A method for content determination and impurity determination of tamibarotene and preparation thereof

Abstract

The invention relates to a medicine analyzing method and particularly relates to a method for measuring impurities in tamibarotene and a preparation thereof by using high performance liquid chromatography. Octadecyl silane bonding silica gel is used as a filling agent, a phosphoric acid buffer solution with a volume ratio of water to phosphoric acid being 2000:1-2000:5 is used as a mobile phase A, acetonitrile is used as a mobile phase B, and a gradient elution process is adopted to establish a sensitive, exclusive and comprehensive tamibarotene impurity detecting and analyzing method. The method can be adopted to effectively detect changes of impurities in production and storage processes of the tamibarotene, and has important practical significance to medicine quality control.

Description

technical field

[0001] The invention relates to a drug analysis method, in particular to a method for determining content and impurities in tamibarotene and its preparations by high performance liquid chromatography. Background technique

[0002] Drug impurity research is one of the main guarantees for controlling drug quality and safety. Because a drug has to go through a relatively complicated and lengthy process from the synthesis of raw materials to the preparation of related preparations, and then through storage, transportation, and use, during which each process may produce related impurities. Into starting materials, reagents, intermediates, by-products and isomers, etc.; special impurities such as degradation products, polymers or crystal transformations may be produced during storage and transportation. Impurities in pharmaceuticals generally refer to process impurities or degradation products produced during the production, storage and transportation of pharmaceu...

Examples

Embodiment 1

[0115] The self-made crude tamibarotene and impurity 1, impurity 2, and impurity 3 were used as samples to be tested.

[0116] Chromatographic conditions: chromatographic column with octadecylsilane bonded silica gel as filler; detection wavelength 240nm; column temperature 30°C; phosphate buffer solution with a volume ratio of water to phosphoric acid of 2000:1 as mobile phase A, and acetonitrile as mobile phase B Phase, where the gradient elution program of mobile phase A and mobile phase B is:

[0117] time (minutes)

Mobile phase A(%)

Mobile phase B(%)

0

70

30

20

55

45

40

30

70

60

30

70

[0118] Sample solution configuration: Take an appropriate amount of crude tamibarotene in a volumetric flask, add acetonitrile-water and phosphoric acid with a volume ratio of 2000:1 phosphate buffer solution (60:40) to dissolve, add mobile phase to dilute to the mark, shake uniform, as the Tamibarotene test ...

Embodiment 2

[0122] The self-made crude tamibarotene and impurity 1, impurity 2, and impurity 3 were used as samples to be tested.

[0123] Chromatographic conditions: chromatographic column with octadecylsilane bonded silica gel as filler; detection wavelength 240nm; column temperature 30°C; phosphate buffer solution with a volume ratio of water to phosphoric acid of 2000:5 as mobile phase A, and acetonitrile as mobile phase B Phase, where the gradient elution program of mobile phase A and mobile phase B is:

[0124] time (minutes)

Mobile phase A(%)

Mobile phase B(%)

0

70

30

20

55

45

40

30

70

60

30

70

[0125] Sample solution configuration: Take an appropriate amount of crude tamibarotene in a volumetric flask, add acetonitrile-water to phosphoric acid with a volume ratio of 2000:5 phosphate buffer solution (60:40) to dissolve, add mobile phase to dilute to the mark, shake uniform, as the Tamibarotene test s...

Embodiment 3

[0129] The self-made crude tamibarotene and impurity 1, impurity 2, and impurity 3 were used as samples to be tested.

[0130] Chromatographic conditions: chromatographic column with octadecylsilane bonded silica gel as filler; detection wavelength 240nm; column temperature 30°C; phosphate buffer solution with a volume ratio of water to phosphoric acid of 2000:3 as mobile phase A, and acetonitrile as mobile phase B Phase, where the gradient elution program of mobile phase A and mobile phase B is:

[0131] time (minutes)

Mobile phase A(%)

Mobile phase B(%)

0

70

30

20

55

45

40

30

70

60

30

70

[0132] Sample solution configuration: Take an appropriate amount of crude tamibarotene in a volumetric flask, add acetonitrile-water and phosphoric acid with a volume ratio of 2000:3 phosphate buffer solution (60:40) to dissolve, add mobile phase to dilute to the mark, shake Evenly, as the test solution of Ta...

technical field

[0001] The invention relates to a drug analysis method, in particular to a method for determining content and impurities in tamibarotene and its preparations by high performance liquid chromatography. Background technique

[0002] Drug impurity research is one of the main guarantees for controlling drug quality and safety. Because a drug has to go through a relatively complicated and lengthy process from the synthesis of raw materials to the preparation of related preparations, and then through storage, transportation, and use, during which each process may produce related impurities. Into starting materials, reagents, intermediates, by-products and isomers, etc.; special impurities such as degradation products, polymers or crystal transformations may be produced during storage and transportation. Impurities in pharmaceuticals generally refer to process impurities or degradation products produced during the production, storage and transportation of pharmaceu...

Examples

Embodiment 1

[0115] The self-made crude tamibarotene and impurity 1, impurity 2, and impurity 3 were used as samples to be tested.

[0116] Chromatographic conditions: chromatographic column with octadecylsilane bonded silica gel as filler; detection wavelength 240nm; column temperature 30°C; phosphate buffer solution with a volume ratio of water to phosphoric acid of 2000:1 as mobile phase A, and acetonitrile as mobile phase B Phase, where the gradient elution program of mobile phase A and mobile phase B is:

[0117] time (minutes)

Mobile phase A(%)

Mobile phase B(%)

0

70

30

20

55

45

40

30

70

60

30

70

[0118] Sample solution configuration: Take an appropriate amount of crude tamibarotene in a volumetric flask, add acetonitrile-water and phosphoric acid with a volume ratio of 2000:1 phosphate buffer solution (60:40) to dissolve, add mobile phase to dilute to the mark, shake uniform, as the Tamibarotene test ...

Embodiment 2

[0122] The self-made crude tamibarotene and impurity 1, impurity 2, and impurity 3 were used as samples to be tested.

[0123] Chromatographic conditions: chromatographic column with octadecylsilane bonded silica gel as filler; detection wavelength 240nm; column temperature 30°C; phosphate buffer solution with a volume ratio of water to phosphoric acid of 2000:5 as mobile phase A, and acetonitrile as mobile phase B Phase, where the gradient elution program of mobile phase A and mobile phase B is:

[0124] time (minutes)

Mobile phase A(%)

Mobile phase B(%)

0

70

30

20

55

45

40

30

70

60

30

70

[0125] Sample solution configuration: Take an appropriate amount of crude tamibarotene in a volumetric flask, add acetonitrile-water to phosphoric acid with a volume ratio of 2000:5 phosphate buffer solution (60:40) to dissolve, add mobile phase to dilute to the mark, shake uniform, as the Tamibarotene test s...

Embodiment 3

[0129] The self-made crude tamibarotene and impurity 1, impurity 2, and impurity 3 were used as samples to be tested.

[0130] Chromatographic conditions: chromatographic column with octadecylsilane bonded silica gel as filler; detection wavelength 240nm; column temperature 30°C; phosphate buffer solution with a volume ratio of water to phosphoric acid of 2000:3 as mobile phase A, and acetonitrile as mobile phase B Phase, where the gradient elution program of mobile phase A and mobile phase B is:

[0131] time (minutes)

Mobile phase A(%)

Mobile phase B(%)

0

70

30

20

55

45

40

30

70

60

30

70

[0132] Sample solution configuration: Take an appropriate amount of crude tamibarotene in a volumetric flask, add acetonitrile-water and phosphoric acid with a volume ratio of 2000:3 phosphate buffer solution (60:40) to dissolve, add mobile phase to dilute to the mark, shake Evenly, as the test solution of Ta...

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