Lysine Hydrochloride (lye' seen hye'' droe klor' ide). DEFINITION Lysine Hydrochloride contains NLT 98.5% and NMT 101.5% of l-lysine hydrochloride (C6H14N2O2·HCl), calculated on the dried basis. IDENTIFICATION ASSAY • Procedure Sample: 90 mg of Lysine Hydrochloride Blank: Mix 3 mL of formic acid and 50 mL of glacial acetic acid. Titrimetric system (See Titrimetry 541.) Mode: Direct titration Titrant: 0.1 N perchloric acid VS Endpoint detection: Potentiometric Analysis: Dissolve the Sample in 3 mL of formic acid and 50 mL of glacial acetic acid. Add 10 mL of mercuric acetate TS, and titrate with theTitrant. Perform the Blank determination. Calculate the percentage of lysine hydrochloride (C6H14N2O2·HCl) in the Sample taken: Result = {[(VS VB) × N × F]/W} × 100
Acceptance criteria: 98.5%101.5% on the dried basis OTHER COMPONENTS • Content of Chloride Sample: 350 mg of Lysine Hydrochloride Blank: 140 mL of water Titrimetric system (See Titrimetry 541.) Mode: Direct titration Titrant: 0.1 N silver nitrate VS Endpoint detection: Visual Analysis: Transfer the Sample to a porcelain casserole, and add 140 mL of water and 1 mL of dichlorofluorescein TS. Titrate with the Titrant until the silver chloride flocculates and the mixture acquires a faint pink color. Perform the Blank determination. Calculate the percentage of chloride (Cl) in the Sample taken: Result = {[(VS VB) × N × F]/W} × 100
Acceptance criteria: 19.0%19.6% IMPURITIES • Residue on Ignition 281: NMT 0.1% • Chloride and Sulfate, Sulfate 221 Standard solution: 0.10 mL of 0.020 N sulfuric acid Sample: 0.33 g of Lysine Hydrochloride Acceptance criteria: NMT 0.03% • Iron 241: NMT 30 ppm • Heavy Metals, Method I 231: NMT 15 ppm • Related Compounds Standard solution: 0.05 mg/mL of USP l-Lysine Hydrochloride RS in water. [NoteThis solution has a concentration equivalent to 0.5% of that of the Sample solution. ] Sample solution: 10 mg/mL of Lysine Hydrochloride in water System suitability solution: 0.4 mg/mL each of USP l-Lysine Hydrochloride RS and USP Arginine Hydrochloride RS Chromatographic system Mode: TLC Adsorbent: 0.25-mm layer of chromatographic silica gel mixture Application volume: 5 µL Developing solvent system: Isopropyl alcohol and ammonium hydroxide (7:3) Spray reagent: 0.2 g of ninhydrin in a mixture of butyl alcohol and 2 N acetic acid (95:5) System suitability Suitability requirements: The chromatogram of the System suitability solution exhibits two clearly separated spots. Analysis Samples: Standard solution, System suitability solution, and Sample solution Dry the plate between 100 and 105 until the ammonia completely disappears. Spray with Spray reagent, and heat between 100 and 105 for 15 min. Examine the plate under white light. Acceptance criteria: Any secondary spot of the Sample solution is not larger or more intense than the principal spot of the Standard solution. Individual impurities: NMT 0.5% Total impurities: NMT 2.0% SPECIFIC TESTS • Optical Rotation, Specific Rotation 781S Sample solution: 80 mg/mL in 6 N hydrochloric acid Acceptance criteria: +20.4 to +21.4 • Loss on Drying 731: Dry a sample at 105 for 3 h: it loses NMT 0.4% of its weight. ADDITIONAL REQUIREMENTS • Packaging and Storage: Preserve in well-closed containers. Auxiliary Information Please check for your question in the FAQs before contacting USP.
USP35NF30 Page 3733 Chromatographic Column Chromatographic columns text is not derived from, and not part of, USP 35 or NF 30. |