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Detection method and application of enantiomers in ivabradine hydrochloride intermediate

A technology for ivabradine hydrochloride and enantiomers is applied in the field of detection of enantiomers in ivabradine hydrochloride intermediates, and achieves the effects of strong practicability, symmetrical peak shape and good detection effect

Active Publication Date: 2022-04-26
HAINAN XINOPEN SOURCE MEDICAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But the existing chiral effective control method and detection only for ivabradine hydrochloride finished product, patent CN102478560A a kind of content detection method of ivabradine hydrochloride optical isomers mentions adopting OD-RH (chiralcel, 150mm * 4.6mm , 5μm) chiral column, mobile phase (n-hexane-absolute ethanol-triethylamine=85:15:0.5), column temperature 35°C, flow rate 1.0ml / min, detection wavelength 287nm, also only for ivabre hydrochloride Customized products for testing

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  • Detection method and application of enantiomers in ivabradine hydrochloride intermediate
  • Detection method and application of enantiomers in ivabradine hydrochloride intermediate
  • Detection method and application of enantiomers in ivabradine hydrochloride intermediate

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Embodiment 1

[0045] Embodiment 1-In order to carry out quality control to the key intermediate of ivabradine hydrochloride, and continuously improve the safety and effectiveness of ivabradine hydrochloride medicines, the present invention proposes a kind of ivabradine hydrochloride intermediate enantiomer The detection method of isomers, the intermediate of ivabradine hydrochloride is 3-[3-[[[(7S)-3,4-dimethoxybicyclo[4.2.0]octane-1,3,5-tri En-7-yl]methyl]methylamino]propyl]-1,3-dihydro-2H-benzazepin-2-one, whose enantiomer is 3-[3-[[[ (7R)-3,4-Dimethoxybicyclo[4.2.0]oct-1,3,5-trien-7-yl]methyl]methylamino]propyl]-1,3-dihydro -2H-benzazepin-2-one, its detection method is:

[0046] Prepare the sample solution to be tested respectively: the reference substance solution of the enantiomer, the test solution of the ivabradine hydrochloride intermediate and the mixed solution of the ivabradine hydrochloride intermediate and the enantiomer, inject the high-efficiency chromatographic The determi...

Embodiment 2

[0047] The detection method of enantiomer in embodiment 2-a kind of ivabradine hydrochloride intermediate, comprises the steps:

[0048] (1) Prepare the sample solution to be tested:

[0049] S1. Preparation of 3-[3-[[[(7S)-3,4-dimethoxybicyclo[4.2.0]oct-1,3,5-trien-7-yl]methyl]methylamino ]Propyl]-1,3-dihydro-2H-benzazepin-2-one for the test solution:

[0050] Take ivabradine hydrochloride intermediate sample and mobile phase and mix and be mixed with need testing solution, stand-by, according to mass volume ratio (g / L), ivabradine hydrochloride intermediate sample: the ratio of mobile phase is ( 0.1~5):1.

[0051] S2. Preparation of 3-[3-[[[(7R)-3,4-dimethoxybicyclo[4.2.0]oct-1,3,5-trien-7-yl]methyl]methylamino ]Propyl]-1,3-dihydro-2H-benzazepin-2-one reference substance stock solution:

[0052] Take by weighing enantiomers and add in volumetric flask, mix with mobile phase and prepare reference substance stock solution, stand-by, according to mass volume ratio (g / L), en...

Embodiment 3

[0070] Select 3-[3-[[[(7S)-3,4-dimethoxybicyclo[4.2.0]oct-1,3,5-trien-7-yl]methyl] with batch number 191104 Methylamino] propyl] -1,3-dihydro-2H-benzazepin-2-one content is detected, comprising the following steps:

[0071] S1, prepare the test solution of ivabradine hydrochloride intermediate:

[0072] Take by weighing 10mg ivabradine hydrochloride intermediate sample and add 10mL mobile phase, after mixing uniformly, be mixed with the solution that every 1mL contains ivabradine hydrochloride intermediate 1.0mg, as need testing solution, stand-by.

[0073] S2, prepare the reference substance stock solution of enantiomer:

[0074] Weigh an appropriate amount of the reference substance of the enantiomer, weigh it precisely, dissolve it in the mobile phase and quantitatively dilute it to make a solution containing about 10 μg per 1 mL, as the stock solution of the reference substance of the enantiomer, and stand-by.

[0075] S3, prepare the reference substance solution of enan...

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Abstract

The invention provides a detection method and application of enantiomers in an ivabradine hydrochloride intermediate, the detection method comprising: respectively preparing sample solutions to be tested, injecting them into a high-performance liquid chromatograph, and measuring conditions: the chromatographic column is CHIRALPAK IC column, column temperature 25~40℃, detection wavelength 280~290nm; mobile phase is a mixture of n-hexane, dichloromethane and diethylamine with a volume ratio of (76~80):(20~24):0.5 , the flow rate of the mobile phase is 0.8~1.2mL / min; the present invention can accurately quantitatively analyze the enantiomers in the intermediate of ivabradine hydrochloride, the peak shape is symmetrical, there is no tailing phenomenon, and the separation degree and quantitative limit The detection limit, repeatability, precision, and solution stability all meet the relevant requirements, and the detection limit can reach 0.0337 μg / mL, and more than 0.01% of the enantiomers in the ivabradine hydrochloride intermediate can be detected.

Description

technical field [0001] The invention relates to the technical field of medicinal chemistry, in particular to a detection method and application of an enantiomer in an ivabradine hydrochloride intermediate. Background technique [0002] Ivabradine hydrochloride (Ivabradine hydrochloride), the chemical name is 3-[3-[[[(7S)-3,4-dimethoxybicyclo[4.2.0]octa-1,3,5-triene -7-yl]methyl]-methylamino]propyl]-7,8-dimethoxy-1,3,4,5-tetrahydro-2H-3-benzazepine-2-one Hydrochloride. Ivabradine hydrochloride, its hydrochloride salt, has very valuable pharmacological and therapeutic properties, especially heart rate-lowering properties, and can be used to treat or prevent various clinical manifestations of myocardial ischemia, such as angina pectoris, myocardial infarction and related Rhythm disorders, and many diseases involving rhythm disorders, especially supraventricular arrhythmias, and can be used for systolic heart failure and diastolic heart failure. The chemical structural formul...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/86
CPCG01N30/02G01N30/06G01N30/8679G01N2030/047
Inventor 夏中宁白秉信王仕伟
Owner HAINAN XINOPEN SOURCE MEDICAL TECH CO LTD
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