A method for the determination of genotoxic impurities in rivaroxaban by high performance liquid chromatography
A technology of high-performance liquid chromatography and rivaroxaban, which is applied in the field of high-performance liquid chromatography for the determination of genotoxic impurities in rivaroxaban, can solve the problems of complex detection methods, inability to effectively detect genotoxic impurities at the same time, and high cost. Achieve the effect of improving detection sensitivity, increasing concentration and injection volume, and good control
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experiment example 1
[0022] Experimental example 1 System suitability test:
[0023] Preparation of each impurity localization solution: Take an appropriate amount of 1-hydroxybenzotriazole, SM2, SM3 and 4,5-dichloro-thiophene-2-carboxylic acid reference substance, add water to dissolve and dilute to prepare each 1mL containing the above A solution of 0.1 mg of impurities is used as an impurity localization solution.
[0024] Preparation of rivaroxaban positioning solution: Weigh an appropriate amount of rivaroxaban, add acetonitrile-water (3:2) to dissolve and dilute to make a solution containing 0.1 mg per 1 mL, as the rivaroxaban positioning solution.
[0025] Preparation of the test solution: Take about 10 mg of rivaroxaban, weigh it accurately, put it in a 10ml measuring bottle, add an appropriate amount of water, sonicate for 10 minutes, dilute with water to the mark, shake well, filter, and take the subsequent filtrate as the test solution .
[0026] Reference substance solution: Accurate...
experiment example 2
[0054] Experimental example 2 linearity and range test
[0055] Preparation of impurity (0.1mg / ml) solution: take the appropriate amount of each impurity (1-hydroxybenzotriazole, SM2, SM3, 4,5-dichloro-thiophene-2-carboxylic acid) under the methodology research item, and prepare respectively into a 0.1mg / ml solution, shake well, and set aside.
[0056] Preparation of linear (5μg / ml) solution: Accurately measure 5ml of each of the above impurity (0.1mg / ml) solutions, put them in the same 100ml measuring bottle, add water to dilute to the mark, and shake well to obtain.
[0057] Preparation of 200% linear solution: Accurately measure 3ml of linear (5μg / ml) solution, put it in a 50ml measuring bottle, add water to dilute to the mark, shake well, and you get it.
[0058] Preparation of 120% linear solution: accurately measure 6ml of 200% linear solution, put it in a 10ml measuring bottle, add water to dilute to the mark, shake well, and you get it.
[0059] Preparation of 100% l...
experiment example 3
[0066] Experimental Example 3 Recovery Test
[0067] Preparation of reference substance stock solution: measure 1-hydroxybenzotriazole (0.1mg / ml) solution, SM2 (0.1mg / ml) solution, SM3 (0.1mg / ml) solution, 4,5-dichloro-thiophene - 1ml each of 2-formic acid solution (0.1mg / ml), put in a 100ml measuring bottle, add water to dilute to the mark, shake well, and obtain.
[0068] Preparation of the reference substance solution: Accurately measure 1.5ml of the reference substance stock solution, put it in a 10ml measuring bottle, add water to dilute to the mark, shake well, and obtain.
[0069] 80%, 100%, 120% reference substance solution: Accurately measure 6ml, 7.5ml, 9ml of the reference substance stock solution respectively, place them in three 50ml measuring bottles, add water to dilute to the mark, shake well, and use as 80%, 100% respectively %, 120% reference substance solution.
[0070] Preparation of the test solution: Weigh about 10 mg of rivaroxaban, weigh 9 parts in pa...
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