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Method for splitting amlodipine antimer by high-performance liquid chromatography

A technology of high-performance liquid chromatography and amlodipine, which is applied in the field of enantiomer resolution and detection, can solve the problems of cumbersome resolution methods, large amount of resolution solvents, and solvent residues, etc., and achieve increased diversity and high separation efficiency , good selective effect

Inactive Publication Date: 2016-10-26
颜海
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In recent years, a lot of methods about amlodipine enantiomer resolution have been disclosed. There are crystal resolution methods using various solvents as resolving agents, but they have the disadvantages of using a large amount of resolution solvent, high cost, and tedious resolution methods. , low yield and easy to have solvent residues and other shortcomings; also use high performance capillary electrophoresis to split amlodipine enantiomers
At present, there is no report on the separation of amlodipine enantiomers by high-performance liquid chromatography. Therefore, the present invention uses high-performance liquid chromatography to resolve amlodipine enantiomers, and establishes a high-efficiency separation method. A new method with good selectivity, high detection sensitivity, automatic operation and wide application range is used to separate the amlodipine enantiomers by high performance capillary electrophoresis, which is useful for the two enantiomers of amlodipine in medicine and Clinical application is of great significance

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 1. Setting of chromatographic conditions

[0025] UV detection wavelength: 230nm; detection temperature: 20°C; flow rate of mobile phase: 0.5mL / min.

[0026] 2. Drug pretreatment

[0027] a. Sample: prepare amlodipine enantiomer sample with distilled water, the concentration of sample is 1.15x10 -4 mol / L, and filtered through a 0.22 μL microporous membrane for later use.

[0028] b. Mobile phase: Prepare potassium dihydrogen phosphate with a concentration of 3 mmol / L and a pH of 2.3, and the volume ratio with methanol and isopropanol is 65:25:10, and use a 0.22 μm organic filter membrane for pumping After filtering, degassing treatment with ultrasonic wave for 5min, set aside.

[0029] 3. Injection split

[0030] Using normal phase mobile phase system and C 18 Chromatographic column, with sulfobutyl ether-β-cyclodextrin as the stationary phase, run the high-performance liquid chromatograph according to the chromatographic conditions set above, when the baseline is ...

Embodiment 2

[0032] 1. Setting of chromatographic conditions

[0033] UV detection wavelength: 234nm; detection temperature: 22°C; flow rate of mobile phase: 0.6mL / min.

[0034] 2. Drug pretreatment

[0035] a. Sample: prepare amlodipine enantiomer sample with distilled water, the concentration of sample is 1.15x10 -4 mol / L, and filtered through a 0.22 μL microporous membrane for later use.

[0036] b. Mobile phase: Prepare potassium dihydrogen phosphate with a concentration of 4mmol / L and a pH of 2.4, and the volume ratio with methanol and isopropanol is 65:25:10, and use a 0.22μm organic filter membrane for pumping After filtering, degassing treatment with ultrasonic wave for 5min, set aside.

[0037] 3. Injection split

[0038] Using normal phase mobile phase system and C 18 Chromatographic column, with sulfobutyl ether-β-cyclodextrin as the stationary phase, run the high-performance liquid chromatograph according to the chromatographic conditions set above, when the baseline is st...

Embodiment 3

[0040] 1. Setting of chromatographic conditions

[0041] UV detection wavelength: 237nm; detection temperature: 23°C; flow rate of mobile phase: 0.7mL / min.

[0042] 2. Drug pretreatment

[0043] a. Sample: prepare amlodipine enantiomer sample with distilled water, the concentration of sample is 1.15x10 -4 mol / L, and filtered through a 0.22 μL microporous membrane for later use.

[0044] b. Mobile phase: Prepare potassium dihydrogen phosphate with a concentration of 5 mmol / L and a pH of 2.5, and the volume ratio with methanol and isopropanol is 65:25:10, and use a 0.22 μm organic filter membrane for pumping After filtering, degassing treatment with ultrasonic wave for 5min, set aside.

[0045] 3. Injection split

[0046] Using normal phase mobile phase system and C 18 The chromatographic column uses carboxymethyl-β-cyclodextrin as the stationary phase, and operates the high-performance liquid chromatograph according to the chromatographic conditions set above. When the bas...

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PUM

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Abstract

The invention belongs to the technical field of detection and splitting and in particular discloses a method for splitting an amlodipine antimer by high-performance liquid chromatography. According to the method, a normal-phase mobile phase system and a C18 chromatographic column are adopted, and the amlodipine antimer is split by taking a cyclodextrin derivative as an immobile phase and potassium dihydrogen phosphate, methanol and iso-propanol as a mobile phase under certain ultraviolet detection wavelength, detection temperature and flow speed of the mobile phase. The method disclosed by the invention has the advantages of high separation efficiency, good selectivity, high detection sensitivity, automation in operation and wide application range, and can be used for splitting the amlodipine antimer very well; diversification of amlodipine antimer splitting methods is increased.

Description

【Technical field】 [0001] The invention relates to the technical field of enantiomer resolution and detection, in particular to a method for resolving enantiomers of amlodipine. 【Background technique】 [0002] Levoamlodipine is a long-acting calcium ion antagonist, clinically used to treat various types of hypertension and angina, especially spontaneous angina, and has very important uses in the field of cardiovascular and cerebrovascular. Compared with common calcium antagonists, it has the advantages of not affecting the myocardial contraction rate, not causing reflex tachycardia, and having low incidence of side effects. [0003] Compared with levamlodipine, although its dextrorotatory form lacks calcium channel blocking activity, it is a potent inhibitor of smooth muscle cell migration and can be used in the treatment of atherosclerosis, restenosis after angioplasty and endometriosis bit. [0004] Since the two isomers of amlodipine have good pharmacological activities,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/74G01N30/06
CPCG01N30/74G01N30/06
Inventor 颜海
Owner 颜海