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
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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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