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Candesartan ester of related substances
source:Vitalpharms Company Ltd.    Release date:2017-12-6 10:18:25

Take about 20 mg, candesartan ester in 50 ml volumetric flask and add acetonitrile - water (3:2) dissolve and diluted to scale, shake well, as the test solution; Precision measuring 1 ml, 100 ml volumetric flask, using acetonitrile and water (3:2) diluted to scale, shake well, as the reference solution. As high performance liquid chromatography (2 2010 edition pharmacopoeia appendix Ⅴ D) determination, using octadecyl silane bonded silica as filler (recommended Ecosil C18 column C18 column or Kromasil100-5, 4.6 mm * 250 mm, 5 microns or efficiency of chromatographic column); With acetonitrile - glacial acetic acid and water (57:1:43) as the mobile phase A, acetonitrile - glacial acetic acid and water (90:1) as mobile phase B, detection wavelength of 254 nm. A linear gradient elution according to the table below. Take 20 ml of test sample solution, add 0.1 mol/L HCL solution 1.0 ml, 90 ℃ water bath heating after 10 minutes, add the 1.0 ml and 0.1 mol/L sodium hydroxide solution, as the system suitability solution, system suitability solution 10 mu L injection liquid chromatograph, record chromatograph chart, candesartan ester peak retention time is about 20 minutes, (+) - 1 - [[(cyclohexanol oxygen generation) carbonyl oxygen generation) ethyl - 2 - oxygen generation - 3 - [(2 '- (1 h - four nitrogen imidazolyl - 5 - base) al phenyl methyl - 4 - base]] - 2, 3-2 h - 1 h - benzene and imidazole - 4 - carboxylic acid ester Ⅰ (impurities) of the relative retention time of about 0.6; theoretical plate number by candesartan ester peaks is not less than 12000, trailing factor shall not be over 1.5. Precision measuring each 10 mu L solution and reference solution into the liquid chromatograph, record chromatograph chart, in the chromatogram of test sample solution, if there is any impurity peak Ⅰ impurity peak area shall not be greater than 0.3 times as much land as main reference solution (0.3%), and other individual impurity peak area shall not be greater than 0.2 times as much land as main reference solution (0.2%), and shall not be greater than the reference solution of each impurity peak area of the main peak area 0.6 times (0.6%). Any less than the reference solution in the chromatograph chart of test sample solution main area is 0.05 times the peak can be neglected.

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