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Detection method for tetraacetylribose in azacitidine raw material

A detection method, the technology of azacitidine, which is applied in the detection field of impurities, can solve the problems such as unusable detection and inability to detect tetraacetyl ribose, and achieve good peak shape symmetry, simple and easy operation, and high detection efficiency Effect

Inactive Publication Date: 2015-01-21
SICHUAN HUIYU PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method cannot be used to detect tetraacetyl ribose in azacitidine. Even if the maximum absorption wavelength of tetraacetyl ribose is 210nm as the detection wavelength, other conditions remain unchanged, and tetraacetyl ribose in azacitidine cannot be detected.

Method used

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  • Detection method for tetraacetylribose in azacitidine raw material
  • Detection method for tetraacetylribose in azacitidine raw material
  • Detection method for tetraacetylribose in azacitidine raw material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] A detection method for tetraacetyl ribose in azacitidine raw material, adopts high performance liquid chromatography, selects Agilent zorbax SB-C18 chromatographic column, the particle size of the filler is 5 μm, and the specification is 150mm×4.6mm. The volume percentage of water and methanol is 70%: 30% for isocratic elution, the flow rate is 1.0mL / min, the column temperature is 25°C, measure 50μL, 5mg / mL azacitidine aqueous solution for detection, and the detection wavelength It is 210nm, and the elution time is 20min. Test results such as figure 1 shown. Tetraacetylribose impurity peak retention time (R = 10.510min), and adjacent peaks are well separated (resolution R = 4.54), the number of peak theoretical plates is high (N = 9662), and the peak shape has good symmetry (Symm=0.96). It shows that the method has high accuracy and high sensitivity, and can accurately detect the content of the tetraacetyl ribose impurity in the azacitidine raw material.

Embodiment 2

[0029] A detection method for tetraacetylribose in azacitidine raw material, using high performance liquid chromatography, using Agilent XDB-C 18 For the chromatographic column, the particle size of the filler is 5 μm, and the specification is 150mm×4.6mm. The volume percentage of water and methanol is 65%: 35% for isocratic elution, the flow rate is 1.2mL / min, the column temperature is 30°C, and 50μL of 0.5mg / mL azacitidine aqueous solution is measured for detection. The wavelength is 210nm, and the elution time is 20min. Test results: Tetraacetylribose impurity peak retention time (R=8.286min), adjacent peaks are well separated, peak theoretical plate number is high (N=9671), peak shape symmetry is good (Symm=0.98 ). It shows that the method has high accuracy and high sensitivity, and can accurately detect the content of the tetraacetyl ribose impurity in the azacitidine raw material.

Embodiment 3

[0031] A detection method for tetraacetylribose in azacitidine raw materials, using high performance liquid chromatography, using Agilent zorbax SB-C18 chromatographic column, the particle size of the filler is 5 μm, and the specification is 150mm×4.6mm. The volume percentage of water and methanol is 55%: 45% for isocratic elution, the flow rate is 0.8mL / min, the column temperature is 35°C, and 50μL of 10mg / mL azacitidine aqueous solution is used for detection. The detection wavelength It is 215nm, and the elution time is 20min. Test results such as figure 2 shown. Tetraacetylribose impurity peak retention time (R=4.540min), and adjacent peaks are well separated, the peak theoretical plate number is high (N=6417), and the peak shape symmetry is good (Symm=0.96). It shows that the method has high accuracy and high sensitivity, and can accurately detect the content of the tetraacetyl ribose impurity in the azacitidine raw material.

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Abstract

The invention discloses an impurity detection method, in particular to a detection method for tetraacetylribose in azacitidine. The method adopts high performance liquid chromatography, a octadecyl silane bonded silica gel chromatographic column is selected, and water-methanol is employed as the mobile phase to conduct isocratic elution, the flow rate is 0.8-1.2mL / min, the column temperature is 25-35DEG C, and the detection wavelength of the sample is 205nm-215nm. The mobile phase is employed to perform isocratic elution, wherein the volume percentage of methanol is 30-45%. The detection method has the advantages of high sensitivity, high accuracy, good impurity peak shape symmetry, and high column efficiency, etc.

Description

technical field [0001] The invention relates to a method for detecting impurities, in particular to a method for detecting tetraacetyl ribose in azacitidine. Background technique [0002] Azacitidine, English name Azacitidine, chemical name 1-(β-D-ribofuranosyl)-4-amino-1,3,5-triazin-2(1H)-one, also known as 5-aza Cytidine, its structural formula is as follows: [0003] [0004] Azacitidine is a cytidine drug. It can be directly incorporated into DNA, inhibit DNA and RNA synthesis, and can kill cells in S phase. The U.S. FDA first approved Celgene corp to market the drug in May 2004. The trade name is: Vidaza, which is mainly used for the treatment of myelodysplastic syndrome and acute non-lymphocytic leukemia. [0005] Tetraacetyl ribose is one of the commonly used raw materials for the synthesis of azacitidine, and tetraacetyl ribose impurities may exist in the synthesized azacitidine. Impurity detection is one of the important indicators to control the quality of m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 张光宪丁兆孙朝国胡刚
Owner SICHUAN HUIYU PHARMA
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