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Separation and detection method for roflumilast and intermediate thereof

A technology for roflumilast and intermediates, which is applied in the field of separation and detection of roflumilast and its intermediates, and can solve problems such as difficulty in simultaneous separation and detection

Inactive Publication Date: 2014-03-12
NEW FOUNDER HLDG DEV LLC +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, it is very difficult to separate and detect roflumilast and each intermediate simultaneously under conventional conditions, and so far, there is no literature report that can successfully separate and detect roflumilast and its intermediates. method

Method used

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  • Separation and detection method for roflumilast and intermediate thereof
  • Separation and detection method for roflumilast and intermediate thereof
  • Separation and detection method for roflumilast and intermediate thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] 1) Instruments and conditions

[0059] High-performance liquid chromatography: Shimadzu LC-2010AHT; filler: C18 (150mm×4.6mm, 5μm); mobile phase A: take 1.6g of sodium dihydrogen phosphate and 1.2g of sodium decanesulfonate, add 1000ml of water to dissolve, and use Adjust the pH value to 2.5 with phosphoric acid, mobile phase B: methanol; adopt linear gradient elution method; gradient elution method is as follows:

[0060] time (min)

Mobile phase A%

0

80%

8

40%

25

40%

25.01

80%

40

80%

[0061] The column temperature is 30°C; the flow rate is 1.0ml / min; the detection wavelength is 215nm; the injection volume is 10μl.

[0062] 2) Experimental steps

[0063] Take 25mg each of roflumilast and its intermediates, accurately weigh them, put them in the same 50ml measuring bottle, add methanol to dissolve and dilute to the mark, shake well, and use it as a mixed solution. Carry out...

Embodiment 2

[0065] 1) Instruments and conditions

[0066] High-performance liquid chromatography: Shimadzu LC-2010AHT; filler: C18 (150mm×4.6mm, 5μm); mobile phase A: take 1.6g of potassium dihydrogen phosphate, 2.0g of sodium heptanesulfonate, add 1000ml of water to dissolve, and use Adjust the pH value to 2.0 with phosphoric acid, mobile phase B: methanol; adopt linear gradient elution method; gradient elution method is as follows:

[0067] time (min)

Mobile phase A%

0

80%

8

40%

25

40%

25.01

80%

40

80%

[0068] The column temperature is 35°C; the flow rate is 1.0ml / min; the detection wavelength is 215nm; the injection volume is 10μl.

[0069] 2) Experimental steps

[0070] Take 25mg each of roflumilast and its intermediates, accurately weigh them, put them in the same 50ml measuring bottle, add methanol to dissolve and dilute to the mark, shake well, and use it as a mixed solution. Carry ou...

Embodiment 3

[0072] 1) Instruments and conditions

[0073] High-performance liquid chromatography: Shimadzu LC-2010AHT; filler: C18 (150mm×4.6mm, 5μm); mobile phase A: take 0.8g disodium hydrogen phosphate, 0.2g sodium octane sulfonate, add water 1000ml to dissolve, and use Adjust the pH value to 3.0 with phosphoric acid, mobile phase B: methanol; adopt linear gradient elution method; gradient elution method is as follows:

[0074] time (min)

Mobile phase A%

[0075] 0

60%

8

40%

25

40%

25.01

60%

40

60%

[0076] The column temperature is 25°C; the flow rate is 1.0ml / min; the detection wavelength is 215nm; the injection volume is 10μl.

[0077] 2) Experimental steps

[0078] Take 15mg of roflumilast and its intermediates, weigh them accurately, put them in the same 50ml measuring bottle, add methanol to dissolve and dilute to the mark, shake well, and use it as a mixed solution. Carry ...

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Abstract

The invention relates to a separation and detection method for roflumilast and an intermediate thereof. According to the invention, to realize separation and detection, high performance liquid chromatography and a reversed phase column are adopted, a buffer solution containing ions and having a pH value of 2 to 7.5 on a reagent is used as a mobile phase A, methanol or acetonitrile is used as a mobile phase B, detection wavelength is 215 nm, and a linear gradient elution mode is employed.

Description

technical field [0001] The application relates to the separation and detection method of drugs, in particular to the separation and detection method of roflumilast and its intermediates. Background technique [0002] In July 2010, the European Union approved the marketing of a drug manufactured by Nycomed—roflumilast (Daxas) for the treatment of chronic obstructive pulmonary disease (COPD). Roflumilast is a selective phosphodiesterase 4 (PDE4) inhibitor, which is a new class of drugs approved by the European Union for the treatment of COPD for the first time in more than ten years. [0003] Usually need to go through several key intermediate synthetic steps to chemically synthesize roflumilast. Therefore, various intermediates may remain in roflumilast, which will affect the quality and purity of roflumilast used as a drug. Therefore, it is very necessary to establish a separation and detection method for roflumilast and its intermediates to control their quality and purit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 易崇勤朱丹郑少辉
Owner NEW FOUNDER HLDG DEV LLC
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