阿托伐他汀钙原料药美国药典USP34标准(WORD版).docx

USP 34 Official Monographs / Atorvastatin 1949. Atorvastatin CalciumC66H68CaF2N4O10 · 3H2O 1209.42C66H68CaF2N4O10 1155.341H-Pyrrole-1-heptanoic acid, 2-(4-fluorophenyl)-?,?-dihydroxy-5-(1-methylethyl)-3-phenyl-4-[(phenylami-no)carbonyl]-, calcium salt (2:1), trihydrate [R-(R*,R*)]-;Calcium (?R,?R)-2-(p-fluorophenyl)-?,?-dihydroxy-5-isopropyl-3-phenyl-4-(phenylcarbamoyl)pyrrole-1-heptanoate (1:2), trihy-drate [344423-98-9].Anhydrous [134523-03-8].DEFINITIONAtorvastatin Calcium contains NLT 98.0% and NMT 102.0% ofC66H68 CaF2N4O10, calculated on the anhydrous basis.IDENTIFICATION·?A. INFRARED ABSORPTION （197K?·?B. CALCIUMDiluent: Methanol, water, and hydrochloric acid (75:25:2)Blank: DiluentSample solution: 0.05 mg/mL of Atorvastatin Calcium inDiluentAnalysisSamples: Sample solution and BlankSpectrometric conditions(see Chromatography （621?)—The (See Spectrophotometry and Light-Scattering （851?.)Mode: Atomic absorption spectrophotometryAnalytical wavelength: Calcium emission line at 422.7nmFlame: Air–acetyleneAcceptance criteria: The Sample solution exhibits a significant absorption at the calcium emission line at 422.7 nm.ASSAY ?PROCEDURE Buffer: 3.9 g/L of ammonium acetate in water. Adjust withglacial acetic acid to a pH of 5.0±0.1.Solution A: Acetonitrile, stabilizer-free tetrahydrofuran,andBuffer (21:12:67)Solution B: Acetonitrile, stabilizer-free tetrahydrofuran, andBuffer (61:12:27)Diluent: N,N-dimethylformamideMobile phase: See the gradient table below. [NOTE—If necessary, adjust the Mobile phase by increasingor decreasing the percentage of acetonitrile or the pH of the ammonium acetate solution to achieve a retention time of 26–34 min for the atorvastatin peak.]Time(min)Solution A(%)Solution B(%)01000401000702080850100100010010510001151000System suitability solution: 0.05 mg/mL of USP Atorvastatin Calcium RS and 0.06 mg/mL of USP Atorvastatin RelatedCompound B RS in DiluentStandard solution: 0.4 mg/mL of USP Atorvastatin CalciumRS in Diluent. [NOTE—Use sonicati