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A kind of detection method of galanthamine hydrobromide intermediate and impurity

A technology for the detection of galantamine and its detection method, which is applied in the field of detection of galantamine hydrobromide intermediates and impurities, and can solve problems such as inability to accurately integrate and quantify, and inability to verify quantitative limits and detection limits

Active Publication Date: 2022-02-01
安徽美诺华药物化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This property causes in the detection method of other routine impurity, galantamine intermediate I and compound III go out 2 chromatographic peaks in reverse phase chromatography, compound IV goes out 3 chromatographic peaks, and the percentage content of each peak is constant Transformation occurs, cannot be accurately integrated and quantified; and the limit of quantification and detection limit of the above method cannot be verified

Method used

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  • A kind of detection method of galanthamine hydrobromide intermediate and impurity
  • A kind of detection method of galanthamine hydrobromide intermediate and impurity
  • A kind of detection method of galanthamine hydrobromide intermediate and impurity

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Embodiment 1

[0034] This embodiment is a system adaptability test. Before using the HPLC method to test related substances, a system adaptability test must be carried out to confirm that the detection system can meet the detection requirements: generally refers to the separation degree of the main peak and adjacent impurities or a certain degree of separation. The resolution requirements between some adjacent impurities. The detection conditions of this embodiment are:

[0035] Instrument: Agilent 1260 high performance liquid chromatograph and its workstation, UV or DAD detector;

[0036] Chromatographic column: Waters Xbridge C18, 4.6×150mm, 3.5μm;

[0037] Mobile phase A: 0.03mol / L potassium dihydrogen phosphate buffer solution (adjust pH 2.5 with phosphoric acid);

[0038] Mobile phase B: acetonitrile-tetrahydrofuran (90:10, V / V);

[0039] Detection wavelength: 230nm;

[0040] Flow rate: 1.2mL / min;

[0041] Injection volume: 5μL;

[0042] Column temperature: 70°C

[0043] Gradien...

Embodiment 2

[0049] The detection process of the test galantamine hydrobromide intermediate and the detection method of impurity in the test of galantamine intermediate I sample solution is as follows:

[0050] Instrument: Agilent 1260 high performance liquid chromatograph and its workstation, UV or DAD detector;

[0051] Chromatographic column: Waters Xbridge C18, 4.6×150mm, 3.5μm;

[0052] Mobile phase A: 0.03mol / L potassium dihydrogen phosphate buffer solution (adjust pH 2.5 with phosphoric acid);

[0053] Mobile phase B: acetonitrile-tetrahydrofuran (90:10);

[0054] Detection wavelength: 230nm;

[0055] Flow rate: 1.2mL / min;

[0056] Injection volume: 5μL;

[0057] Column temperature: 70°C

[0058] Gradient elution table: see Table 1;

[0059] Diluent: acetonitrile-water (40:60, V / V)

[0060] Take about 25 mg of galantamine intermediate I, put it in a 25 mL volumetric flask, dissolve and dilute to the mark with a diluent, and shake well. Prepare a solution containing galantamine...

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Abstract

The invention relates to a method for detecting galantamine hydrobromide intermediates and impurities. The steps are: preparing the galantamine intermediate to be tested with a diluent to prepare a sample solution, and using octadecyl bonded silica gel as a fixation method. Phase, using inorganic salt buffer solution as mobile phase A, organic solvent as mobile phase B, carry out gradient elution, and record the chromatogram at the absorption wavelength of the galantamine intermediate. In the present invention, octadecyl bonded silica gel is used as the stationary phase, the inorganic salt buffer solution is used as the mobile phase A, and the organic solvent is used as the mobile phase B to carry out gradient elution, and the absorption wavelength of the galantamine intermediate is recorded at a suitable column temperature. The chromatogram can completely separate the galantamine intermediate I and the main impurities, and the peak shape is symmetrical, so that the main substance and each impurity only show one chromatographic peak on the chromatogram, thereby realizing the accurate quantitative detection of each impurity.

Description

technical field [0001] The invention relates to a detection method of a galanthamine hydrobromide intermediate and impurities. Background technique [0002] Galantamine hydrobromide is a reversible inhibitor of acetylcholinesterase activity, similar to neostigmine. It also has intrinsic activity on nicotinic receptors and is mainly used for the symptomatic treatment of mild to moderate to severe dementia in Alzheimer's disease. [0003] Galanthamine hydrobromide chemical name: (4aS,6R,8aS)-3-methoxy-11-methyl-5,6,9,10,11,12-hexahydro-4aH-benzo[2 ,3]benzofuro[4,3-cd]aza-6-hydroxyhydrobromide; CAS number: 1953-04-4; molecular formula is C 17 h 21 NO 3 HBr; the structural formula is as follows: [0004] [0005] Galanthamine hydrobromide intermediate chemical name: 1-bromo-3-methoxy-oxo-5,6,9,10-tetrahydro-4aH-benzo[2,3]benzofuro[ 4,3-cd]aza-11(12H)-carboxamide; CAS No. 122584-14-9; molecular formula C 17 h 16 BrNO 4 ; The structural formula is as follows: [0006]...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 黄勤田艳平三迪普.萨达帕金佳英黄想亮
Owner 安徽美诺华药物化学有限公司
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