CN101769904A - Method utilizing HPLC (high performance liquid chromatography) to measure oxalate escitalopram optical isomer - Google Patents
Method utilizing HPLC (high performance liquid chromatography) to measure oxalate escitalopram optical isomer Download PDFInfo
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- CN101769904A CN101769904A CN200810246555A CN200810246555A CN101769904A CN 101769904 A CN101769904 A CN 101769904A CN 200810246555 A CN200810246555 A CN 200810246555A CN 200810246555 A CN200810246555 A CN 200810246555A CN 101769904 A CN101769904 A CN 101769904A
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Abstract
The invention discloses a method utilizing HPLC (high performance liquid chromatography) to measure an oxalate escitalopram optical isomer. Vancomycin silane bonding silica gel is selected as a chromatographic column of padding. A mixed solvent of methanol, absolute ethyl alcohol, triethylamine and glacial acetic acid is adopted as a flowing phase. The method in the invention can be used for carrying out quality control on the oxalate escitalopram optical isomer.
Description
Technical field:
The present invention relates to a kind of high performance liquid chromatogram method, particularly a kind of high-performance liquid chromatogram determination method of oxalic acid escitalopram optical isomer.
Background technology:
The oxalic acid escitalopram is antidepressants, and molecular formula is C
20H
21FN
2OC
2H
2O
4, chemistry S-(+) by name-1-(3-dimethylamino-propyl)-1-(4-fluorophenyl)-1,3-dihydroisobenzofuran-5-formonitrile HCN oxalates, its structural formula is as follows:
It is the chromatographic column of filler that this law adopts vancomycin silane group silica gel, realized the mensuration of oxalic acid escitalopram optical isomer fast and accurately, thereby realized the control of oxalic acid escitalopram optical isomer, guarantee the quality controllable of oxalic acid escitalopram, had realistic meaning.
Summary of the invention:
The object of the present invention is to provide a kind of method, can be used for the quality control of oxalic acid escitalopram with high efficiency liquid chromatography for separating and determining oxalic acid escitalopram optical isomer.
The invention provides a kind of method with high-performance liquid chromatogram determination oxalic acid escitalopram optical isomer, selecting vancomycin silane group silica gel for use is the chromatographic column of filler, with the mixed solvent of methyl alcohol, absolute ethyl alcohol, triethylamine and glacial acetic acid as moving phase.
The invention provides a kind of method with high-performance liquid chromatogram determination oxalic acid escitalopram optical isomer, the methyl alcohol in the moving phase and the ratio of absolute ethyl alcohol are 1: 1～4.
The invention provides a kind of method with high-performance liquid chromatogram determination oxalic acid escitalopram optical isomer, the methyl alcohol in the moving phase and the ratio of absolute ethyl alcohol are 1: 1.
The invention provides a kind of method with high-performance liquid chromatogram determination oxalic acid escitalopram optical isomer, the methyl alcohol in the moving phase and the ratio of triethylamine are 30～70: 0.05～0.2.
The invention provides a kind of method with high-performance liquid chromatogram determination oxalic acid escitalopram optical isomer, the methyl alcohol in the moving phase and the ratio of triethylamine are 50: 0.5.
The invention provides a kind of method with high-performance liquid chromatogram determination oxalic acid escitalopram optical isomer, the triethylamine in the moving phase and the ratio of glacial acetic acid are 1: 1～3.
The invention provides a kind of method with high-performance liquid chromatogram determination oxalic acid escitalopram optical isomer, the triethylamine in the moving phase and the ratio of glacial acetic acid are 1: 1.
The invention provides a kind of method, can realize by the following method with high-performance liquid chromatogram determination oxalic acid escitalopram optical isomer:
1) it is an amount of to get the oxalic acid escitalopram, with the moving phase dissolving, is mixed with the sample solution that every 1ml contains felodipine 0.5mg, as need testing solution; Precision is measured need testing solution 1ml, puts in the 100ml measuring bottle, is diluted to scale with moving phase, shakes up, in contrast solution;
2) it is an amount of to get raceme, makes the solution that contains 0.1mg among every 1ml with moving phase dissolving and dilution, as the raceme sample solution.
3) selecting vancomycin silane group silica gel for use is the chromatographic column of filler; It is 0.5～1.0ml/min that flow rate of mobile phase is set, and the flow velocity of moving phase is preferably 0.6ml/min; Detect wavelength 210～260nm, the optimum detection wavelength is 238nm.
4) get 1) and 2) solution 10～50 μ l, preferred 10 μ l inject high performance liquid chromatograph, finish the mensuration of oxalic acid escitalopram optical isomer.
The present invention can effectively measure the optical isomer of oxalic acid escitalopram, the method simple and fast, and the sensitivity for analysis height, the result is accurately and reliably.Can be used for the quality control of oxalic acid escitalopram.
Description of drawings
The liquid chromatogram of Fig. 1 oxalic acid escitalopram
The high-efficient liquid phase chromatogram of Fig. 2 oxalic acid escitalopram raceme
The high-efficient liquid phase chromatogram of Fig. 3 oxalic acid escitalopram and raceme compound sample
Embodiment:
Following examples are used for further understanding the present invention, but are not limited to the scope of this enforcement.
Instrument and condition
Day island proper Tianjin LC-10ATVP pump, Tianjin, island SPD-10AVP ultraviolet-visible light multiwavelength detector, RHEODYNE 7725i injector and TL9900 chromatographic data workstation, chromatographic column: AstecCHIROBIOTIV
TMV, SUPELCO, 250 * 4.6mm, 5 μ m, ultraviolet detection wavelength: 238nm, moving phase: methyl alcohol-absolute ethyl alcohol-triethylamine-glacial acetic acid (50: 50: 0.1: 0.1).
Experimental procedure
It is an amount of to get oxalic acid escitalopram and raceme, makes certain density solution with the moving phase dissolving, carries out high-efficient liquid phase analysis by above-mentioned condition, and the record chromatogram the results are shown in Figure 1.
Retention time is that 31.750 minutes chromatographic peak is the chromatographic peak of oxalic acid escitalopram among Fig. 1, and retention time is that 29.667 chromatographic peak is the chromatographic peak of oxalic acid escitalopram raceme.The chromatographic peak degree of separation of oxalic acid escitalopram and raceme thereof is good under these conditions, can satisfy the requirement of Chinese Pharmacopoeia.
Claims (8)
1. method with high-performance liquid chromatogram determination oxalic acid escitalopram optical isomer, it is characterized in that selecting for use vancomycin silane group silica gel is the chromatographic column of filler, with the mixed solvent of methyl alcohol, absolute ethyl alcohol, triethylamine and glacial acetic acid as moving phase.
2. according to the described method of claim r, it is characterized in that the methyl alcohol in the moving phase and the ratio of absolute ethyl alcohol are 1: 1～4.
3. method according to claim 2 is characterized in that the methyl alcohol in the moving phase and the ratio of absolute ethyl alcohol are 1: 1.
4. method according to claim 1 is characterized in that the methyl alcohol in the moving phase and the ratio of triethylamine are 30～70: 0.05～0.2.
5. method according to claim 4 is characterized in that the methyl alcohol in the moving phase and the ratio of triethylamine are 50: 0.5.
6. method according to claim 1 is characterized in that the triethylamine in the moving phase and the ratio of glacial acetic acid are 1: 1～3.
7. method according to claim 6 is characterized in that the triethylamine in the moving phase and the ratio of glacial acetic acid are 1: 1.
8. according to each described method of claim 1～7, it is characterized in that: it is an amount of to get the oxalic acid escitalopram, with the moving phase dissolving, is mixed with the sample solution that every 1ml contains felodipine 0.5mg, as need testing solution; Precision is measured need testing solution 1ml, puts in the 100ml measuring bottle, is diluted to scale with moving phase, shakes up, in contrast solution; It is an amount of to get raceme, makes the solution that contains 0.1mg among every 1ml with moving phase dissolving and dilution, as the raceme sample solution; Detect wavelength 238nm, selecting vancomycin silane group silica gel for use is the chromatographic column of filler, and flow velocity is 0.6ml/min, gets each 10 μ l of need testing solution, contrast solution and raceme solution, inject high performance liquid chromatograph, finish the mensuration of oxalic acid escitalopram optical isomer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810246555A CN101769904A (en) | 2008-12-29 | 2008-12-29 | Method utilizing HPLC (high performance liquid chromatography) to measure oxalate escitalopram optical isomer |
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| CN200810246555A CN101769904A (en) | 2008-12-29 | 2008-12-29 | Method utilizing HPLC (high performance liquid chromatography) to measure oxalate escitalopram optical isomer |
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| CN101769904A true CN101769904A (en) | 2010-07-07 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106018618A (en) * | 2016-07-05 | 2016-10-12 | 湖南洞庭药业股份有限公司 | Escitalopram oxalate tablet composition and quality control method |
| CN106226427A (en) * | 2016-07-18 | 2016-12-14 | 江苏德源药业股份有限公司 | A kind of supercritical fluid chromatography quickly splits the method for aranidipine racemic modification |
| CN106324141A (en) * | 2016-08-30 | 2017-01-11 | 山东京卫制药有限公司 | HPLC (high-performance liquid chromatography) detection method for escitalopram oxalate related substances |
| CN106568863A (en) * | 2016-11-04 | 2017-04-19 | 北京万全德众医药生物技术有限公司 | Method for separating and determining escitalopram oxalate intermediate and optical isomer thereof by using high-performance liquid chromatography |
-
2008
- 2008-12-29 CN CN200810246555A patent/CN101769904A/en active Pending
Non-Patent Citations (3)
| Title |
|---|
| A. MØRK，ET AL: "The R-enantiomer of citalopram counteracts escitalopram-induced increase in extracellular 5-HT in the frontal cortex of freely moving rats", 《NEUROPHARMACOLOGY》 * |
| 杨雪梅等: "HPLC测定S-西酞普兰", 《第一军医大学学报》 * |
| 潘红娟等: "氢溴酸西酞普兰的手性拆分及草酸依地普仑ee值检查", 《中国医药工业杂志》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106018618A (en) * | 2016-07-05 | 2016-10-12 | 湖南洞庭药业股份有限公司 | Escitalopram oxalate tablet composition and quality control method |
| CN106018618B (en) * | 2016-07-05 | 2018-06-22 | 湖南洞庭药业股份有限公司 | Escitalopram oxalate tablet composition and quality control method |
| CN106226427A (en) * | 2016-07-18 | 2016-12-14 | 江苏德源药业股份有限公司 | A kind of supercritical fluid chromatography quickly splits the method for aranidipine racemic modification |
| CN106324141A (en) * | 2016-08-30 | 2017-01-11 | 山东京卫制药有限公司 | HPLC (high-performance liquid chromatography) detection method for escitalopram oxalate related substances |
| CN106324141B (en) * | 2016-08-30 | 2019-06-25 | 山东京卫制药有限公司 | A kind of efficient liquid phase detection method of the escitalopram oxalate in relation to substance |
| CN106568863A (en) * | 2016-11-04 | 2017-04-19 | 北京万全德众医药生物技术有限公司 | Method for separating and determining escitalopram oxalate intermediate and optical isomer thereof by using high-performance liquid chromatography |
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Application publication date: 20100707 |