Calcium Levulinate

C₁₀H₁₄CaO₆.2H₂O 306.32

C₁₀H₁₄CaO₆ 270.30

Pentanoic acid, 4-oxo-, calcium salt (2:1), dihydrate;

Calcium levulinate (1:2) dihydrate CAS RN: 5743-49-7; UNII: T6133S0781. Anhydrous CAS RN®: 591-64-0; UNII: LLQ966USIL.

1 DEFINITION

Calcium Levulinate contains NLT 97.5% and NMT 100.5% of calcium levulinate (C₁₀H₁₄CaO₆), calculated on the dried basis.

2 IDENTIFICATION

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.

3 ASSAY

PROCEDURE

Sample: 600 mg of Calcium Levulinate

Blank: 150 mL of water containing 2 mL of 3 N hydrochloric acid

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 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 = {[(V_S-V_B) x Mx F/W) x 100

V_s = Titrant volume consumed by the Sample (mL)

V_B = 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

4 IMPURITIES

4.1 CHLORIDE AND SULFATE, Chloride (221).

Standard: 1.0 mL of 0.020 N hydrochloric acid

Sample: 1.0 g

Acceptance criteria: NMT 0.07%

4.2 CHLORIDE AND SULFATE, Sulfate (221).

Standard: 1.0 mL of 0.020 N sulfuric acid

Sample: 2.0 g

Acceptance criteria: NMT 0.05%

4.3 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.

5 SPECIFIC TESTS

MELTING RANGE OR TEMPERATURE, Class I(741): 119°-125°

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.

6 ADDITIONAL REQUIREMENTS

PACKAGING AND STORAGE: Preserve in well-closed containers.