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A kind of high performance liquid chromatography analysis method of macitentan related substances

A technology of high performance liquid chromatography and macitentan, which is applied in the direction of analyzing materials, material separation, measuring devices, etc., can solve the problems that there are no relevant literature reports on the analysis methods of macitentan raw materials and their preparations, and achieve specificity strong effect

Active Publication Date: 2017-03-08
合肥启旸生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] At present, there is no relevant literature report on the analysis method of macitentan raw material and its preparation

Method used

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  • A kind of high performance liquid chromatography analysis method of macitentan related substances
  • A kind of high performance liquid chromatography analysis method of macitentan related substances
  • A kind of high performance liquid chromatography analysis method of macitentan related substances

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Testing equipment and chromatographic conditions:

[0047] High performance liquid chromatograph: LC-10AD pump, SPD-M10A detector

[0048] Column: Agilent C18 (250×4.6mm, 5μm); mobile phase A: acetonitrile-water-formic acid solution with a volume ratio of 49:51:0.1; mobile phase B: acetonitrile-water with a volume ratio of 85:15:0.1 -Formic acid solution; detection wavelength: 260nm; flow rate: 1.0ml / min; injection volume: 20μl.

[0049] Experimental steps:

[0050] (1) Sample preparation:

[0051] Take an appropriate amount of macitentan and known impurity AR, and use a volume ratio of 1:4 ammonium bicarbonate buffer (take 1.58g of ammonium bicarbonate, add 1000ml of water to dissolve, adjust the pH to 9.0 with ammonia)-acetonitrile solution ultrasound Dissolve and dilute to prepare a solution containing about 1mg / ml of macitentan and about 1μg / ml of impurity AR, as a sample solution;

[0052] (2) Gradient elution program setting:

[0053] Time (minutes) Mobile phase A (%) ...

Embodiment 2

[0057] Testing equipment and chromatographic conditions:

[0058] High performance liquid chromatograph: LC-10AD pump, SPD-M10A detector

[0059] Chromatographic column: Agilent C18 (250×4.6mm, 5μm); mobile phase A: same as Example 1, mobile phase B: same as Example 1; flow rate: 1.0 ml / min; detection wavelength: 260 nm; injection volume: 20 μl.

[0060] (1) Sample preparation:

[0061] Acid destruction: take macitentan tablets, grind finely, take an appropriate amount of fine powder (about 50mg containing macitentan), take 50mg of macitentan raw material, put it in a 50ml measuring flask, and add 5ml of 1mol / L hydrochloric acid solution Put it in a water bath at 80℃ for 1 hour, quickly cool it, add 5ml of 1mol / L sodium hydroxide solution to neutralize, and use a volume ratio of 1:4 ammonium bicarbonate buffer (take 1.58g of ammonium bicarbonate, add 1000ml of water to dissolve, use ammonia Adjust the pH to 9.0)-Dissolve and dilute the acetonitrile solution to the mark, shake well, f...

Embodiment 3

[0071] Testing equipment and chromatographic conditions:

[0072] High performance liquid chromatograph: SSI Series 1500 pump, Series 1500 PDA detector

[0073] Chromatographic column: Agilent C18 (250×4.6mm, 5μm); mobile phase A: same as Example 1, mobile phase B: same as Example 1; flow rate: 1.0 ml / min; detection wavelength: 260 nm; injection volume: 20 μl.

[0074] Experimental steps:

[0075] (1) Sample preparation: Take an appropriate amount of macitentan, use 1:4 ammonium bicarbonate buffer (take 1.58g of ammonium bicarbonate, add 1000ml of water to dissolve, adjust the pH to 9.0 with ammonia)-acetonitrile solution ultrasonic Dissolve and dilute to make a solution containing 1 mg / ml of macitentan as a sample solution.

[0076] (2) Gradient elution program setting:

[0077] Time (minutes) Mobile phase A (%) Mobile phase B (%) 01000 101000 350100 400100 421000 501000

[0078] (3) Detection: Take each of the above-mentioned sample solutions, inject 20μl respectively, and record ...

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Abstract

The invention discloses a high performance liquid chromatography method of macitentan related substances. The method adopts a reversed phase chromatographic column and an ultraviolet detector, and adopts acetonitrile-water-formic acid as a mobile phase to carry out gradient elution. The method can be used to simultaneously analyze all known impurities in a macitentan raw material and preparations thereof, and also allows the content of the known impurities to be effectively controlled through a correction factor-containing main component self-contrasted technology, the resolution among all impurity peaks and the resolution between a main peak and an adjacent impurity peak are respectively greater than 1.5, and the peak purities of the main peak and all the impurity peaks are 1.0. The method is a simple and reliable analysis method for quality control of the macitentan raw material and the preparations thereof.

Description

[0001] 1. Technical Field [0002] The invention relates to a method for analyzing the purity of chemical drugs, in particular to a method for analyzing related substances of macitentan by high performance liquid chromatography. [0003] 2. Background technology [0004] Macitentan, the chemical name is N-[5-(4-bromophenyl)-6-[2-[(5-bromo-2-pyrimidinyl)oxy]ethoxy]-4-pyrimidine Group]-N'-propylsulfonamide, the chemical structural formula is as follows: formula (I): [0005] [0006] Macitentan is a bidirectional endothelin receptor antagonist, developed by Actelion Pharmaceuticals Inc. of Switzerland. It was approved by the US FDA on October 18, 2013 for the treatment of pulmonary arterial hypertension (PAH) to delay disease progression. [0007] There are many impurities in macitentan. From the structural point of view, the core of 5-(4-bromophenyl)-4,6-disubstituted pyrimidine and the structure of diethoxy have two reactive sites (chlorine Atom, hydroxyl), double condensation impurit...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88G01N30/34G01N30/89
CPCG01N30/34G01N30/88G01N30/89G01N2030/027G01N2030/8872
Inventor 吴标李晓梅王娟施伶俐
Owner 合肥启旸生物科技有限公司
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