Calcium Saccharate (kal' see um sak' a rate). C6H8CaO8·4H2O320.26 d-Glucaric acid, calcium salt (1:1) tetrahydrate; Calcium d-glucarate (1:1), tetrahydrate [5793-89-5]. DEFINITION Calcium Saccharate is the calcium salt of d-saccharic acid. It contains NLT 98.5% and NMT 102.0% of C6H8CaO8·4H2O. IDENTIFICATION • A. Identification TestsGeneral, Calcium 191 Sample: 0.2 g Analysis: Dissolve the Sample in 10 mL of water by the addition of 2 mL of hydrochloric acid. Acceptance criteria: Meets the requirements • B. Infrared Absorption 197M: Meets the requirements ASSAY • Procedure Sample: 600 mg Blank: 150.0 mL of water 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 with the aid of a sufficient volume of hydrochloric acid. While stirring, preferably with a magnetic stirrer, add 30 mL of Titrant from a 50-mL buret. Add 15 mL of 1 N sodium hydroxide and 300 mg of hydroxy naphthol blue. Continue the titration to a blue endpoint. Perform a Blank determination and make any necessary corrections. Calculate the percentage of calcium saccharate (C6H8CaO8·4H2O) in the portion of Calcium Saccharate taken: Result = {[(VS VB) × N × F]/W} × 100
Acceptance criteria: 98.5%102.0% IMPURITIES • Chloride and Sulfate, Chloride 221 Standard: 0.50 mL of 0.020 N hydrochloric acid Sample: 0.50 g dissolved in 10 mL of water by the addition of 2 mL of nitric acid Acceptance criteria: NMT 0.07% • Chloride and Sulfate, Sulfate 221 Standard: 0.6 mL of 0.020 N sulfuric acid Sample: 0.50 g dissolved in 10 mL of water by the addition of 2 mL of hydrochloric acid Acceptance criteria: NMT 0.12% • Heavy Metals, Method II 231: NMT 20 ppm • Sucrose and Reducing Sugars Sample: 0.5 g Analysis: Dissolve the Sample in 10 mL of water with the addition of 2 mL of hydrochloric acid, and boil the solution for about 2 min. Cool, add 15 mL of sodium carbonate TS, allow to stand for 5 min, and filter. Add 5 mL of the clear filtrate to about 2 mL of alkaline cupric tartrate TS, and boil for 1 min. Acceptance criteria: No red precipitate is formed immediately. SPECIFIC TESTS • Optical Rotation, Specific Rotation 781S Sample solution: 60 mg/mL in 4.8 N hydrochloric acid that has been allowed to stand for 1 h Acceptance criteria: +18.5 to +22.5 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 2467 Pharmacopeial Forum: Volume No. 27(6) Page 3261Chromatographic Column Chromatographic columns text is not derived from, and not part of, USP 35 or NF 30. |