Calcium Glubionate Syrup
»Calcium Glubionate Syrup is a solution containing equimolar amounts of Calcium Gluconate and Calcium Lactobionate or with Calcium Lactobionate predominating.It contains not less than 95.0percent and not more than 105.0percent of the labeled amount of calcium (Ca).
Packaging and storage— Preserve in tight containers,at a temperature not exceeding 30,and avoid freezing.
Identification—
A: Adilution of the Syrup with water (1in 10)responds to the tests for Calcium á191ñ.
B: Dilute a portion of the Syrup with water to obtain a test solution containing about 0.4mg of calcium per mL.Prepare a Standard solution in water containing 2mg of calcium gluconate and 4mg of calcium lactobionate per mL.Apply separately 5µLof the test solution and 5µLof the Standard solution to a suitable thin-layer chromatographic plate coated with 0.25-mm layer of chromatographic silica gel (see Chromatography á621ñ).Dry the plate in a current of cool air.Place the plate in a suitable chromatographic chamber lined with filter paper and previously equilibrated with a solvent system consisting of a mixture of alcohol,water,ethyl acetate,and ammonium hydroxide (50:30:10:10).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 100for 20minutes.Allow to cool,and spray with a spray reagent prepared as follows:Dissolve 2.5g of ammonium molybdate in about 50mLof 2Nsulfuric acid in a 100-mLvolumetric flask,add 1.0g of ceric sulfate,swirl to dissolve,dilute with 2Nsulfuric acid to volume,and mix.Heat the plate at 110for about 10minutes:the two principal spots obtained from the test solution correspond in color,size,and RFvalue to those obtained from the Standard solution.[NOTE—Sucrose,if present in the test solution,appears in the chromatogram as a spot between two principal spots.]
pHá791ñ: between 3.4and 4.5.
Assay— Transfer an accurately measured portion of Syrup,equivalent to about 70mg of Ca,to a suitable beaker.Add 2mLof 3Nhydrochloric acid,and dilute with water to about 150mL.While stirring with a magnetic stirrer,add about 20mLof 0.05Medetate disodium VSfrom a 50-mLburet.Add 15mLof 1Nsodium hydroxide and 300mg of hydroxy naphthol blue,and continue the titration to a blue endpoint.Each mLof 0.05Medetate disodium is equivalent to 2.004mg of calcium (Ca).
Auxiliary Information— Staff Liaison:Lawrence Evans,III,Ph.D.,Scientist
Expert Committee:(PA1)Pharmaceutical Analysis 1
USP28–NF23Page 325
Pharmacopeial Forum:Volume No.27(6)Page 3257
Phone Number:1-301-816-8389