CN101531601B - Method for separating and analyzing dopexamine hydrochloride by using HPLC method - Google Patents
Method for separating and analyzing dopexamine hydrochloride by using HPLC method Download PDFInfo
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- CN101531601B CN101531601B CN200810101630.2A CN200810101630A CN101531601B CN 101531601 B CN101531601 B CN 101531601B CN 200810101630 A CN200810101630 A CN 200810101630A CN 101531601 B CN101531601 B CN 101531601B
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- dopexamine hydrochloride
- dopexamine
- analyzing
- hydrochloride
- separating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/26—Selective adsorption, e.g. chromatography characterised by the separation mechanism
- B01D15/30—Partition chromatography
- B01D15/305—Hydrophilic interaction chromatography [HILIC]
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- Treatment Of Liquids With Adsorbents In General (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Investigating Or Analysing Biological Materials (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a method for separating, analyzing and determining relevant substances of dopexamine hydrochloride, which adopts an HILIC affinity chromatographic column (250mm multiplied by 4.6mm, 5 microns). Buffer salt which is an organic modifying agent and contains organic base is adopted as a moving phase. The method is used for rapidly separating and analyzing the dopexamine hydrochloride and the relevant substances.
Description
Technical field
The present invention relates to a kind of high-efficient liquid phase analysis separation method, particularly a kind of method with high performance liquid chromatography separating and analyzing dopexamine hydrochloride.
Background technology
Dopexamine hydrochloride has very strong β
2adrenergic receptor excitation, is mainly used in the low patient of cardiac output after acute heart failure and heart operation.Its structural formula is:
Molecular formula is C
22h
34cl
2n
2o
2, molecular weight 429.4
Dopexamine hydrochloride has stronger polarity compared with its intermediate, the sharp separation of realizing them under same chromatographic condition has larger difficulty, therefore, realize dopexamine hydrochloride and its intermediate fast, be simply separated in dopexamine hydrochloride quality control aspect synthetic and preparation process have important practical significance.
Summary of the invention
The object of the present invention is to provide a kind of efficient liquid-phase chromatography method of simple, sharp separation analyzing dopexamine hydrochloride related substance, thereby realize the quality control to dopexamine hydrochloride.
Applicant finds, with HILIC affinity post, taking buffering salt-organic modifiers of containing organic bases as moving phase, can realize dopexamine hydrochloride and its intermediate simply, sharp separation, thereby can accurately control the quality of dopexamine hydrochloride and preparation thereof.
The said method with high performance liquid chromatography separating and analyzing dopexamine hydrochloride of the present invention, selects HILIC affinity chromatography post, taking sodium acetate buffer-acetonitrile as moving phase, wherein contains a small amount of organic bases.
The chromatographic column that the present invention adopts is that (250mm × 4.6mm, 5 μ m) for HILIC affinity chromatography post.
The organic modifiers that the present invention adopts is selected from acetonitrile, methyl alcohol, and most preferred organic modifiers is acetonitrile.
In the moving phase of method of the present invention, the volume ratio of sodium acetate buffer-organic modifiers mixing solutions is 40: 60～62: 38.
The organic bases comprising in the moving phase of the inventive method is selected from quadrol, diethylamine, triethylamine, and most preferred is triethylamine, and the concentration of organic bases is (V/V) 0.1%～0.5%.
Method for separating and analyzing of the present invention, can realize in accordance with the following methods:
(1) take dopexamine hydrochloride sample appropriate, use moving phase sample dissolution, be mixed with the sample solution of every 1mL containing formoterol tartrate 0.2mg～2mg.
(2) flow rate of mobile phase being set is 0.6～1.2mL/min, and detection wavelength is 280 ± 3nm.
(3) get the sample solution 2-50 μ L injection liquid chromatography of step (1), complete the separation and analysis of dopexamine hydrochloride.
Wherein:
High performance liquid chromatograph: Shimadzu: LC-10ATvp, SPD-M10Avp, SCL-10Avp, DGU-12A
Chromatographic column: (250mm × 4.6mm, 5 μ m) for HILIC affinity chromatography post
Moving phase: sodium acetate buffer-acetonitrile-triethylamine=50: 50: 0.2
Flow velocity: 1.0mL/min
Detect wavelength: 280nm
Column temperature: room temperature
Sampling volume: 20 μ L
The present invention adopt HILIC affinity chromatography post (250mm × 4.6mm, 5 μ m), effectively separating and analyzing dopexamine hydrochloride related substance; Selective flow phased soln sample, can eliminate solvent to the interference detecting; Select sampling volume 20 μ L, column temperature is room temperature, adds organic bases to improve the symmetry of chromatographic peak.The invention solves the problem of simple, sharp separation and analyzing dopexamine hydrochloride related substance, thereby guaranteed the quality controllable of dopexamine hydrochloride bulk drug and preparation.
Brief description of the drawings
Fig. 1 embodiment 1, sodium acetate buffer-acetonitrile (50: 50) also adds dopexamine hydrochloride and the intermediate biased sample high-efficient liquid phase chromatogram of triethylamine
Fig. 2 embodiment 2, sodium acetate buffer-acetonitrile (50: 50) also adds the dopexamine hydrochloride high-efficient liquid phase chromatogram of triethylamine
Fig. 3 embodiment 3, sodium acetate buffer-acetonitrile (50: 50) dopexamine hydrochloride high-efficient liquid phase chromatogram
Embodiment: following examples are used for further understanding the present invention, but be not limited to the scope of this enforcement.
Embodiment 1
Instrument and condition
High performance liquid chromatograph: Japanese Shimadzu: LC-10Avp, SPD-10Avp;
Chromatographic column: (250mm × 4.6mm, 5 μ m) for HILIC affinity chromatography post
Moving phase: sodium acetate buffer-acetonitrile-triethylamine (40: 60: 0.2)
Flow velocity: 1.0mL/min;
Detect wavelength: 280nm;
Column temperature: room temperature;
Sampling volume: 20 μ L.
Experimental procedure
Take dopexamine hydrochloride 50mg, intermediate compound I, the each 10mg of intermediate II, be placed in 50mL volumetric flask, adds moving phase and dissolve and be diluted to scale, shakes up, as need testing solution.Get need testing solution, under above-mentioned chromatographic condition, carry out efficient liquid phase chromatographic analysis, record color atlas, the results are shown in accompanying drawing 1.
In Fig. 1, retention time is the chromatographic peak that the chromatographic peak of 5.150 minutes is dopexamine hydrochloride.Retention time is that the chromatographic peak of 3.250 minutes and 6.050 minutes is the chromatographic peak of intermediate compound I and intermediate II.Color atlas shows that dopexamine hydrochloride can reach quick, good separating with its intermediate.
Embodiment 2
Instrument and condition
High performance liquid chromatograph: Japanese Shimadzu: LC-10Avp, SPD-10Avp;
Chromatographic column: (250mm × 4.6mm, 5 μ m) for HILIC affinity chromatography post
Moving phase: sodium acetate buffer-acetonitrile-triethylamine (40: 60: 0.2)
Flow velocity: 1.0mL/min;
Detect wavelength: 280nm;
Column temperature: room temperature;
Sampling volume: 20 μ L.
Experimental procedure
Take dopexamine hydrochloride 50mg, be placed in 50mL volumetric flask, add moving phase and dissolve and be diluted to scale, shake up, as need testing solution.Get need testing solution, under above-mentioned chromatographic condition, carry out efficient liquid phase chromatographic analysis, record color atlas, the results are shown in accompanying drawing 2.
Embodiment 3
Instrument and condition
High performance liquid chromatograph: Japanese Shimadzu: LC-10Avp, SPD-10Avp;
Chromatographic column: (250mm × 4.6mm, 5 μ m) for HILIC affinity chromatography post
Moving phase: sodium acetate buffer-acetonitrile (40: 60 :)
Flow velocity: 1.0mL/min;
Detect wavelength: 280nm;
Column temperature: room temperature;
Sampling volume: 20 μ L.
Experimental procedure
Take dopexamine hydrochloride 50mg, be placed in 50mL volumetric flask, add moving phase and dissolve and be diluted to scale, shake up, as need testing solution.Get need testing solution, under above-mentioned chromatographic condition, carry out efficient liquid phase chromatographic analysis, record color atlas, the results are shown in accompanying drawing 3.
Claims (3)
1. a method for high performance liquid chromatography separating and analyzing dopexamine hydrochloride related substance, is characterized in that adopting HILIC affinity post, taking sodium acetate buffer-acetonitrile-triethylamine=50:50:0.2 as moving phase.
2. method according to claim 1, is characterized in that described chromatographic column is HILIC affinity chromatography post 250 × 4.6mm, 5 μ m.
3. method according to claim 1, is characterized in that comprising the following steps:
(1) take dopexamine hydrochloride sample appropriate, use moving phase sample dissolution, be mixed with the solution of the hydrochloric dopexamine sample of every 1mL 0.2～2mg;
(2) flow rate of mobile phase being set is 0.6～1.2mL/min, and detection wavelength is 280 ± 3nm;
(3) get the sample solution 2-50 μ L injection liquid chromatography of step (1), complete the separation and analysis of dopexamine hydrochloride and related substance thereof.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810101630.2A CN101531601B (en) | 2008-03-10 | 2008-03-10 | Method for separating and analyzing dopexamine hydrochloride by using HPLC method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810101630.2A CN101531601B (en) | 2008-03-10 | 2008-03-10 | Method for separating and analyzing dopexamine hydrochloride by using HPLC method |
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| Publication Number | Publication Date |
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| CN101531601A CN101531601A (en) | 2009-09-16 |
| CN101531601B true CN101531601B (en) | 2014-07-09 |
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| CN200810101630.2A Active CN101531601B (en) | 2008-03-10 | 2008-03-10 | Method for separating and analyzing dopexamine hydrochloride by using HPLC method |
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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101920130B (en) * | 2010-08-11 | 2013-01-02 | 苏州大学 | Sample loading device for column chromatography |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1813693A (en) * | 2005-11-30 | 2006-08-09 | 山东长富洁晶药业有限公司 | Dopexamine hydrochloride injection and its preparing method |
| WO2007008907A2 (en) * | 2005-07-11 | 2007-01-18 | Abbott Laboratories | Methods for determining how to treat congestive heart failure |
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2008
- 2008-03-10 CN CN200810101630.2A patent/CN101531601B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007008907A2 (en) * | 2005-07-11 | 2007-01-18 | Abbott Laboratories | Methods for determining how to treat congestive heart failure |
| CN1813693A (en) * | 2005-11-30 | 2006-08-09 | 山东长富洁晶药业有限公司 | Dopexamine hydrochloride injection and its preparing method |
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Effective date of registration: 20201130 Address after: No. 279 Nanhai Road, Xiuying District 570314 Hainan city of Haikou Province Patentee after: AVENTIS PHARMA (HAINAN) Co.,Ltd. Address before: 100097, Wanquan mansion, 3 Jin Zhuang, Haidian District, Beijing, Sijiqing Patentee before: BEIJING D-VENTURE PHARMACEUTICAL TECHNOLOGY Corp. |
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