Calcium Levulinate
(kal' see um lev'' ue lin' ate).
Click to View Image

C10H14CaO6·2H2O 306.32

C10H14CaO6 270.30
Pentanoic acid, 4-oxo-, calcium salt (2:1), dihydrate;    
Calcium levulinate (1:2) dihydrate     [5743-49-7].
Anhydrous     [591-64-0].
Calcium Levulinate contains NLT 97.5% and NMT 100.5% of calcium levulinate (C10H14CaO6), calculated on the dried basis.
•  A. Identification Tests—General, 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.
•  Procedure
Sample:  600 mg of Calcium Levulinate
Blank:  150 mL of water containing 2 mL of 3 N hydrochloric acid
Titrimetric system 
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
VS== Titrant volume consumed by the Sample (mL)
VB== Titrant volume consumed by the Blank (mL)
M== Titrant molarity (mM/mL)
F== equivalency factor, 270.3 mg/mM
W== Sample weight (mg)
Acceptance criteria:  97.5%–100.5% on the dried basis
•  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.
•  pH 791
Sample solution:  100 mg/mL
Acceptance criteria:  7.0–8.5
•  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.
•  Packaging and Storage: Preserve in well-closed containers.
Auxiliary Information— Please check for your question in the FAQs before contacting USP.
Topic/Question Contact Expert Committee
Monograph Huy T. Dinh, M.S.
Scientific Liaison
(DS2010) Monographs - Dietary Supplements
USP35–NF30 Page 2460
Pharmacopeial Forum: Volume No. 27(6) Page 3260