CN101718751B - Method for determining desven lafaxine related matters by utilizing high-efficiency liquid-phase chromatography - Google Patents
Method for determining desven lafaxine related matters by utilizing high-efficiency liquid-phase chromatography Download PDFInfo
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- CN101718751B CN101718751B CN 200810224007 CN200810224007A CN101718751B CN 101718751 B CN101718751 B CN 101718751B CN 200810224007 CN200810224007 CN 200810224007 CN 200810224007 A CN200810224007 A CN 200810224007A CN 101718751 B CN101718751 B CN 101718751B
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- desmethylvenlafaxine
- desven
- lafaxine
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Abstract
The invention discloses a determining method for separation and analysis of desven lafaxine related matters. Cyano silicane-bonded silica gel is used as a chromatographic column (250*4.6 mm, 5 micrometers) of a filling agent. An organic modifying agent containing a surface active agent and a buffer salt is used as a flowing phase, and then the desven lafaxine related matters are separated and analyzed under the same chromatogram condition.
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 desmethylvenlafaxine related substance.
Background technology
Desmethylvenlafaxine is the active metabolite of Venlafaxine, is a kind of weak inhibitor of dopamine, can suppress the picked-up again of serotonin and norepinephrine effectively, and absorbing again of dopamine had certain inhibiting effect.Be mainly used in treating PD (MDD).Its structural formula is:
Molecular formula is: C
16H
25NO
2, molecular weight: 263.4
It is bigger that desmethylvenlafaxine and its intermediate are compared the polarity difference, under same chromatographic condition, do not use gradient elution and realize that their separation has certain difficulty, therefore, realize that desmethylvenlafaxine is having important practical significance aspect the quality control of the synthetic and preparation process of desmethylvenlafaxine with its intermediate separating with analysis under same chromatographic condition.
Summary of the invention
The object of the present invention is to provide a kind of under same chromatographic condition the efficient liquid-phase chromatography method of compartment analysis desmethylvenlafaxine related substance, thereby realize quality control to desmethylvenlafaxine.
The applicant finds, be the chromatographic column of filling agent with cyano group silane group silica gel, be the phase that flows with the buffer salt-organic modifiers that contains surfactant, desmethylvenlafaxine and its intermediate separating and analysis under same chromatographic condition can be realized, thereby the quality of desmethylvenlafaxine and preparation thereof can be accurately controlled.
The said method with high performance liquid chromatography compartment analysis desmethylvenlafaxine of the present invention, selecting cyano group silane group silica gel for use is the chromatographic column of filling agent, is the phase that flows with phosphate sodium dihydrogen buffer solution-acetonitrile, wherein contains a spot of surfactant.
The chromatographic column that the present invention adopts is that cyano group silane group silica gel is the chromatographic column (250mm * 4.6mm, 5 μ m) of filling agent.
The organic modifiers that the present invention adopts is selected from acetonitrile, methyl alcohol, and most preferred organic modifiers is acetonitrile.
The inventive method flow mutually, the volume ratio of phosphate sodium dihydrogen buffer solution-organic modifiers mixed solution is 80:20～95:5.
The inventive method flow mutually in the surfactant that comprises be selected from sodium pentanesulfonate, sodium heptanesulfonate, most preferred is sodium heptanesulfonate, surfactant concentrations is 0.002mol/L～0.007mol/L.
Method for separating and analyzing of the present invention, can realize in accordance with the following methods:
(1) it is an amount of to take by weighing the desmethylvenlafaxine sample, with the phased soln sample that flows, is mixed with the sample solution that every 1ml contains desmethylvenlafaxine 0.2mg～2mg approximately.
(2) flow rate of mobile phase being set is 0.8～1.2ml/min, and the detection wavelength is 226nm+3nm.
(3) the sample solution 5-40 μ l that gets step (1) injects liquid chromatograph, finishes separation and the analysis of desmethylvenlafaxine.
Wherein:
High performance liquid chromatograph: Tianjin, island: LC-10ATvp, SPD-10Avp, SCL-10Avp, DGU-12A
Chromatographic column: cyano group silane group silica gel is the chromatographic column (250mm * 4.6mm, 5 μ m) of filling agent
Phase flows: phosphate sodium dihydrogen buffer solution (contain the 0.005mol/L sodium heptanesulfonate, regulating the pH value with phosphoric acid,diluted is 2.6)-acetonitrile=90:10
Flow velocity: 1.0ml/min
Detect wavelength: 226nm
Column temperature: room temperature
Sampling volume: 20 μ l
It is the chromatographic column (250mm * 4.6mm, 5 μ m) of filling agent, effectively compartment analysis desmethylvenlafaxine related substance that the present invention adopts cyano group silane group silica gel; Select the phased soln sample that flows, can eliminate the interference of solvent to detecting; Select sampling volume 20 μ l, column temperature is room temperature, adds the symmetry that surfactant has improved chromatographic peak.The invention solves and under same chromatographic condition, do not use gradient elution and energy simple separation and the problem of analyzing the desmethylvenlafaxine related substance, thereby guaranteed the quality controllable of desmethylvenlafaxine bulk drug and preparation.
Description of drawings
Fig. 1 embodiment 1, phosphate sodium dihydrogen buffer solution-acetonitrile (90:10) also adds desmethylvenlafaxine and the intermediate biased sample high-efficient liquid phase chromatogram of sodium heptanesulfonate
Fig. 2 embodiment 2, phosphate sodium dihydrogen buffer solution-acetonitrile (90:10) also adds the desmethylvenlafaxine high-efficient liquid phase chromatogram of sodium heptanesulfonate
Fig. 3 embodiment 3, phosphate sodium dihydrogen buffer solution-acetonitrile (95:5) also adds desmethylvenlafaxine and the intermediate biased sample high-efficient liquid phase chromatogram of sodium heptanesulfonate
Embodiment:
Following examples are used for further understanding the present invention, but are not limited to the scope of this enforcement.
Embodiment 1
Instrument and condition
High performance liquid chromatograph: day island proper Tianjin: LC-10ATvp, SPD-10Avp
Chromatographic column: cyano group silane group silica gel is the chromatographic column (250mm * 4.6mm, 5 μ m) of filling agent
Phase flows: phosphate sodium dihydrogen buffer solution (contain the 0.005mol/L sodium heptanesulfonate, the pH value is 2.6)-acetonitrile (90:10)
Flow velocity: 1.0ml/min
Detect wavelength: 226nm
Column temperature: room temperature
Sampling volume: 20 μ l
Experimental procedure
Take by weighing desmethylvenlafaxine 50mg, intermediate compound I, impurity I, each 10mg of impurity II place the 50mL volumetric flask, add to flow phased soln and be diluted to scale, shake up, as need testing solution.Get need testing solution, carry out efficient liquid phase chromatographic analysis under above-mentioned chromatographic condition, the record chromatogram the results are shown in accompanying drawing 1.
Retention time is that 9.5 minutes chromatographic peak is the chromatographic peak of desmethylvenlafaxine among Fig. 1.Retention time is that 17.0 minutes chromatographic peak is the chromatographic peak of intermediate compound I, and retention time is the chromatographic peak that the chromatographic peak of 33.4 minutes and 14.7 minutes is respectively impurity I, impurity II.Chromatogram shows that desmethylvenlafaxine can be issued to good separating at same chromatographic condition with its intermediate and impurity.
Instrument and condition
High performance liquid chromatograph: day island proper Tianjin: LC-10TAvp, SPD-10Avp
Chromatographic column: cyano group silane group silica gel is the chromatographic column (250mm * 4.6mm, 5 μ m) of filling agent
Phase flows: phosphate sodium dihydrogen buffer solution (contain the 0.005mol/L sodium heptanesulfonate, the pH value is 2.6)-acetonitrile (90:10)
Flow velocity: 1.0ml/min
Detect wavelength: 226nm
Column temperature: room temperature
Sampling volume: 20 μ l
Experimental procedure
Take by weighing desmethylvenlafaxine 50mg, place the 50mL volumetric flask, add and flow phased soln and be diluted to scale, shake up, as need testing solution.Get need testing solution, carry out efficient liquid phase chromatographic analysis under above-mentioned chromatographic condition, the record chromatogram the results are shown in accompanying drawing 2.
Embodiment 3
Instrument and condition
High performance liquid chromatograph: day island proper Tianjin: LC-10ATvp, SPD-10Avp
Chromatographic column: cyano group silane group silica gel is the chromatographic column (250mm * 4.6mm, 5 μ m) of filling agent
Phase flows: phosphate sodium dihydrogen buffer solution (contain the 0.005mol/L sodium heptanesulfonate, the pH value is 2.6)-acetonitrile (95:5)
Flow velocity: 1.0ml/min
Detect wavelength: 226nm
Column temperature: room temperature
Sampling volume: 20 μ l
Experimental procedure
Take by weighing desmethylvenlafaxine 50mg, intermediate compound I, impurity I, each 10mg of impurity II place the 50mL volumetric flask, add to flow phased soln and be diluted to scale, shake up, as need testing solution.Get need testing solution, carry out efficient liquid phase chromatographic analysis under above-mentioned chromatographic condition, the record chromatogram the results are shown in accompanying drawing 3.
Claims (1)
1. the method for a high performance liquid chromatography compartment analysis desmethylvenlafaxine related substance is characterized in that step is as follows:
(1) it is an amount of to take by weighing the desmethylvenlafaxine sample, with the phased soln sample that flows, is mixed with the sample solution that every 1ml contains desmethylvenlafaxine 0.2mg～2mg;
(2) flow rate of mobile phase being set is 1.0ml/min, and the detection wavelength is 226nm;
(3) the sample solution 20 μ l that get step (1) inject liquid chromatograph,
Wherein:
High performance liquid chromatograph: Tianjin, island: LC-10ATvp, SPD-10Avp, SCL-10Avp, DGU-12A
Chromatographic column: cyano group silane group silica gel is the chromatographic column of filling agent, 250mm * 4.6mm, 5 μ m
Phase flows: phosphate sodium dihydrogen buffer solution-acetonitrile=90: 10, and wherein phosphate sodium dihydrogen buffer solution contains the 0.005mol/L sodium heptanesulfonate, and regulating the pH value with phosphoric acid,diluted is 2.6
Column temperature: room temperature.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200810224007 CN101718751B (en) | 2008-10-09 | 2008-10-09 | Method for determining desven lafaxine related matters by utilizing high-efficiency liquid-phase chromatography |
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|---|---|---|---|
| CN 200810224007 CN101718751B (en) | 2008-10-09 | 2008-10-09 | Method for determining desven lafaxine related matters by utilizing high-efficiency liquid-phase chromatography |
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|---|---|
| CN101718751A CN101718751A (en) | 2010-06-02 |
| CN101718751B true CN101718751B (en) | 2013-09-18 |
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| CN 200810224007 Expired - Fee Related CN101718751B (en) | 2008-10-09 | 2008-10-09 | Method for determining desven lafaxine related matters by utilizing high-efficiency liquid-phase chromatography |
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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108982714A (en) * | 2018-06-06 | 2018-12-11 | 上海市精神卫生中心（上海市心理咨询培训中心） | A kind of method that simple and effective detects human plasma Venlafaxine and its active metabolite O-Goven Wenfasin concentration |
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2008
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Non-Patent Citations (6)
| Title |
|---|
| Analysis of the second generation antidepressant venlafaxine and its main active metabolite O-desmethylvenlafaxine in human plasma by HPLC with spectrofluorimetric detection;Roberto Mandrioli etal;《Journal of Chromatography B》;20071231;第856卷;88页2.1至90页2.3 * |
| Bhavin N. Patel etal.Liquid chromatography tandem mass spectrometry assay for the simultaneous determination of venlafaxine and O-desmethylvenlafaxine in human plasma and its application to a bioequivalence study.《Journal of Pharmaceutical and Biomedical Analysis》.2008,第47卷603-611. |
| Liquid chromatography tandem mass spectrometry assay for the simultaneous determination of venlafaxine and O-desmethylvenlafaxine in human plasma and its application to a bioequivalence study;Bhavin N. Patel etal;《Journal of Pharmaceutical and Biomedical Analysis》;20080226;第47卷;604页2.1至604页2.3 * |
| Roberto Mandrioli etal.Analysis of the second generation antidepressant venlafaxine and its main active metabolite O-desmethylvenlafaxine in human plasma by HPLC with spectrofluorimetric detection.《Journal of Chromatography B》.2007,第856卷88-94. |
| 张素霞 等.高效液相色谱法测定饲料中莱克多巴胺.《中国饲料》.2005,(第10期),33-35. |
| 高效液相色谱法测定饲料中莱克多巴胺;张素霞 等;《中国饲料》;20051231(第10期);34页2.1至34页2.4 * |
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