Alanine (al' a neen). DEFINITION Alanine contains NLT 98.5% and NMT 101.5% of C3H7NO2, as l-alanine, calculated on the dried basis. IDENTIFICATION ASSAY • Procedure Sample: 80 mg of Alanine Titrimetric system (See Titrimetry 541.) Mode: Direct titration Titrant: 0.1 N perchloric acid VS Endpoint detection: Potentiometric Blank: 3 mL of formic acid in 50 mL of glacial acetic acid Analysis: Dissolve the Sample in a mixture of 3 mL of formic acid and 50 mL of glacial acetic acid, and titrate with 0.1 N perchloric acid VS. Calculate the percentage of C3H7NO2 in the portion taken: Result = [(V B) × N × F × 100]/W
Acceptance criteria: 98.5%101.5% on the dried basis IMPURITIES Inorganic Impurities • Residue on Ignition 281: NMT 0.15% • Chloride and Sulfate, Chloride 221: A 1.0-g portion shows no more chloride than corresponds to 0.70 mL of 0.020 N hydrochloric acid (0.05%). • Chloride and Sulfate, Sulfate 221: A 1.0-g portion shows no more sulfate than corresponds to 0.30 mL of 0.020 N sulfuric acid (0.03%). • Iron 241: NMT 30 ppm • Heavy Metals, Method I 231: NMT 15 ppm Organic Impurities • Procedure Adsorbent: 0.25-mm layer of chromatographic silica gel mixture Standard solution: 0.05 mg/mL of USP l-Alanine RS. [NoteThis solution has a concentration equivalent to 0.5% of that of the Sample solution. ] System suitability solution: 0.4 mg/mL each of USP l-Alanine RS and USP Glycine RS Sample solution: 10 mg/mL of Alanine Spray reagent: 2 mg/mL of ninhydrin in a mixture of butyl alcohol and 2 N acetic acid (95:5) Developing solvent system: Butyl alcohol, glacial acetic acid, and water (60:20:20) Application volume: 5 µL Analysis Samples: Standard solution, System suitability solution, and Sample solution Proceed as directed for Chromatography 621, Thin-Layer Chromatography. After air-drying the plate, repeat the development process. After air-drying a second time, spray with Spray reagent, and heat to 100105 for 15 min. Examine the plate under white light. The chromatogram obtained from the System suitability solution exhibits two clearly separated spots. Acceptance criteria Individual impurities: Any secondary spot of the Sample solution is not larger or more intense than the principal spot of the Standard solution, NMT 0.5% Total impurities: NMT 2.0% SPECIFIC TESTS • Optical Rotation, Specific Rotation 781S: +13.7 to +15.1 Sample solution: 100 mg/mL in 6 N hydrochloric acid • pH 791: 5.57.0, in a solution (1 in 20) • Loss on Drying 731: Dry a sample at 105 for 3 h: it loses NMT 0.2% of its weight. ADDITIONAL REQUIREMENTS • Packaging and Storage: Preserve in tight containers, and store at controlled room temperature. Auxiliary Information Please check for your question in the FAQs before contacting USP.
USP35NF30 Page 2081 Pharmacopeial Forum: Volume No. 27(5) Page 2973Chromatographic Column Chromatographic columns text is not derived from, and not part of, USP 35 or NF 30. |