Calcium Saccharate
(kal' see um sak' a rate).
C6H8CaO8·4H2O 320.26 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 3261
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