Glutamine (gloo' ta meen). DEFINITION Glutamine contains NLT 98.5% and NMT 101.5% of l-glutamine (C5H10N2O3), calculated on the dried basis. IDENTIFICATION ASSAY • Procedure Sample: 150 mg of Glutamine 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, and titrate with the Titrant. Perform a Blank determination. Calculate the percentage of glutamine (C5H10N2O3) in the Sample taken: Result = {[(VS VB) × N × F]/W} × 100
Acceptance criteria: 98.5%101.5% on the dried basis IMPURITIES • Residue on Ignition 281: NMT 0.3% • Chloride and Sulfate, Chloride 221 Standard solution: 0.50 mL of 0.020 N hydrochloric acid Sample: 0.7 g of Glutamine Acceptance criteria: NMT 0.05% • Chloride and Sulfate, Sulfate 221 Standard solution: 0.25 mL of 0.020 N sulfuric acid Sample: 0.8 g of Glutamine 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 Glutamine RS in water Sample solution: 10 mg/mL of Glutamine in water Chromatographic system Mode: TLC Adsorbent: 0.25-mm layer of chromatographic silica gel mixture Application volume: 5 µL Developing solvent system: Butyl alcohol, glacial acetic acid, and water (3:1:1) Spray reagent: 2 mg/mL of ninhydrin in a mixture of butyl alcohol and 2 N acetic acid (95:5) Analysis: Dry the plate at 80 for 30 min. Spray the plate with Spray reagent, heat at 80 for 10 min, and examine under white light. Acceptance criteria: No secondary spot of the Sample solution is larger or more intense than the principal spot of the Standard solution (NMT 0.5%). SPECIFIC TESTS • Optical Rotation, Specific Rotation 781S Sample solution: 40 mg/mL in water. Warm at 40 to dissolve. Analysis: Proceed as directed in the chapter, except measure at 20. Acceptance criteria: +6.3 to +7.3 • Loss on Drying 731: Dry a sample at 105 for 3 h: it loses NMT 0.3% of its weight. ADDITIONAL REQUIREMENTS • Packaging and Storage: Preserve in well-closed containers, and store at controlled room temperature. Auxiliary Information Please check for your question in the FAQs before contacting USP.
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