Calcium Levulinate (kal' see um lev'' ue lin' ate). C10H14CaO6270.30 Pentanoic acid, 4-oxo-, calcium salt (2:1), dihydrate; Calcium levulinate (1:2) dihydrate [5743-49-7]. Anhydrous [591-64-0]. DEFINITION Calcium Levulinate contains NLT 97.5% and NMT 100.5% of calcium levulinate (C10H14CaO6), calculated on the dried basis. IDENTIFICATION • A. Identification TestsGeneral, Calcium 191: A 100 mg/mL solution meets the requirements. • B. Sample solution: 0.5 g in 5 mL of water Analysis: To the Sample solution add 5 mL of 1 N sodium hydroxide, and filter. To the filtrate add 5 mL of iodine TS. Acceptance criteria: A precipitate of iodoform is produced. ASSAY • Procedure Sample: 600 mg of Calcium Levulinate Blank: 150 mL of water containing 2 mL of 3 N hydrochloric acid Titrimetric system (See Titrimetry 541.) Mode: Direct titration Titrant: 0.05 M edetate disodium VS Endpoint detection: Visual Analysis: Dissolve the Sample in 150 mL of water containing 2 mL of 3 N hydrochloric acid. While stirring with a magnetic stirrer, add 30 mL of Titrant from the titration buret. Add 15 mL of 1 N sodium hydroxide and 300 mg of hydroxy naphthol blue, and continue the titration to a blue endpoint. Perform the Blank determination. Calculate the percentage of calcium levulinate (C10H14CaO6) in the Sample taken: Result = {[(VS VB) × M × F]/W} × 100
Acceptance criteria: 97.5%100.5% on the dried basis IMPURITIES • Chloride and Sulfate, Chloride 221 Standard: 1.0 mL of 0.020 N hydrochloric acid Sample: 1.0 g Acceptance criteria: NMT 0.07% • Chloride and Sulfate, Sulfate 221 Standard: 1.0 mL of 0.020 N sulfuric acid Sample: 2.0 g Acceptance criteria: NMT 0.05% • Heavy Metals 231: NMT 20 ppm • Reducing Sugars Sample: 0.50 g Analysis: Dissolve the Sample in 10 mL of water, add 2 mL of 3 N hydrochloric acid, boil for about 2 min, and cool. Add 5 mL of sodium carbonate TS, allow to stand for 5 min, dilute with water to 20 mL, and filter. Add 5 mL of the clear filtrate to 2 mL of alkaline cupric tartrate TS, and boil for 1 min. Acceptance criteria: No red precipitate is formed immediately. SPECIFIC TESTS • Melting Range or Temperature, Class I 741: 119125 • Loss on Drying 731: Dry a sample at a pressure not exceeding 5 mm of mercury at 60 for 5 h: it loses 10.5%12.0% 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 2460 Pharmacopeial Forum: Volume No. 27(6) Page 3260Chromatographic Column Chromatographic columns text is not derived from, and not part of, USP 35 or NF 30. |