C14H26CaO16 (anhydrous) 490.42

Glucoheptonic acid, calcium salt (2:1).
Calcium glucoheptonate (1:2) [29039-00-7].

Packaging and storage— Preserve in well-closed containers.

Labeling— Label it to indicate whether it is hydrous or anhydrous; if hydrous, label it to indicate also the degree of hydration.

USP Reference standards 11— USP Calcium Gluceptate RS.

Identification—

pH 791: between 6.0 and 8.0, in a solution (1 in 10).

Loss on drying 731 (see Thermal Analysis 891)— [NOTE—The quantity taken for the determination may be adjusted, if necessary, for instrument sensitivity. Weight loss occurring at temperatures above about 160, indicative of decomposition, is not to be interpreted as Loss on drying.] Determine the percentage of volatile substances by thermogravimetric analysis on an appropriately calibrated instrument, using 10 to 25 mg of Calcium Gluceptate accurately weighed. Heat the specimen under test at a rate of 5 per minute in an atmosphere of nitrogen, at a flow rate of 40 mL per minute. Record the thermogram to 150: the anhydrous form loses not more than 1.0%, the 2H2O form not more than 6.9%, and the 3½H2O form not more than 11.4%, of its weight.

Chloride 221— A 1.0-g portion shows no more chloride than corresponds to 1.0 mL of 0.020 N hydrochloric acid (0.07%).

Sulfate 221— A 2.0-g portion shows no more sulfate than corresponds to 1.0 mL of 0.020 N sulfuric acid (0.05%).

Heavy metals 231— Dissolve 1 g in 25 mL of water: the limit is 0.002%.

Reducing sugars— Dissolve 0.50 g in 10 mL of hot water, add 2 mL of 3 N hydrochloric acid, boil for about 2 minutes, and cool. Add 5 mL of sodium carbonate TS, allow to stand for 5 minutes, dilute with water to 20 mL, and filter. Add 5 mL of the clear filtrate to about 2 mL of alkaline cupric tartrate TS, and boil for 1 minute: no red precipitate is formed immediately.

Organic volatile impurities, Method I 467: meets the requirements.

Residual solvents 467: meets the requirements.

Assay— Dissolve about 800 mg of Calcium Gluceptate, accurately weighed, in 150 mL of water containing 2 mL of 3 N hydrochloric acid. While stirring, preferably with a magnetic stirrer, add about 25 mL of 0.05 M edetate disodium VS from a 50-mL buret. Add 15 mL of 1 N sodium hydroxide and 300 mg of hydroxy naphthol blue, and continue the titration to a blue endpoint. Each mL of 0.05 M edetate disodium is equivalent to 24.52 mg of C14H26CaO16.

Expert Committee : (DSN05) Dietary Supplements - Non-Botanicals

USP29–NF24 Page 352

Phone Number : 1-301-816-8389