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

A high-performance liquid chromatography, istradefylline technology, applied in the direction of analysis of materials, material separation, measurement devices, etc., can solve the problem of no relevant literature reports on the analysis method, and achieve great positive progress and practical application value, method strong specific effect

Active Publication Date: 2018-01-30
HEFEI JIUNUO MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] At present, there is no relevant literature report on the analysis method of istradefylline raw material and its preparation based on comprehensive impurity profile analysis

Method used

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Detection equipment and chromatographic conditions:

[0041] High performance liquid chromatography: Agilent PUMP, Agilent DAD detector

[0042]Chromatographic column: Diamonsil C18 chromatographic column (250 × 4.6mm, 5 μ m); Mobile phase: acetonitrile-0.05mol / L phosphate buffer (potassium hydroxide adjusts the pH value to 6.1) with a volume ratio of 50:50; detection wavelength: 230nm; flow rate: 1.0ml / min; injection volume: 20μl.

[0043] Experimental steps:

[0044] (1) Sample preparation:

[0045] Take an appropriate amount of istradefylline and known impurities A-H, and use acetonitrile-phosphate buffer solution with a volume ratio of 1:1 (take 6.8 g of potassium dihydrogen phosphate, add 1000 ml of water to dissolve, adjust the pH value to 6.1 with potassium hydroxide) Ultrasonic dissolved and diluted to make a solution containing about 0.5 mg / ml of istradefylline and about 5 μg / ml of impurities A-H as the sample solution.

[0046] (2) Detection: Take the abov...

Embodiment 2

[0049] Detection equipment and chromatographic conditions:

[0050] High performance liquid chromatography: Agilent PUMP, Agilent DAD detector

[0051] Chromatographic column: Diamonsil C18 chromatographic column (250×4.6 mm, 5 μm); mobile phase: same as in Example 1; detection wavelength: 230 nm; flow rate: 1.0 ml / min.

[0052] (1) Sample preparation:

[0053] Acid destruction: take istradefylline tablets, grind finely, take an appropriate amount of fine powder (approximately equivalent to 10mg containing istradefylline), put it in a 20ml brown measuring bottle, add 2ml of 1mol / L hydrochloric acid solution, and put it in a water bath at 60°C for 2 hours , take it out, let it cool, add 2ml of 1mol / L sodium hydroxide solution, use acetonitrile-phosphate buffer solution with a volume ratio of 1:1 (take 6.8g of potassium dihydrogen phosphate, add 1000ml of water to dissolve, adjust the pH value with potassium hydroxide to 6.1) Dissolve and dilute to the mark, shake well, filter...

Embodiment 3

[0062] Detection equipment and chromatographic conditions:

[0063] High performance liquid chromatography: Agilent PUMP, Agilent DAD detector

[0064] Chromatographic column: Diamonsil C18 chromatographic column (250 × 4.6mm, 5 μ m); Mobile phase: acetonitrile-0.05mol / L phosphate buffer (potassium hydroxide adjusts the pH value to 6.1) with a volume ratio of 50:50; detection wavelength: 230nm; flow rate: 1.0ml / min; injection volume: 20μl.

[0065] Experimental steps:

[0066] (1) Sample preparation: Take an appropriate amount of istradefylline, dissolve and dilute it with acetonitrile-0.05mol / L phosphate buffer (adjust the pH value to 6.1 with potassium hydroxide) at a volume ratio of 1:1 to make about 0.5 mg solution, shake well, as the sample solution.

[0067] (2) Detection: Take the above sample solution, inject 20 μl of it, and record the chromatogram.

[0068] For a typical chromatogram see Figure 8 .

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Abstract

The invention discloses a high-performance liquid chromatography analytical method for istradefylline related substances. A reversed phase chromatographic column and an ultraviolet detector are adopted for isocratic elution with acetonitrile-phosphate buffer as a mobile phase. All known impurities in raw materials and preparations of istradefylline can be analyzed simultaneously, contents of the known impurities can be effectively controlled by a main component self contrast method with correction factors, a degree of separation between each impurity peak and a main peak is larger than 1.5, and purity of each impurity peak and the main peak is 1.0. The high-performance liquid chromatography analytical method for the istradefylline related substances is a high-specificity simple analytical method for quality control analysis of the raw materials and the preparations of the istradefylline.

Description

1. Technical field [0001] The invention relates to a method for analyzing the purity of chemical drugs, in particular to a high-performance liquid chromatography analysis method for related substances of istradefylline. 2. Background technology [0002] Itradefylline, the chemical name is (E)-8-(3,4-dimethoxystyryl)-1,3-diethyl-7-methyl-3,7-dihydro -1H-purine-2,6-dione, the chemical structure is as follows: [0003] [0004] Itradefylline is a selective adenosine A2A receptor antagonist developed by Kyowa Hakko Kirin in Japan. Itraphylline Tablets (trade name Nouriast, specification 20mg) was approved for marketing by PMDA in Japan in March 2013. It is clinically used to treat Parkinson's disease and improve the dyskinesia in the early stage of Parkinson's syndrome. End-of-dose phenomenon due to treatment. [0005] There are many impurities in istradefylline. From a structural point of view, the impurities are mainly related to the structural change of the substituted ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/027
Inventor 吴标崔红晓施伶俐王娟
Owner HEFEI JIUNUO MEDICAL TECH
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