Calcium Lactobionate (kal' see um lak'' toe bye' oh nate). C24H42CaO24·2H2O790.68 d-Gluconic acid, 4-O--d-galactopyranosyl-, calcium salt (2:1), dihydrate; Lactobionic acid, calcium salt (2:1), dihydrate; Calcium lactobionate (1:2), dihydrate [110638-68-1]. DEFINITION Calcium Lactobionate contains NLT 96.0% and NMT 102.0% of calcium lactobionate (C24H42CaO24·2H2O). IDENTIFICATION • A. Identification TestsGeneral, Calcium 191: A 20 mg/mL solution meets the requirements. • C. Thin Layer Chromatography Standard solution: 10 mg/mL of USP Calcium Lactobionate RS in water Sample solution: 10 mg/mL of Calcium Lactobionate in water Chromatographic system Mode: TLC Adsorbent: 0.25-mm layer of chromatographic silica gel Application volume: 5 µL Developing solvent system: Alcohol, ethyl acetate, ammonium hydroxide, and water (50:10:10:30) Spray reagent: Dissolve 2.5 g of ammonium molybdate in 50 mL of 2 N sulfuric acid in a 100-mL volumetric flask. Add 1.0 g of ceric sulfate, swirl to dissolve, dilute with 2 N sulfuric acid to volume, and mix. Analysis: Samples: Standard solution and Sample solution Develop the chromatogram until the solvent front has moved about three-fourths of the length of the plate. Remove the plate from the chamber, and dry at 100 for 20 min. Allow to cool, and spray with the Spray reagent. Heat the plate at 110 for about 10 min. Acceptance criteria: The principal spot of the Sample solution corresponds in color, size, and RF value to that of the Standard solution. ASSAY • Procedure Sample: 800 mg of Calcium Lactobionate Blank: 150 mL of water and 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 a mixture of water and 3 N hydrochloric acid (150:2). While stirring with a magnetic stirrer, add 15 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 lactobionate (C24H42CaO24·2H2O) in the Sample taken: Result = {[(VS VB) × M × F]/W} × 100
Acceptance criteria: 96.0%102.0% IMPURITIES • Halides Standard solution: 0.7 mL of 0.020 N hydrochloric acid Sample: 1.2 g Analysis: Proceed as directed for Chloride and Sulfate 221, Chloride. Acceptance criteria: NMT 0.04% • Chloride and Sulfate, Sulfate 221 Standard solution: 1 mL of 0.020 N sulfuric acid Sample: 2.0 g Analysis: Dissolve the Sample in boiling water. Acceptance criteria: NMT 0.05% • Heavy Metals 231 Test preparation: Mix 1 g in 4 mL of 1.2 N hydrochloric acid. Add water to make 25 mL, warm gently until dissolved, and cool to room temperature. Acceptance criteria: NMT 20 ppm • Reducing Substances Sample: 1.0 g of Calcium Lactobionate Blank: 20 mL of water Titrimetric system (See Titrimetry 541.) Mode: Residual titration Titrant: 0.1 N iodine VS Back-titrant: 0.1 N sodium thiosulfate VS Endpoint detection: Visual Analysis: Transfer the Sample to a 250-mL conical flask, dissolve in the Blank, and add 25 mL of alkaline cupric citrate TS. Cover the flask, boil gently for 5 min, accurately timed, and cool rapidly to room temperature. Add 25 mL of 0.6 N acetic acid, 10.0 mL of Titrant, and 10 mL of 3 N hydrochloric acid, and titrate with Back-titrant, adding 3 mL of starch TS as the endpoint is approached. Perform the Blank determination. Calculate the percentage of reducing substances (as dextrose) in the Sample taken: Result = {[(VB VS) × N × F]/W} × 100
Acceptance criteria: NMT 1.0% SPECIFIC TESTS • Optical Rotation, Specific Rotation 781S Sample solution: 100 mg/mL Acceptance criteria: +22.0 to +26.5 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 2459 Pharmacopeial Forum: Volume No. 27(6) Page 3260Chromatographic Column Chromatographic columns text is not derived from, and not part of, USP 35 or NF 30. |