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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. Looked at the above introduction, believe that everyone has to candesartan ester of related substances have a certain understanding, if you have not understand place, can consult candesartan ester manufacturer of professional and technical personnel, must be able to solve your problem. Hope these information can help to you.
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