylamine solution as A phases, using methanol as B phases, carry out gradient and wash
It is de-, Amlodipine Besylate Tablet and its side reaction product and catabolite can be effectively separated.Selective flow mixes desampling
Product, it is ensured that the stability of solution.
Brief description of the drawings
Fig. 1 is that mobile phase A is methanol in embodiment 1：Acetonitrile：0.5% triethylamine solution=35:20:45（v/v/v）HPLC
Collection of illustrative plates.
Fig. 2 is that mobile phase A is methanol in embodiment 2：Acetonitrile；0.3% triethylamine solution=35:23:42（v/v/v）HPLC
Collection of illustrative plates.
Mobile phase A is methanol in Fig. 3 embodiments 3：Acetonitrile；0.8% triethylamine solution=35:25:40（v/v/v）HPLC figure
Spectrum.
Embodiment
The technical scheme in the present invention is made below in conjunction with specific embodiments further elucidated above.Unless otherwise saying
Bright, reagent, material and instrument used in the following example can be obtained by routine business means.
Embodiment 1：
Instrument and condition：
High performance liquid chromatograph：Thermo U3000 (match is silent to fly)；
Chromatographic column：Phenomenex Gemini Cl8 posts（4.6mm × 250mm, 5 μm）；
Mobile phase A：Methanol：Acetonitrile：0.5% triethylamine solution=35:20:45（v/v/v）；The pH of 0.5% triethylamine solution is 4.0；
Mobile phase B：Methanol；
Gradient elution program
| Time/min | A% | B% |
| 0 | 95 | 5 |
| 15 | 80 | 20 |
| 30 | 20 | 80 |
| 35 | 20 | 80 |
Flow velocity：0.8ml/min；
Column temperature：30℃；
Detection wavelength：237nm；
Sampling volume：10μl.
Implementation steps：
It is each appropriate to weigh Amlodipine Besylate Tablet, impurity A, B, D, E, F, G and H, adds flowing phased soln and dilutes and be made every milliliter
1mg containing Amlodipine Besylate Tablet, impurity A, each 0.1mg of B, D, E, F, G and H solution, as system suitability solution.Take benzene sulphur
Sour Amlodipine 25mg, it is accurately weighed, it is placed in 25 ml volumetric flasks, adds flowing phased soln and be diluted to scale, as test sample
Solution.
Measure the μ l of system suitability solution 10 injection liquid chromatograph, record chromatogram, Amlodipine Besylate Tablet with its before
Separating degree between rear impurity should be not less than 2.0, and the separating degree between other each peaks should be not less than 1.5.Take the μ of need testing solution 10
L injects liquid chromatograph, records chromatogram, is calculated by area normalization method, each impurity content must not be big in Amlodipine Besylate Tablet
In 0.2%.
As a result accompanying drawing 1 is seen, Amlodipine Besylate Tablet retention time is 16.215min, and impurity A retention time is
42.115min, B retention time are 29.842min, and D retention times are 10.418 min, and E retention times are 20.680min, and F is protected
It is 12.405 min to stay the time, and G retention times are 26.737 min, and H retention times are 30.580 min, separating degree between each peak
2.0 are all higher than, each impurity content is less than 0.2%.
Embodiment 2：
Instrument and condition：
High performance liquid chromatograph：Thermo U3000 (match is silent to fly)；
Chromatographic column：Phenomenex Gemini Cl8 posts（4.6mm × 250mm, 5 μm）；
Mobile phase A：Methanol：Acetonitrile：0.3% triethylamine solution=35:23:42（v/v/v）；The pH of 0.3% triethylamine solution is 4.5；
Mobile phase B：Methanol
Gradient elution program
| Time/min | A% | B% |
| 0 | 95 | 5 |
| 15 | 80 | 20 |
| 30 | 20 | 80 |
| 35 | 20 | 80 |
Flow velocity：1.2ml/min；
Column temperature：35℃；
Detection wavelength：237nm；
Sampling volume：20μl.
Implementation steps：
Implementation steps：It is each appropriate to weigh Amlodipine Besylate Tablet, impurity A, B, D, E, F, G and H, adds flowing phased soln and dilutes system
Into every milliliter of 1mg containing Amlodipine Besylate Tablet, impurity A, each 0.1mg of B, D, E, F, G and H solution, it is molten as system suitability
Liquid.Amlodipine Besylate Tablet 30mg is taken, it is accurately weighed, it is placed in 25 ml volumetric flasks, adds flowing phased soln and be diluted to scale,
As need testing solution.
Measure the μ l of system suitability solution 20 injection liquid chromatograph, record chromatogram, Amlodipine Besylate Tablet with its before
Separating degree between miscellaneous afterwards should be not less than 2.0, and the separating degree between other each peaks should be not less than 1.5.Take the μ l of need testing solution 20
Liquid chromatograph is injected, chromatogram is recorded, is calculated by area normalization method, each impurity content cannot be greater than in Amlodipine Besylate Tablet
0.2%。
As a result accompanying drawing 2 is seen, Amlodipine Besylate Tablet retention time is 14.725 min, and impurity A retention time is 40.417
Min, B retention time are 28.225 min, and D retention times are 9.340 min, and E retention times are 19.035 min, when F retains
Between be 11.130 min, G retention times are 24.845 min, and H retention times are 28.958 min, and separating degree is big between each peak
In 2.0, each impurity content is less than 0.2%.
Embodiment 3
Instrument and condition：
High performance liquid chromatograph：Thermo U3000 (match is silent to fly)；
Chromatographic column：Phenomenex Gemini Cl8 posts（4.6mm × 250mm, 5 μm）；
Mobile phase A：Methanol：Acetonitrile：0.8% triethylamine solution=35:25:40（v/v/v）；The pH of 0.8% triethylamine solution is 3.5；
Mobile phase B：Methanol
Gradient elution program
| Time/min | A% | B% |
| 0 | 95 | 5 |
| 15 | 80 | 20 |
| 30 | 20 | 80 |
| 35 | 20 | 80 |
Flow velocity：1.0ml/min；
Column temperature：35℃；
Detection wavelength：237nm；
Sampling volume：15μl.
Implementation steps：
Implementation steps：It is each appropriate to weigh Amlodipine Besylate Tablet, impurity A, B, D, E, F, G and H, adds flowing phased soln and dilutes system
Into every milliliter of 1mg containing Amlodipine Besylate Tablet, impurity A, each 0.1mg of B, D, E, F, G and H solution, it is molten as system suitability
Liquid.Amlodipine Besylate Tablet 20mg is taken, it is accurately weighed, it is placed in 25 ml measuring bottles, adds flowing phased soln and be diluted to scale, make
For need testing solution.
Measure the μ l of system suitability solution 15 injection liquid chromatograph, record chromatogram, Amlodipine Besylate Tablet with its before
Separating degree between miscellaneous afterwards should be not less than 2.0, and the separating degree between other each peaks should be not less than 1.5.Take the μ l of need testing solution 15
Liquid chromatograph is injected, chromatogram is recorded, is calculated by area normalization method, each impurity content cannot be greater than in Amlodipine Besylate Tablet
0.2%。
As a result accompanying drawing 3 is seen, Amlodipine Besylate Tablet retention time is 13.763 min, and impurity A retention time is 39.213
Min, B retention time are 27.090 min, and D retention times are 8.608 min, and E retention times are 17.923 min, when F retains
Between be 10.327 min, G retention times are 23.622 min, and H retention times are 27.877 min, and separating degree is big between each peak
In 2.0, each impurity content is less than 0.2%.
Claims (5)
1. a kind of method of high performance liquid chromatography detection Amlodipine Besylate Tablet and its impurity, it is characterised in that：Benzene sulfonic acid ammonia chlorine
The concentration of Horizon sample is 0.8 ~ 1.2mg/ml;Chromatographic column is Cl8 posts, and 30 ~ 35 DEG C of column temperature, mobile phase A is methanol：Acetonitrile：Three
Ethylamine solution=35:（20~25）:（40~45）(v:v:V), Mobile phase B is methanol, carries out gradient elution；Detector is ultraviolet inspection
Survey device.
2. detection method according to claim 1, it is characterised in that gradient elution program is as follows：
Time：0 ~ 15min, mobile phase A 95% ~ 80%, Mobile phase B 5% ~ 20%;
Time：15 ~ 30min, mobile phase A 80% ~ 20%, Mobile phase B 20% ~ 80%;
Time：After 30min, mobile phase A is with Mobile phase B with volume ratio 80：20 operation 5min.
3. detection method according to claim 1, it is characterised in that the triethylamine solution in mobile phase A is volume basis
Than the aqueous solution for 0.3 ~ 0.8%, the pH value of triethylamine solution is 3.5 ~ 4.5.
4. detection method according to claim 1, it is characterised in that comprise the following steps：
（1）The preparation of reference substance solution：It is each suitable that precision weighs reference substance Amlodipine Besylate Tablet, impurity A, B, D, E, F, G and H
Amount, add flowing phased soln, be made every milliliter of 1mg containing Amlodipine Besylate Tablet, impurity A, each 0.1mg of B, D, E, F, G and H it is molten
Liquid, as system suitability solution；
（2）The preparation of need testing solution：Precision weighs test sample Amlodipine Besylate Tablet, adds flowing phased soln, and every 1 ml is made
The sample solution of 0.8 ~ 1.2mg containing Amlodipine Besylate Tablet；
（3）High-efficient liquid phase chromatogram condition：Chromatographic column is Cl8 posts；Mobile phase A is methanol：Acetonitrile：Triethylamine solution=35:（20~
25）:（40~45）(v:v:V), Mobile phase B is methanol, carries out gradient elution；UV-detector, Detection wavelength 237nm；Flow velocity
For 0.8 ~ 1.2ml/min, 30 ~ 35 DEG C of column temperature, sample size is 5 ~ 20 μ l；
Gradient elution program is as follows：
Time：0 ~ 15min, mobile phase A 95% ~ 80%, Mobile phase B 5% ~ 20%;
Time：15 ~ 30min, mobile phase A 80% ~ 20%, Mobile phase B 20% ~ 80%;
Time：After 30min, mobile phase A is with Mobile phase B with volume ratio 80：20 operation 5min;
（4）Take step（1）The reference substance solution of middle preparation, high performance liquid chromatograph is injected, record chromatogram；Take step（2）In
The need testing solution of preparation, high performance liquid chromatograph is injected, record chromatogram；Benzene in test sample is calculated using area normalization method
Sulfonic acid Amlodipine, impurity A, the content of each material of B, D, E, F, G and H, between Amlodipine Besylate Tablet and its front and rear impurity
Separating degree should >=2.0, separating degree between other each peaks should >=1.5, complete separation detection process.
5. detection method according to claim 4, it is characterised in that step is poly-（1）Gather with step（2）It is middle dissolving reference substance and
The mobile phase of test sample is mobile phase A.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110286185A (en) * | 2018-06-11 | 2019-09-27 | 南京济群医药科技股份有限公司 | A kind of Phenylsulfonic acid amido chloro diping dispersion tablet dissolution curve measuring method |
| CN114478571A (en) * | 2022-01-25 | 2022-05-13 | 安徽美致诚药业有限公司 | Preparation method of amlodipine besylate degradation impurities and detection method of impurities in amlodipine besylate |
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Cited By (2)
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| CN110286185A (en) * | 2018-06-11 | 2019-09-27 | 南京济群医药科技股份有限公司 | A kind of Phenylsulfonic acid amido chloro diping dispersion tablet dissolution curve measuring method |
| CN114478571A (en) * | 2022-01-25 | 2022-05-13 | 安徽美致诚药业有限公司 | Preparation method of amlodipine besylate degradation impurities and detection method of impurities in amlodipine besylate |
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