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Detection method of substances relative to raw material and preparation of ambrisentan

An ambrisentan and detection method technology, which is applied in the field of drug analysis, can solve problems such as research and elaboration of the detection method of raw materials and preparations without ambrisentan, and research on the detection method of substances, so as to achieve accurate and credible detection results and suitable retention time. , special effect

Active Publication Date: 2015-04-15
TIANJIN INSTITUTE OF PHARMA RESEARCH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The above two patent applications did not research and elaborate on the detection methods of related substances of ambrisentan raw materials and preparations
In addition, in the PCT patent application WO2010 / 091877A2 ("Process For Producing Ambrisentan"), it mainly describes a synthesis process of ambrisentan and the determination of the optical isomerism of ambrisentan, and does not carry out the determination method of related substances. Research

Method used

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  • Detection method of substances relative to raw material and preparation of ambrisentan
  • Detection method of substances relative to raw material and preparation of ambrisentan
  • Detection method of substances relative to raw material and preparation of ambrisentan

Examples

Experimental program
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Effect test

Embodiment 1

[0065] Detection method for related substances of ambrisentan raw material of the present invention

[0066] 1. Testing instruments and testing conditions

[0067] Instrument: Waters e2695; Waters2489 UV detector

[0068] Chromatographic column: C18 column (5μ, 4.6×250mm)

[0069] Mobile phase: A: Acetonitrile: 30mM potassium dihydrogen phosphate (phosphoric acid adjusted to pH 3.5) = 45: 55 (v / v);

[0070] B: Acetonitrile: 30mM potassium dihydrogen phosphate (phosphoric acid adjusted to pH 3.5) = 70:30 (v / v);

[0071] Flow rate: 1ml / min; detection wavelength: 220nm;

[0072] Column temperature: 30°C; automatic sample chamber temperature is 4°C.

[0073] 2. Solution preparation: take the ambrisentan raw material sample, add mobile phase A to dissolve and make the test solution containing about 0.5mg of ambrisentan in every 1ml.

[0074] Precisely measure 1ml of the test solution, put it in a 100ml volumetric flask, dilute to the mark with mobile phase A, shake well, and u...

Embodiment 2

[0084] Detection method for related substances of ambrisentan preparation of the present invention

[0085] 1. Testing instruments and testing conditions

[0086] Instrument: Waters e2695; Waters2489 UV detector

[0087] Chromatographic column: C18 column (5μ, 4.6×250mm)

[0088] Mobile phase: A: Acetonitrile: 30mM potassium dihydrogen phosphate (phosphoric acid adjusted to pH 3.5) = 45: 55 (v / v)

[0089] B: Acetonitrile: 30mM potassium dihydrogen phosphate (phosphoric acid adjusted to pH 3.5) = 70:30 (v / v)

[0090] Flow rate: 1ml / min; detection wavelength: 220nm;

[0091] Column temperature: 30°C; automatic sample chamber temperature is 25°C;

[0092] 2. Solution preparation: take 10 ambrisentan tablets, grind them evenly in a mortar, accurately weigh the tablet powder, put it in a volumetric flask, add mobile phase A for ultrasonic dissolution, dilute to the mark with mobile phase A for cooling, and measure by centrifugation. The supernatant was made into a test solutio...

Embodiment 3

[0100] Detection method for related substances of ambrisentan raw material of the present invention

[0101] 1. Testing instruments and testing conditions

[0102] Instrument: Waters e2695; Waters2489 UV detector

[0103] Chromatographic column: C8 column (5μ, 4.6×250mm)

[0104] Mobile phase: A: Acetonitrile: 30mM potassium dihydrogen phosphate (phosphoric acid adjusted to pH 3.5) = 45: 55 (v / v);

[0105] B: Acetonitrile: 30mM potassium dihydrogen phosphate (phosphoric acid adjusted to pH 3.5) = 70:30 (v / v);

[0106] Flow rate: 1ml / min; detection wavelength: 220nm;

[0107] Column temperature: 30°C; automatic sample chamber temperature is 4°C.

[0108] 2. Solution preparation: take the ambrisentan raw material sample, add mobile phase A to dissolve and make the test solution containing about 0.5mg of ambrisentan in every 1ml.

[0109] Precisely measure 1ml of the test solution, put it in a 100ml volumetric flask, dilute to the mark with mobile phase A, shake well, and us...

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Abstract

The invention provides a detection method of relative substances in raw materials and preparations of ambrisentan. The method is carried out through an HPLC method and includes following steps: (1) preparing a sample solution of the ambrisentan; and (2) feeding the sample solution into an HPLC instrument, performing gradient elution to the sample solution with a mobile phase A and a mobile phase B as a mobile phase and recording a chromatogram, wherein a stationary phase filling agent of a chromatographic column of the HPLC is octadecylsilane chemically bonded silica or octylsilane chemically bonded silica; the mobile phase A is prepared from acetonitrile and a phosphate buffer solution with a volume ratio being 30-50:50-70; and the mobile phase B is prepared from acetonitrile and a phosphate buffer solution with a volume ratio being 50-80:20-50. By means of the detection method, under the same liquid-phase condition, the relative substances in the raw materials or the preparations of the ambrisentan can be measured. The detection method is simple in operation, is high in separation degree, is strong in specificity and is accuracy and reliable in result.

Description

technical field [0001] The invention belongs to the field of drug analysis. Specifically, the present invention relates to a method for detecting related substances of ambrisentan raw materials and preparations by using high performance liquid chromatography. Background technique [0002] Ambrisentan (Letairis) is a selective endothelin receptor A (ETAR) antagonist developed by Gilead Science, USA. Its chemical name is (+)-(2S)-2-[(4,6 -Dimethylpyrimidin-2-yl)oxy]-3-methoxy 3,3-diphenylpropionic acid, English chemical name: (2S)-2-[(4,6-Dimethylpyrimidin-2-yl)oxy ]-3-methoxy-3, 3-diphenylpropanoic acid, the chemical structure is as follows: [0003] [0004] Its molecular weight is 378.42 and its molecular formula is C 22 h 22 N 2 o 4 . [0005] Ambrisentan can potently inhibit the vasoconstriction induced by endostatin. It was approved by the US FDA on June 15, 2007. It is used orally for the treatment of pulmonary hypertension, which can improve exercise capacity...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 王博李洪起连潇嫣任晓文徐为人张海枝
Owner TIANJIN INSTITUTE OF PHARMA RESEARCH
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