Calcium Gluceptate USP Grade

Calcium Gluceptate is anhydrous or contains varying amounts of water of hydration. It consists of the calcium salt of the alpha epimer of glucoheptonic acid or of a mixture of the alpha and beta epimers of glucoheptonic acid. It contains not less than 95.0 percent and not more than 102.0 percent of C 14H26CaO16, calculated on the dried basis.

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

Identification:
A: Infrared Absorption 197K .
B: A solution (1 in 50) responds to the tests for Calcium 191 .
pH: between 6.0 and 8.0, in a solution (1 in 10).
Loss on drying: [NOTE—The quantity taken for the determination may be adjusted, if necessary, for instrument sensitivity. Weight loss occurring at temperatures above about 160 degree 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 degrees per minute in an atmosphere of nitrogen, at a flow rate of 40 mL per minute. Record the thermogram to 150 degree: 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: A 1.0-g portion shows no more chloride than corresponds to 1.0 mL of 0.020 N hydrochloric acid (0.07%).
Sulfate: 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: 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, 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 and boil for 1 minute: no red precipitate is formed immediately.
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 EDTA disodium 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 EDTA disodium is equivalent to 24.52 mg of C14H26CaO16.

Calcium Glucoheptonate BP Grade

DEFINITION
Mixture in variable proportions, of calcium di(D-glycero-D-gulo-heptonate) and calcium di (D-glycero-D-ido-heptonate).
Content: 98.0 per cent to 102.0 per cent of calcium 2,3,4,5,6,7-hexahydroxyheptanoate (dried substance).

CHARACTERS
Appearance: White or very slightly yellow, amorphous powder, hygroscopic.
Solubility: Very soluble in water, practically insoluble in acetone and in ethanol (96 per cent).

IDENTIFICATION
A. Thin-layer chromatography.
B. 0.2 ml of (see Tests) gives reaction (b) of calcium.

TESTS
Solution S: Dissolve 10.0 g in carbon dioxide-free water prepared from distilled water and dilute to 100 ml with the same solvent.
Appearance of solution: Solution S is clear and not more intensely coloured than reference solution.
pH: 6.0 to 8.0 for solution S.
Reducing sugars: Maximum 1 per cent, expressed as glucose.
Cyanide: To pass the test.
Chlorides: Maximum 100 ppm.
Sulphates: Maximum 100 ppm, determined on solution S.
Iron: Maximum 40 ppm.
Heavy metals: Maximum 10 ppm.
Loss on drying: Maximum 5.0 per cent, determined on 1.000 g by drying in an oven at 105C for 3 h.
Bacterial endotoxins: Less than 167 IU/g, if intended for use in the manufacture of parenteral dosage forms without a further appropriate procedure for the removal of bacterial endotoxins.
ASSAY: Dissolve 0.800 g in a mixture of 150 ml of water and 2 ml of 3 M hydrochloric acid . While stirring, add 12.5 ml of 0.1 M sodium EDTA , 15 ml of 1 M sodium hydroxide and 0.3 g of hydroxynaphthol blue, sodium salt. Titrate with 0.1 M sodium EDTA until the colour changes from violet to pure blue.
1 ml of 0.1 M sodium EDTA is equivalent to 49.04 mg of C14H26CaO16.