A kind of detection method and application of macitentan intermediate

A detection method, the technology of macitentan, applied in the detection of macitentan intermediates and its application field, achieves the effects of fast dissolution, high sensitivity, and simple preparation and operation

Active Publication Date: 2017-03-01
CHENGDU CLIMB PHARMA TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, there is no detection method of any bibliographical information (II) or its salt, therefore, research and development a kind of specificity strong, the detection method of highly sensitive N-propylaminosulfonamide or its salt seems very important

Method used

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  • A kind of detection method and application of macitentan intermediate
  • A kind of detection method and application of macitentan intermediate
  • A kind of detection method and application of macitentan intermediate

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Experimental program
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Effect test

Embodiment 1

[0055] The selection of embodiment 1 chromatographic conditions

[0056] Instruments and conditions: Alltech liquid chromatography system, evaporative light scattering detector (2000ES), chromatographic column: Innoval Silica column (250×4.6mm, 100A, 5μm); column temperature 30°C.

[0057] experiment procedure:

[0058] Preparation of the test solution: take N-propylaminosulfonamide and macitentan, and prepare a solution containing about 50 μg / ml of N-propylaminosulfonamide and about 50.0 mg / ml of macitentan;

[0059]Chromatographic condition 1: Alltech liquid chromatography system, evaporative light scattering detector (2000ES), chromatographic column: InnovalSilica column (250×4.6mm, 100A, 5μm); n-hexane-isopropanol as mobile phase (90:10) ;Drift tube temperature: 35°C.

[0060] Chromatographic condition 2: Alltech liquid chromatography system, evaporative light scattering detector (2000ES), chromatographic column: InnovalSilica column (250 * 4.6mm, 100A, 5 μ m); With n-...

Embodiment 2

[0066] Embodiment 2 limit of quantification and limit of detection

[0067] Detector: Evaporative Light Scattering Detector (ELSD)

[0068] Mobile phase: n-hexane-isopropanol-diethylamine (80:20:0.2)

[0069] Chromatographic column: silica gel

[0070] Flow rate: 0.5ml / min

[0071] Drift tube temperature: 40°C

[0072] Air flow rate: 3.0L

[0073] experiment procedure:

[0074] Accurately weigh an appropriate amount of N-propylaminosulfonamide, add mobile phase to dissolve and carry out gradient dilution, the result:

[0075] When the concentration of the test product solution is 6.042 μg / ml, the signal-to-noise ratio (S / N) in the chromatogram is about 10. After calculation, the quantitative limit of the test product is 54.35 ng;

[0076] When the concentration of the test solution is 2.016 μg / ml, the signal-to-noise ratio (S / N) in the chromatogram is about 3. After calculation, the detection limit of the test is 15.75ng.

Embodiment 3

[0077] Embodiment 3 linearity test

[0078] Detector: Evaporative Light Scattering Detector (ELSD)

[0079] Mobile phase: n-hexane-isopropanol-diethylamine (80:20:0.2)

[0080] Chromatographic column: silica gel

[0081] Flow rate: 0.5ml / min

[0082] Drift tube temperature: 40°C

[0083] Air flow rate: 3.0L

[0084] experiment procedure:

[0085] Weigh N-propylaminosulfonamide and macitentan respectively, prepare the test solution with mobile phase gradient dilution, and measure respectively, take the concentration of the test solution as the abscissa, and the chromatographic peak area as the ordinate to carry out linear regression .

[0086]

[0087]

[0088] figure 1 It is a linear relationship diagram of N-propylaminosulfonamide. As can be seen from the figure, the concentration of N-propylaminosulfonamide solution has a good linear relationship with its corresponding chromatographic peak area, and the correlation coefficient is 0.999, which meets the requir...

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Abstract

The invention provides a detection method for a macitentan intermediate and application thereof. The intermediate is N-propylamino sulfonamide or its salt. The method is characterized in that it employs high performance liquid chromatography to conduct detection, the detector is an evaporative light scattering detector (ELSD), and the mobile phase contains an alkaline additive of certain proportion. The invention also provides application of the detection method. The detection method provided by the invention can fully separate the main component from other materials very well, and can accurately determine the content of impurities. The method has the advantages that: the sample dissolving speed is fast, the same can be completely dissolved within 1min, and the analysis time is generally within 30min; preparation of the mobile phase is simple in operation; the N-propylamino sulfonamide detection limit of the method is 15.75ng, and the sensitivity is high; with the method, the recovery rate of N-propylamino sulfonamide is more than 90%, and the average recovery rate can reach 98.16%, thus meeting the quantitative determination requirements of N-propylamino sulfonamide. In addition, the prepared solution is stable when it is determined within 36h. In summary, the analysis method is stable and reliable, and has high sensitivity.

Description

technical field [0001] This patent relates to a detection method for the intermediate N-propylaminosulfonamide or its salt used in the treatment of pulmonary arterial hypertension, as well as its application in the drug macitentan and its preparations. Background technique [0002] Macitentan (macitentan) is a small molecule, highly effective tissue-targeted endothelin receptor antagonist, which is also highly lipophilic, and has a strong effect on endothelin-1 (ET-1) and its two receptors (ETA, ETB receptor) has dual inhibitory effects and has tissue targeting. The combination of endothelin and its receptor can promote the contraction of vascular smooth muscle, and can also induce the proliferation and fibrosis of vascular smooth muscle cells through tissue mechanisms, causing vascular inflammation and changing tissue structure. Endothelin plays a role in the occurrence and development of many cardiovascular diseases. play an important role. Therefore, as an endothelin re...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88
Inventor 郭瑞李娟王晓玲刘华英
Owner CHENGDU CLIMB PHARMA TECH
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