CN111141845A - Analysis and detection method of vildagliptin - Google Patents

Analysis and detection method of vildagliptin Download PDF

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CN111141845A
CN111141845A CN201911395673.0A CN201911395673A CN111141845A CN 111141845 A CN111141845 A CN 111141845A CN 201911395673 A CN201911395673 A CN 201911395673A CN 111141845 A CN111141845 A CN 111141845A
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vildagliptin
solution
concentration
detection method
phase
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刘倩
张莹
平熠熠
张晨烨
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Zhuohe Pharmaceutical Group Co Ltd
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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
    • 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
    • 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
    • G01N30/26—Conditioning of the fluid carrier; Flow patterns
    • G01N30/28—Control of physical parameters of the fluid carrier
    • G01N30/30—Control of physical parameters of the fluid carrier of temperature
    • 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
    • G01N30/26—Conditioning of the fluid carrier; Flow patterns
    • G01N30/28—Control of physical parameters of the fluid carrier
    • G01N30/32—Control of physical parameters of the fluid carrier of pressure or speed
    • 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
    • G01N30/26—Conditioning of the fluid carrier; Flow patterns
    • G01N30/28—Control of physical parameters of the fluid carrier
    • G01N30/34—Control of physical parameters of the fluid carrier of fluid composition, e.g. gradient
    • 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
    • G01N30/62—Detectors specially adapted therefor
    • G01N30/74—Optical detectors
    • 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
    • G01N30/86—Signal analysis
    • G01N30/8624—Detection of slopes or peaks; baseline correction
    • G01N30/8631—Peaks
    • G01N30/8637—Peak shape
    • 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
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    • G01N2030/047—Standards external
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    • 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
    • G01N30/26—Conditioning of the fluid carrier; Flow patterns
    • G01N30/28—Control of physical parameters of the fluid carrier
    • G01N30/32—Control of physical parameters of the fluid carrier of pressure or speed
    • G01N2030/324—Control of physical parameters of the fluid carrier of pressure or speed speed, flow rate

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  • Treatment Of Liquids With Adsorbents In General (AREA)

Abstract

The invention discloses an analysis and detection method of vildagliptin, which comprises the following steps: performing High Performance Liquid Chromatography (HPLC) to obtain C18 chromatographic column, wherein the mobile phase comprises water phase and organic phase, and isocratic elution is performed according to volume fraction; and performing quantitative analysis by using an external standard method. In the analysis method, an octadecylsilane chemically bonded silica chromatographic column, a chromatographic column with the size of 150 x 4.6mm and the size of 5 mu or equivalent thereof is adopted, the pH value of a water phase in a mobile phase is adjusted to be 1.5 to 3.5 by phosphoric acid, and the volume ratio of the water phase in the mobile phase to an organic phase is 3: 7 to 1: 1, the detection wavelength is 276nm to 280nm, the column temperature is 30 to 40 ℃, the sample amount is 10 mu l to 20 mu l, the flow rate is 0.8 to 1.2ml/min, and isocratic elution is carried out. Through a series of examinations on the chromatographic conditions, the fact that the chromatographic conditions are simple and convenient, the content of vildagliptin can be accurately detected, and the reproducibility is good can be found.

Description

Analysis and detection method of vildagliptin
FIELD
The invention relates to the technical field of drug analysis, in particular to a vildagliptin analysis and detection method.
Background
The glucagon secretion promoting effect of GIP of type 2 diabetes patients is impaired, only GLP21 can play the secretion promoting effect of insulin hormone, and the secretion promoting effect can promote the secretion of insulin by acting on a receptor on the cell membrane of pancreatic islet β. GLP21 can also inhibit the secretion of glucagon and inhibit gastric emptying so as to increase satiety (inhibit appetite). DPP24 is combined with protein and exists in a plurality of tissues, such as brush edges of kidney, liver and small intestine membranes, pancreatic duct, lymphocyte and endothelial cell, and can rapidly inactivate the glucagon by hydrolyzing the 2 nd alanine at the N terminal of GLP 21. the activity of the DPP24 complex formed by combining the DPP24 is inhibited, so that the activity of the enzyme is obviously influenced by reducing the blood sugar concentration and reducing the glucagon concentration while the concentration of GLP21 is increased and the insulin is promoted by insulin producing by the cell of the GLP 734.
SUMMARY
The present disclosure relates to an analytical detection method for vildagliptin, which comprises:
performing High Performance Liquid Chromatography (HPLC) to obtain C18 chromatographic column, wherein the mobile phase comprises water phase and organic phase, and isocratic elution is performed according to volume fraction; and
quantitative analysis was performed by external standard method.
Brief description of the drawings
Figure 1 shows a blank solution profile.
Fig. 2 shows a high performance liquid chromatogram of vildagliptin in example 1.
Fig. 3 shows a high performance liquid chromatogram of vildagliptin in example 2.
Fig. 4 shows a high performance liquid chromatogram of vildagliptin in example 3.
Detailed description of the invention
In the following description, certain specific details are included to provide a thorough understanding of various disclosed embodiments. One skilled in the relevant art will recognize, however, that the embodiments can be practiced without one or more of the specific details, or with other methods, components, materials, and so forth.
Unless otherwise required by the disclosure, throughout the specification and the appended claims, the words "comprise", "comprising", and "have" are to be construed in an open, inclusive sense, i.e., "including but not limited to".
Reference throughout the specification to "one embodiment," "an embodiment," "in another embodiment," or "in certain embodiments" means that a particular reference element, structure, or characteristic described in connection with the embodiment is included in at least one embodiment. Thus, the appearances of the phrases "in one embodiment" or "in an embodiment" or "in another embodiment" or "in certain embodiments" in various places throughout this specification are not necessarily all referring to the same embodiment, and furthermore, particular elements, structures, or features may be combined in any suitable manner in one or more embodiments.
Definition of
In the present disclosure, the term "external standard method" refers to a method of quantifying by comparing response signals of a control substance and a component to be measured in a sample using a pure product of the component to be measured as the control substance.
In the present disclosure, the term "isocratic elution" refers to an elution pattern in which the composition and flow rate of a mobile phase are constant over an analysis cycle of a sample component.
Detailed Description
The present disclosure relates to an analytical detection method for vildagliptin, which comprises:
performing High Performance Liquid Chromatography (HPLC) to obtain C18 chromatographic column, wherein the mobile phase comprises water phase and organic phase, and isocratic elution is performed according to volume fraction; and
quantitative analysis was performed by external standard method.
In certain embodiments, further comprising the preparation of a pre-liquid chromatography detection solution comprising:
a blank solution, the blank solution consisting of ethanol;
the test solution consists of a vildagliptin sample and ethanol; and
the reference substance solution consists of a vildagliptin reference substance and ethanol. In certain embodiments, a sample of vildagliptin is dissolved in a solvent to formulate a test solution.
In certain embodiments, the solvent is selected from methanol, ethanol, or mixtures thereof.
In certain embodiments, the solvent is selected from ethanol.
In certain embodiments, the test solution has a concentration of 0.1 to 5 mg/ml.
In certain embodiments, the test solution has a concentration of 0.2 to 0.8 mg/ml.
In certain embodiments, the test solution has a concentration of 0.5 mg/ml.
In certain embodiments, the vildagliptin control is dissolved in a solvent to make a control solution.
In certain embodiments, the vildagliptin control is vildagliptin pure substance.
In certain embodiments, the solvent is selected from methanol, ethanol, or mixtures thereof.
In certain embodiments, the solvent is selected from ethanol.
In certain embodiments, the control solution has a concentration of 0.1 to 5 mg/ml.
In certain embodiments, the control solution concentration is 0.2 to 0.8 mg/ml.
In certain embodiments, the control solution has a concentration of 0.5 mg/ml.
In certain embodiments, the chromatography column is sized (150mm by 4.6mm,5 μ).
Wherein: the octadecylsilane chemically bonded silica chromatographic column is selected, so that vildagliptin can be kept for a longer time, the chromatographic column has a longer service life, the cost is saved, the determination of vildagliptin content is more accurate, and the reproducibility is good.
In certain embodiments, the aqueous phase comprises water and an acid formulation.
In certain embodiments, the acid reagent is selected from phosphoric acid, hydrochloric acid, trifluoroacetic acid, or mixtures thereof.
In certain embodiments, the acid reagent is selected from phosphoric acid.
In certain embodiments, the aqueous phase in the mobile phase has a pH of 1.5 to 3.5, which is adjusted by the acid agent.
Wherein, within the pH value range, the peak type symmetry is good and the reproducibility is good.
In certain embodiments, the organic solvent is selected from acetonitrile, ethanol, methanol, or mixtures thereof.
In certain embodiments, the organic solvent is selected from methanol.
In certain embodiments, the volume ratio of the aqueous phase to the organic phase in the flowability is 3: 7 to 1: 1.
in the volume ratio range of the water phase and the organic phase, the vildagliptin can obtain parameters such as better peak type and better retention time.
In certain embodiments, the ultraviolet absorption light detector detects wavelengths from 276nm to 280 nm.
Wherein, the ultraviolet absorption of vildagliptin is higher near 278, so the wavelength of 278 plus or minus 2nm is selected, which can make the peak type symmetry good and the reproducibility good.
In certain embodiments, the column temperature of the chromatography column is from 30 to 40 ℃.
In the column temperature range, vildagliptin can obtain a better peak pattern, and the elution time is more ideal.
In certain embodiments, the flow rate of the chromatography column is 0.8 to 1.2 ml/min.
In the flow rate range, the obtained peak theoretical plate number is better, and the elution time is more ideal.
In certain embodiments, the sample size is from 10. mu.l to 20. mu.l.
In the range of the sample injection amount, the number of the obtained peak theoretical plates is better, and the elution time is more ideal.
Example 1
Using an Agilent ZORBAX XDB-C18 column, 150 x 4.6mm,5 μ or equivalent column, adjusting pH of the aqueous phase in the mobile phase to 1.5 with phosphoric acid, and adjusting volume ratio of the mobile phase to 30: 70 phosphoric acid aqueous solution: methanol, column temperature 30 deg.C, detection wavelength 276nm, flow rate 0.8ml/min, and sample amount 10 μ l.
The specific process is as follows:
taking a proper amount of vildagliptin, precisely weighing, adding ethanol for dissolving and diluting to prepare a solution containing about 0.5mg/ml vildagliptin in every 1 ml; preparing a reference solution by the same method; and (3) taking 10 mu l of each of the reference solution and the test solution, injecting the reference solution and the test solution into a liquid chromatograph according to the chromatographic conditions, and recording a chromatogram. The content is calculated according to an external standard method.
As shown in FIG. 1, the spectrum of the blank solution is a horizontal straight line and no peak appears.
As shown in fig. 2, which is a high performance liquid chromatogram of vildagliptin, the peak-appearance retention time of vildagliptin is 7.082min, and the peak area is 2821.4969.
The formula is calculated by an external standard method: content (%) - (test article peak area × control article concentration)/(control article peak area × test article concentration) × 100%
The theoretical plate number calculation formula is as follows: theoretical plate number ═ retention time/peak width2
Wherein the peak area of the test sample is 2821.4969, the concentration of the test sample is 0.4930mg/ml, the peak area of the reference sample is 2956.5220, and the concentration of the reference sample is 0.5155 mg/ml. The retention time of the test sample is 7.082min, and the peak width is 0.073.
The vildagliptin content is 99.7% calculated by an external standard method.
System usability measurement results: the number of theoretical plates of vildagliptin is 9412.
Example 2
Using Phenomenex Luna C18 chromatographic column, 150 × 4.6mm,5 μ or equivalent chromatographic column, adjusting pH of water phase in mobile phase to 3.5 with phosphoric acid, and adjusting volume ratio of mobile phase to 50: 50 phosphoric acid aqueous solution: methanol, column temperature 40 deg.C, detection wavelength 280nm, flow rate 1.2ml/min, and sample amount 10 μ l.
The specific process is as follows:
preparation of a test solution: taking a proper amount of vildagliptin, precisely weighing, adding ethanol for dissolving and diluting to prepare a solution containing about 0.5mg/ml vildagliptin in every 1 ml; preparing a reference solution by the same method; and (3) taking 10 mu l of each of the reference solution and the test solution, injecting the reference solution and the test solution into a liquid chromatograph according to the chromatographic conditions, and recording a chromatogram.
As shown in fig. 3, which is a high performance liquid chromatogram of vildagliptin, the peak-appearance retention time of vildagliptin is 8.213min, and the peak area is 3426.0310.
The formula is calculated by an external standard method: content (%) - (test article peak area × control article concentration)/(control article peak area × test article concentration) × 100%
The theoretical plate number calculation formula is as follows: theoretical plate number ═ retention time/peak width2
Wherein the peak area of the test sample is 3426.0310, the concentration of the test sample is 0.5145mg/ml, the peak area of the reference sample is 3349.6730, and the concentration of the reference sample is 0.5010 mg/ml. The retention time of the test sample is 8.213min, and the peak width is 0.084.
The vildagliptin content is 99.6% calculated by an external standard method.
System usability measurement results: the number of vildagliptin theoretical plates is 9560.
Example 3
By using
Figure BDA0002346231400000051
DB C18 hydrophilic column, 150 x 4.6mm,5 μ or equivalent column, mobile phase aqueous phase adjusted pH 2.3 with phosphoric acid, mobile phase 40: 60 phosphoric acid aqueous solution: methanol, column temperature 35 deg.C, detection wavelength 278nm, flow rate 1.0ml/min, sample size 10 μ l.
The specific process is as follows:
preparation of a test solution: taking a proper amount of vildagliptin, precisely weighing, adding ethanol for dissolving and diluting to prepare a solution containing about 0.5mg/ml vildagliptin in every 1 ml; preparing a reference solution by the same method; and (3) taking 10 mu l of each of the reference solution and the test solution, injecting the reference solution and the test solution into a liquid chromatograph according to the chromatographic conditions, and recording a chromatogram. The content is calculated according to an external standard method.
As shown in fig. 4, which is a high performance liquid chromatogram of vildagliptin, the peak-appearance retention time of vildagliptin is 7.909min, and the peak area is 2537.9648.
The formula is calculated by an external standard method: content (%) - (test article peak area × control article concentration)/(control article peak area × test article concentration) × 100%
The theoretical plate number calculation formula is as follows: theoretical plate number ═ retention time/peak width2
Wherein the peak area of the test sample is 2537.9648, the concentration of the test sample is 0.5358mg/ml, the peak area of the reference sample is 2570.5748, and the concentration of the reference sample is 0.5387 mg/ml. The retention time of the test sample is 7.909min, and the peak width is 0.080.
The vildagliptin content is 99.3% calculated by an external standard method.
System usability measurement results: the number of vildagliptin theoretical plates is 9774.
From the foregoing it will be appreciated that, although specific embodiments of the disclosure have been described herein for purposes of illustration, various modifications or improvements may be made by those skilled in the art without departing from the spirit and scope of the disclosure, and that such modifications or improvements are intended to be within the scope of the appended claims.

Claims (9)

1. The analysis and detection method of vildagliptin comprises the following steps:
performing High Performance Liquid Chromatography (HPLC) to obtain C18 chromatographic column, wherein the mobile phase comprises water phase and organic phase, and isocratic elution is performed according to volume fraction; and
quantitative analysis was performed by external standard method.
2. The assay of claim 1 further comprising the preparation of a pre-liquid chromatography assay solution comprising:
a blank solution, the blank solution consisting of ethanol;
the test solution consists of a vildagliptin sample and ethanol; and
the reference substance solution consists of a vildagliptin reference substance and ethanol.
3. The detection method according to claim 1 or 2, wherein the concentration of the test solution is 0.1 to 5mg/ml, preferably the concentration of the test solution is 0.2 to 0.8mg/ml, more preferably the concentration of the test solution is 0.5 mg/ml; the concentration of the control solution is 0.1 to 5mg/ml, preferably the concentration of the control solution is 0.2 to 0.8mg/ml, and more preferably the concentration of the control solution is 0.5 mg/ml.
4. The assay of any one of claims 1 to 3 wherein the aqueous phase comprises water and an acid reagent, preferably the acid reagent is selected from phosphoric acid, hydrochloric acid, trifluoroacetic acid or mixtures thereof, more preferably the acid reagent is selected from phosphoric acid.
5. The assay of claim 4 wherein the aqueous phase in the mobile phase has a pH of from 1.5 to 3.5, said pH being adjusted by the acid reagent.
6. The detection method according to claim 4 or 5, wherein the solvent of the organic phase is selected from acetonitrile, ethanol, methanol or a mixture thereof, preferably the organic solvent is selected from methanol.
7. The detection method according to any one of claims 4 to 6, wherein the volume ratio of the aqueous phase to the organic phase in the fluidity is 3: 7 to 1: 1.
8. the detection method according to claim 7, wherein the detection wavelength of the ultraviolet absorption photodetector is 276nm to 280 nm.
9. The detection method according to claim 7 or 8, wherein the column temperature of the chromatography is 30 to 40 ℃, the flow rate of the chromatography is 0.8 to 1.2ml/min, and the sample amount is 10 to 20 μ l.
CN201911395673.0A 2019-12-30 2019-12-30 Analysis and detection method of vildagliptin Pending CN111141845A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20080167479A1 (en) * 2007-01-10 2008-07-10 Medichem, S.A. Process for preparing vildagliptin
CN106966944A (en) * 2017-03-01 2017-07-21 山东裕欣药业有限公司 A kind of vildagliptin crystal-form compound and preparation method thereof
CN108689905A (en) * 2017-12-27 2018-10-23 河北医科大学 A kind of vildagliptin impurity compound and preparation method thereof, detection method and purposes

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20080167479A1 (en) * 2007-01-10 2008-07-10 Medichem, S.A. Process for preparing vildagliptin
CN106966944A (en) * 2017-03-01 2017-07-21 山东裕欣药业有限公司 A kind of vildagliptin crystal-form compound and preparation method thereof
CN108689905A (en) * 2017-12-27 2018-10-23 河北医科大学 A kind of vildagliptin impurity compound and preparation method thereof, detection method and purposes

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
K. HANUMANTHA RAO 等: "DEVELOPMENT AND VALIDATION OF HPLC METHOD FOR THE ESTIMATION OF VILDAGLIPTIN IN PHARMACEUTICAL DOSAGE FORM", 《INTERNATIONAL JOURNAL OF PHARMACEUTICAL, CHEMICAL AND BIOLOGICAL SCIENCES》 *
SAVITA V. POL 等: "Formulation and Evaluation of Fast Dissolving Buccal Film containing Vildagliptin", 《 AMERICAN JOURNAL OF PHARMACY & HEALTH RESEARCH》 *
李燕 等: "HPLC法测定维格列汀片中主药和有关物质的含量", 《中国药房》 *
马廉举 等: "反相高效液相色谱法测定维格列汀", 《光谱实验室》 *

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