CN102043023B - Method for measuring materials associated with Ropinirole hydrochloride by high performance liquid chromatography - Google Patents
Method for measuring materials associated with Ropinirole hydrochloride by high performance liquid chromatography Download PDFInfo
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- CN102043023B CN102043023B CN200910236173.2A CN200910236173A CN102043023B CN 102043023 B CN102043023 B CN 102043023B CN 200910236173 A CN200910236173 A CN 200910236173A CN 102043023 B CN102043023 B CN 102043023B
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- ropinirole hydrochloride
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- liquid chromatography
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Abstract
The invention discloses a separation and analysis measurement method for materials associated with Ropinirole hydrochloride. In the method, a chromatographic column taking phenylchemically bonded silica as a filler is adopted, and cation pair buffer salt solution and an organic modifier form a flowing phase. The method is used for separating and analyzing materials associated with Ropinirole hydrochloride.
Description
Technical field
The invention belongs to and relate to a kind of high performance liquid chromatography method for separating and analyzing, particularly a kind of method with high performance liquid chromatography compartment analysis ropinirole hydrochloride related substance.
Background technology
Ropinirole hydrochloride is that one is treated Parkinsonian novel dopamine agonist, is mainly used in treating Parkinson's.Chemistry 4-(2-(dipropylamino) ethyl) indolin-2-onehydrochloride by name, its structural formula:
Molecular formula: C
16h
25clN
2o, molecular weight: 296.17
This law is effectively carried out purity analysis to ropinirole hydrochloride, this test adopts common chromatographic column (phenyl chromatographic column) to realize fast and accurately the mensuration of ropinirole hydrochloride related substance, thereby realize the control of ropinirole hydrochloride impurity, guaranteed the quality controllable of ropinirole hydrochloride, the quality control of synthetic and preparation process aspect 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 compartment analysis ropinirole hydrochloride related substance, thereby realize the quality control to ropinirole hydrochloride.
Applicant finds, the chromatographic column that is filling agent with phenyl silane bonded silica gel, take negative ion to buffer salt solution one organic modifiers as mobile phase, can realize the separation and analysis of ropinirole hydrochloride and its intermediate, thereby can accurately control the quality of ropinirole hydrochloride and preparation thereof.
The said method with high performance liquid chromatography compartment analysis ropinirole hydrochloride of the present invention, selecting phenyl silane bonded silica gel is the chromatographic column of filling agent, take sodium heptanesulfonate to potassium phosphate buffer (pH5.0)-acetonitrile as mobile phase.
The chromatographic column that the present invention adopts is that phenyl silane bonded silica gel is that (250mm × 4.6mm, 5 μ m) for the chromatographic column of filling agent.
The organic modifiers that the present invention adopts is selected from acetonitrile, methyl alcohol, and most preferred organic modifiers is acetonitrile.
In the mobile phase of the inventive method, sodium heptanesulfonate is 80:20～75:25 to the volume ratio of potassium phosphate buffer (pH5.0)-organic modifiers mixed solution.
The sodium heptanesulfonate of the inventive method is 5.0 to potassium phosphate buffer pH value.
Method for separating and analyzing of the present invention, can realize in accordance with the following methods:
(1) take ropinirole hydrochloride sample appropriate, use mobile phase dissolution sample, be mixed with the about saliferous of every 1ml
The sample solution of acid Ropinirole 0.2mg～2mg.
(2) flow rate of mobile phase being set is 0.8～1.2ml/min, and detection wavelength is 250nm.
(3) get the sample solution 5-40 μ l injection liquid chromatography of step (1), complete ropinirole hydrochloride point
From with analysis.
Wherein:
High performance liquid chromatograph: Shimadzu: LC-10ATvp, SPD-10Avp, SCL-10Avp, DGU-12A
Chromatographic column: (250mm × 4.6mm, 5 μ m) for the chromatographic column that phenyl silane bonded silica gel is filling agent
Mobile phase: sodium heptanesulfonate is to potassium phosphate buffer (pH5.0)-acetonitrile=77:23
Flow velocity: 1.0ml/min
Detect wavelength: 250nm
Column temperature: room temperature
Sampling volume: 10 μ l
The present invention can effectively measure the related substance of ropinirole hydrochloride, method simple and fast, and sensitivity for analysis is high, and result is accurately and reliably.Can be used for the quality control of ropinirole hydrochloride, guarantee the quality controllable of bulk drug and preparation.
Accompanying drawing explanation
Fig. 1 embodiment 1, sodium heptanesulfonate is to potassium phosphate buffer (pH5.0)-acetonitrile (77:23) ropinirole hydrochloride and intermediate biased sample high-efficient liquid phase chromatogram
Fig. 2 embodiment 2, sodium heptanesulfonate is to potassium phosphate buffer (pH5.0)-acetonitrile (77:23) ropinirole hydrochloride high-efficient liquid phase chromatogram
Fig. 3 embodiment 3, sodium heptanesulfonate is to potassium phosphate buffer (pH5.0)-acetonitrile (80:20) ropinirole hydrochloride and intermediate biased sample 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-10ATvp, SPD-10Avp
Chromatographic column: (250mm × 4.6mm, 5 μ m) for the chromatographic column that phenyl silane bonded silica gel is filling agent
Mobile phase: sodium heptanesulfonate potassium phosphate buffer (pH5.0)-acetonitrile (77:23)
Flow velocity: 1.0ml/min
Detect wavelength: 250nm
Column temperature: room temperature
Sampling volume: 10 μ l
Experimental procedure
Take ropinirole hydrochloride 10mg, intermediate compound I, the each 2mg of II, III, be placed in 10ml volumetric flask, adds mobile 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 chromatogram, the results are shown in accompanying drawing 1.
In Fig. 1, retention time is the chromatographic peak that the chromatographic peak of 10.4 minutes is ropinirole hydrochloride, and retention time is 6.9 minutes, 8.3 minutes, 20.6 minutes, is respectively the chromatographic peak of intermediate compound I, II, III.Chromatogram shows that ropinirole hydrochloride can be issued to good separating at same chromatographic condition with its intermediate and impurity.
Instrument and condition
High performance liquid chromatograph: Japanese Shimadzu: LC-10TAvp, SPD-10Avp
Chromatographic column: (250mm × 4.6mm, 5 μ m) for the chromatographic column that phenyl silane bonded silica gel is filling agent
Mobile phase: sodium heptanesulfonate potassium phosphate buffer (pH5.0)-acetonitrile (77:23)
Flow velocity: 1.0ml/min
Detect wavelength: 250nm
Column temperature: room temperature
Sampling volume: 10 μ l
Experimental procedure
Take ropinirole hydrochloride 10mg, be placed in 10ml volumetric flask, add mobile 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 chromatogram, the results are shown in accompanying drawing 2.
Instrument and condition
High performance liquid chromatograph: Japanese Shimadzu: LC-10ATvp, SPD-10Avp
Chromatographic column: (250mm × 4.6mm, 5 μ m) for the chromatographic column that phenyl silane bonded silica gel is filling agent
Mobile phase: sodium heptanesulfonate potassium phosphate buffer (pH5.0)-acetonitrile (80:20)
Flow velocity: 1.0ml/min
Detect wavelength: 250nm
Column temperature: room temperature
Sampling volume: 10 μ l
Experimental procedure
Take ropinirole hydrochloride 10mg, intermediate compound I, the each 2mg of II, III, be placed in 10ml volumetric flask, adds mobile 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 chromatogram, the results are shown in accompanying drawing 3.
Claims (2)
1. the method for a high performance liquid chromatography compartment analysis ropinirole hydrochloride related substance, it is characterized in that adopting phenyl silane bonded silica gel is the chromatographic column of filling agent, model is: 250mm × 4.6mm, 5 μ m, sodium heptanesulfonate potassium phosphate buffer-acetonitrile=77:23 is mobile phase, and described sodium heptanesulfonate potassium phosphate buffer pH is 5.0.
2. method according to claim 1, is characterized in that comprising the following steps:
(1) take ropinirole hydrochloride sample appropriate, use mobile phase dissolution sample, be mixed with the solution of the hydrochloric Ropinirole sample of every 1ml 0.2～2mg;
(2) flow rate of mobile phase being set is 0.8～1.2ml/min, and detection wavelength is 250nm;
(3) get the sample solution 5-40 μ l injection liquid chromatography of step (1), complete the separation and analysis of ropinirole hydrochloride and intermediate thereof.
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| Application Number | Priority Date | Filing Date | Title |
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| CN200910236173.2A CN102043023B (en) | 2009-10-22 | 2009-10-22 | Method for measuring materials associated with Ropinirole hydrochloride by high performance liquid chromatography |
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| CN200910236173.2A CN102043023B (en) | 2009-10-22 | 2009-10-22 | Method for measuring materials associated with Ropinirole hydrochloride by high performance liquid chromatography |
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| CN102043023A CN102043023A (en) | 2011-05-04 |
| CN102043023B true CN102043023B (en) | 2014-05-14 |
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| CN115466209A (en) * | 2022-09-29 | 2022-12-13 | 南通大学 | Synthesis method of ropinirole cyclopentanoindolone impurity |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070254941A1 (en) * | 2006-04-21 | 2007-11-01 | Glenmark Pharmaceuticals Limited | Subtantially pure ropinirole hydrochloride, polymorphic form of ropinirole and process for their preparation |
| CN101393185A (en) * | 2007-09-21 | 2009-03-25 | 北京德众万全药物技术开发有限公司 | Method for analytically separating clopidogrel and enantiomer thereof by HPLC method |
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2009
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070254941A1 (en) * | 2006-04-21 | 2007-11-01 | Glenmark Pharmaceuticals Limited | Subtantially pure ropinirole hydrochloride, polymorphic form of ropinirole and process for their preparation |
| CN101393185A (en) * | 2007-09-21 | 2009-03-25 | 北京德众万全药物技术开发有限公司 | Method for analytically separating clopidogrel and enantiomer thereof by HPLC method |
Non-Patent Citations (7)
| Title |
|---|
| #728 * |
| A. AZEEM 等.Development and validation of a stability-indicating HPLC method for the simultaneous determination of Losartan potassium, hydrochlorothiazide, and their degradation products.《Journal of Pharmaceutical and Biomedical Analysis》.2002,第30卷(第3期),第95-107页. * |
| B. Jancic-Stojanovic 等.Chemometrical evaluation of ropinirole and its impurity’s chromatographic behavior.《Journal of Chromatography A》.2009,第1216卷(第8期),第1263-1269页. |
| Chemometrical evaluation of ropinirole and its impurity’s chromatographic behavior;B. Jancic-Stojanovic 等;《Journal of Chromatography A》;20090220;第1216卷(第8期);第1263页的摘要和1264页的2.1.Chromatographic conditions、2.3.Standard solutions及Table 1 * |
| gmus.Highly sensitive and selective spectrophotometric and spectrofluorimetric methods for the determination of ropinirole hydrochloride in tablets.《Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy》.2008,第70卷(第1期),第69-78页. * |
| Zeynep Aydo˘ |
| Zeynep Aydo& * |
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