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Method for measuring substances related to formoterol intermediate by separation of liquid chromatography

A technology of related substances and determination methods, which is applied in the field of detection of related substances of formoterol intermediates, can solve problems such as incomplete removal of impurities and influence on drug purity and quality, and achieve quality controllable results

Active Publication Date: 2015-05-27
BEIJING VENTUREPHARM BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Impurities in formoterol intermediates are not completely removed, and will be introduced into the final product of the raw material drug, thereby affecting the purity and quality of the drug

Method used

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  • Method for measuring substances related to formoterol intermediate by separation of liquid chromatography
  • Method for measuring substances related to formoterol intermediate by separation of liquid chromatography
  • Method for measuring substances related to formoterol intermediate by separation of liquid chromatography

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Instruments and Conditions

[0040] High performance liquid chromatography: Shimadzu: LC-20AT, CBM-20A, SIL-20AC, SPD-M20A, CTO-10ASvp;

[0041] Column: C 8 (Apollo, 250×4.6 mm, 5 μm);

[0042] Mobile phase: 20 mmol / L disodium hydrogen phosphate (pH 3.0)-acetonitrile (55:45)

[0043] Flow rate: 1.0 mL / min

[0044] Detection wavelength: 215 nm

[0045] Injection volume: 10 μL.

[0046] Experimental procedure

[0047] Take an appropriate amount of formoterol intermediate and its related substances, dissolve the samples in mobile phase respectively, and prepare a sample solution containing about 0.5 mg / mL of formoterol intermediate and its related substances. Perform HPLC analysis according to the above conditions, and record the chromatograms. see attached results Figure 1~2 , figure 1 The chromatographic peak whose retention time is 15.090 min is the formoterol intermediate, and the remaining chromatographic peaks are the chromatographic peaks of the related s...

Embodiment 2

[0049] Instruments and Conditions

[0050] High performance liquid chromatography: Shimadzu: LC-20AT, CBM-20A, SIL-20AC, SPD-M20A, CTO-10ASvp;

[0051] Column: C 8 (Apollo, 250×4.6 mm, 5 μm);

[0052] Mobile phase: 20 mmol / L potassium dihydrogen phosphate (pH 6.0)-acetonitrile (30:70)

[0053] Flow rate: 1.0 mL / min

[0054] Detection wavelength: 215 nm

[0055] Injection volume: 10 μL.

[0056] Experimental procedure

[0057] Take an appropriate amount of formoterol intermediate and its related substances, dissolve the samples in mobile phase respectively, and prepare a sample solution containing about 0.5 mg / mL of formoterol intermediate and its related substances. Perform HPLC analysis according to the above conditions, and record the chromatograms. see attached results Figure 3~4 , image 3 The chromatographic peak whose retention time is 10.323 min is the formoterol intermediate, and the remaining chromatographic peaks are the chromatographic peaks of the related...

Embodiment 3

[0059] Instruments and Conditions

[0060] High performance liquid chromatography: Shimadzu: LC-20AT, CBM-20A, SIL-20AC, SPD-M20A, CTO-10ASvp;

[0061]Chromatographic column: Phenyl (Kromasil, 250×4.6 mm, 5 μm);

[0062] Mobile phase: A: 20 mmol / L potassium dihydrogen phosphate (pH 6.0)

[0063] B: Acetonitrile

[0064] Flow rate: 1.0 mL / min

[0065] Detection wavelength: 215 nm

[0066] Injection volume: 10 μL

[0067] Elution gradient:

[0068] time (min) mobile phase A mobile phase B 0 48 52 27 48 52 30 42 58 65 42 58 80 30 70 81 48 52 95 48 52

[0069] The following items of the analytical method for the above-mentioned formoterol intermediate and its related substances were verified:

[0070] 1. System suitability test

[0071] Under the chromatographic conditions determined above, an appropriate amount of formoterol intermediate and its related substances was taken, and the samples were respectively disso...

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Abstract

The invention belongs to the field of analytical chemistry, and discloses a method for measuring the chemical purities of substances related to formoterol intermediate (R)-1-(3-amino-4-(benzyloxy) phenyl)-2-(benzyl (R)-1-(4-methoxyphenyl) propan-2-yl) amino) ethanol by separation of liquid chromatography. According to the method, phenyl silane bonded silica gel is taken as a chromatographic column of filler and a buffer salt solution-organic phase with a certain proportion is taken as a mobile phase, and the contents of the formoterol intermediate and the substances related to the formoterol intermediate can be measured, so that the mass of the formoterol intermediate can be effectively controlled, and the mass of the final product of formoterol is controllable. The method is high in specificity, high in accuracy and simple and convenient to operate.

Description

technical field [0001] The invention belongs to the technical field of drug analysis, and in particular relates to a quality control method for formoterol, in particular to a detection method for related substances of a formoterol intermediate. Background technique [0002] Formoterol is a long-acting β2-adrenoceptor agonist used for long-term maintenance treatment of bronchoconstriction caused by chronic obstructive pulmonary disease (COPD), including chronic bronchitis and emphysema. The chemical name of formoterol intermediate is (R)-1-(3-amino-4-(benzyloxy)phenyl)-2-(benzyl(R)-1-(4-methoxyphenyl)propan-2-yl)amino )ethanol, the molecular formula is C 32 h 36 N 2 o 3 . The structural formula of formoterol intermediate is: [0003] [0004] In the process of synthesizing this compound, there are several important intermediates that may affect the purity and quality of the formoterol bulk drug due to incomplete removal. There are 5 related substances that are mainly...

Claims

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Application Information

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IPC IPC(8): G01N30/89
Inventor 谭丽媛王宇杰马苏峰
Owner BEIJING VENTUREPHARM BIOTECH
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