UPLC (ultra-high performance liquid chromatography) method for simultaneously determining six related substances in bicalutamide

A technology for bicalutamide and related substances, which is applied in the detection field of chemical drug related substances, can solve problems such as less bicalutamide, and achieve the effects of ensuring safe medication, high sensitivity and shortening analysis time.

Inactive Publication Date: 2015-09-09
CHONGQING MEDICAL & PHARMA COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are few domestic studies on bicalutamide, mainly on the research reports on the content determination of bicalutamide by HPLC method, and fewer reports on related substances of bicalutamide. There is only one article on the synthesis and Research reports on characterization and physical and chemical properties, no reports on the determination of other related substances in bicalutamide

Method used

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  • UPLC (ultra-high performance liquid chromatography) method for simultaneously determining six related substances in bicalutamide
  • UPLC (ultra-high performance liquid chromatography) method for simultaneously determining six related substances in bicalutamide
  • UPLC (ultra-high performance liquid chromatography) method for simultaneously determining six related substances in bicalutamide

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] The determination of 6 kinds of related substances in the bicalutamide crude drug of embodiment 1

[0016] 1 Instruments and reagents

[0017] Waters ACQUITY ultra-high performance liquid chromatography, the reagents used are chromatographically pure, and the water is ultrapure water. Three batches of bicalutamide API, each batch 46g; bicalutamide reference substance 200mg; 4-amino-2-(trifluoromethyl)benzonitrile reference substance 20mg; impurity A reference substance 20mg; Reference substance 20mg; 2-fluoroisomer reference substance 20mg; dehydroxy homologue reference substance 20mg; bicalutamide sulfide reference substance 20mg.

[0018] 2 Methods and results

[0019] 2.1 Chromatographic conditions and system suitability

[0020] Column: ACQUITY UPLC BEH C 18 (1.7 μ m, 2.1 * 50mm); Mobile phase A is the aqueous solution of 0.01% (v / v) trifluoroacetic acid, and mobile phase B is the acetonitrile solution of 0.01% (v / v) trifluoroacetic acid, carries out gradient wa...

Embodiment 2

[0040] Determination of 6 kinds of related substances in embodiment 2 bicalutamide tablets

[0041] 2.7 Sample Determination

[0042] Take three batches of 20 bicalutamide tablets (specification: 50mg / tablet) with known content, weigh them accurately, grind them finely in a mortar, weigh an appropriate amount, add a diluent and ultrasonically dissolve them for 30 minutes, and quantitatively dilute them to make each 1mL Contain about 1 mg of the solution in the solution, shake well, filter with a microporous membrane (0.22 μm), and take the subsequent filtrate to obtain the test solution. Take an appropriate amount of bicalutamide reference substance, accurately weigh it, dissolve it with a diluent and quantitatively dilute it to make a solution containing about 1 μg per 1 mL, as the reference substance solution. Precisely measure 1.5 μL of the reference substance solution and inject it into the liquid chromatograph, adjust the detection sensitivity so that the peak height of ...

Embodiment 3

[0046] Determination of 6 kinds of related substances in embodiment 3 bicalutamide capsules

[0047] 2.7 Sample Determination

[0048] Take the contents of 20 bicalutamide capsules (specification: 50mg / capsule) of three batches of known content respectively, weigh them accurately, take an appropriate amount, add diluent and ultrasonically dissolve them for 30min, and quantitatively dilute them to make about Containing 1 mg of the solution, shake well, filter through a microporous membrane (0.22 μm), and take the subsequent filtrate to obtain the test solution. Take an appropriate amount of bicalutamide reference substance, accurately weigh it, dissolve it with a diluent and quantitatively dilute it to make a solution containing about 1 μg per 1 mL, as the reference substance solution. Precisely measure 1.5 μL of the reference substance solution and inject it into the liquid chromatograph, adjust the detection sensitivity so that the peak height of the main component chromatog...

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Abstract

The invention relates to a UPLC (ultra-high performance liquid chromatography) method for simultaneously determining six related substances in bicalutamide. The method includes the steps of firstly, preparing sample solution; secondly, preparing control solution; thirdly, performing UPLC determination, to be more specific, performing determination analysis on the control solution and the sample solution under the chromatographic conditions, wherein the chromatographic conditions include that a chromatographic column is ACQUITY UPLC BEH C18 (1.7 micrometers, 2.1mm*50mm), the flow phase A is 0.01% (v / v) trifluoroacetic acid aqueous solution, the flow phase B is 0.01% (v / v) trifluoroacetic acid acetonitrile solution, gradient elution is performed, flow speed is 0.5ml.min<-1>, column temperature is 25 DEG C, and detecting wavelength is 270 nanometers. The method has the advantages that under the conditions of the method, the bicalutamide and the six related substances are effectively separated, and methodology results conform to analyzing and determination requirements; the impurities and degradation products of the bicalutamide can be detected fast and accurately, and the method is simple to operate, good in reproducibility, high in flexibility and capable of well controlling bicalutamide product quality.

Description

technical field [0001] The invention relates to the detection of related substances of chemical drugs, in particular to a UPLC method for simultaneously determining six related substances in bicalutamide. Background technique [0002] Bicalutamide (BCT) is a new type of non-steroidal anti-androgen drug developed by AstraZeneca in the UK. It was approved for marketing in the UK in 1995 and was approved for import in my country in 1999. Its chemical name is N-[4- Cyano-3-(trifluoromethyl)phenyl]-3-[(4-fluorophenyl)sulfonyl]-2-hydroxy-2-methylpropionamide, the trade name is Casodex. Bicalutamide can block the action of androgen produced by the adrenal gland, inhibit the binding or absorption of androgen at the nuclear receptor site, and cause the shrinkage of prostate tumors. It is clinically used to treat advanced prostate cancer. During the production and storage of bicalutamide, a series of degradation products and related impurities will be produced. The United States Pharm...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 杨林何丹
Owner CHONGQING MEDICAL & PHARMA COLLEGE
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