SAMPLE - NOT FOR OFFICIAL USE
USP 35 Official Monographs / Calcium 2451
and 10 mL of 0.2 M edetate disodium. If necessar y, adjust
Calcium Citrate
.
with 1 N sodium hydroxide or 1 N hydrochloric acid to a pH
of 5.5. Transfer to a 100-mL volumetric flask, and dilute with
water to volume. This solution contains 0.05 g/mL of
fluoride.
Linearity solution B: Transfer 5.0 mL of the Standard solu-
tion to a 250-mL plastic beaker, and proceed as directed for
Linearity solution A beginning with Add 50 mL of water,.
This solution contains 0.25 g/mL of fluoride.
Linearity solution C: Transfer 10.0 mL of the Standard solu-
C12H10Ca3O14 4H2O 570.49 tion to a 250-mL plastic beaker, and proceed as directed for
1,2,3-Propanetricarboxylic acid, 2-hydroxy-, calcium salt (2:3), Linearity solution A beginning with Add 50 mL of water,.
tetrahydrate; This solution contains 0.50 g/mL of fluoride.
Calcium citrate (3:2), tetrahydrate [5785-44-4]. Sample solution: Transfer 1.0 g of Calcium Citrate to a 100-
DEFINITION mL beaker. Add 10 mL of water and, while stirring, 10 mL
Calcium Citrate contains four molecules of water of hydration. of 1 N hydrochloric acid. When dissolved, boil rapidly for 1
When dried at 150 to constant weight, it contains NL T min, transfer the solution to a 250-mL plastic beaker, and
97.5% and NMT 100.5% of Ca 3(C6H5O7)2. cool in ice water. Add 15 mL of 1.0 M sodium citrate and
10 mL of 0.2 M edetate disodium, and adjust with 1 N so-
IDENTIFICATION dium hydroxide or 1 N hydrochloric acid to a pH of 5.5.
A. Transfer this solution to a 100-mL volumetric flask, and di-
Analysis: Dissolve 0.5 g in a mixture of 10 mL of water and lute with water to volume.
2.5 mL of 2 N nitric acid. Add 1 mL of mer curic sulfate TS, Electrode system: Use a fluoride-specific, ion-indicating
heat to boiling, and add 1 mL of potassium permanganate electrode and a silversilver chloride reference electrode con-
TS. nected to a pH meter capable of measuring potentials with
Acceptance criteria: A white precipitate is formed. a minimum reproducibility of 0.2 mV (see pH 791).
B. Analysis
Sample: 0.5 g of Calcium Citrate Samples: Linearity solution A, Linearity solution B, Linearity
Analysis: Ignite completely the Sample at as low a tempera- solution C, and Sample solution
ture as possible, cool, and dissolve the residue in dilute gla- Transfer 50 mL of each Linearity solution A, Linearity solution
cial acetic acid (1:10). Filter, and add 10 mL of ammonium B, and Linearity solution C to separate 250-mL plastic beak-
oxalate TS to the filtrate. ers, and measure the potential of each solution with the
Acceptance criteria: A voluminous white precipitate that is Electrode system. Between each reading wash the elec-
soluble in hydrochloric acid is formed. trodes with water, and absorb any residual water by blot-
ting the electrodes dr y. Plot the logarithms of the fluoride
ASSAY concentrations (0.05, 0.25, and 0.50 g/mL, respectively)
PROCEDURE versus potential to obtain a Standard response line.
Sample solution: Dissolve 350 mg of Calcium Citrate, previ- Transfer 50 mL of the Sample solution to a 250-mL plastic
ously dried at 150 to constant weight, in 12 mL of 0.5 M beaker, and measure the potential with the Electrode sys-
hydrochloric acid, and dilute with water to about 100 mL. tem. From the measured potential and the Standard re-
Analysis: While stirring the Sample solution, add 30 mL of sponse line determine the concentration, C, in g/mL, of
0.05 M edetate disodium VS from a 50-mL buret. Add 15 fluoride ion in the Sample solution. Calculate the per cent-
mL of 1 N sodium hydroxide and 300 mg of hydroxy naph- age of fluoride in the specimen taken by multiplying C by
thol blue, and continue the titration to a blue endpoint. 0.01.
Each mL of 0.05 M edetate disodium is equivalent to 8.307 Acceptance criteria: NMT 0.003%
mg of calcium citrate (Ca 3(C6H5O7)2). LIMIT OF ACID-INSOLUBLE SUBSTANCES
Acceptance criteria: 97.5%100.5% on the dried basis Sample solution: Dissolve 5 g of Calcium Citrate by heating
with a mixture of hydrochloric acid and water (10:50) for 30
IMPURITIES min.
ARSENIC, Method I 211 Analysis: Filter, wash, and dr y at 105 for 2 h the residue so
Test preparation: Dissolve 1 g of Calcium Citrate in 5 mL of obtained.
3 N hydrochloric acid, and dilute with water to 35 mL. Acceptance criteria: The weight of the residue is NMT 10
Acceptance criteria: NMT 3 ppm mg (0.2%).
HEAVY METALS, Method I 231
Test preparation: Dissolve 1 g of Calcium Citrate in a mix- SPECIFIC TESTS
ture of hydrochloric acid and water (2:20). Add 1.5 mL of LOSS ON DRYING 731: Dry a sample at 150 for 4 h: it loses
ammonium hydroxide, and dilute with water to 25 mL. from 10.0% to 13.3% of its weight.
Acceptance criteria: NMT 20 ppm
LEAD 251 ADDITIONAL REQUIREMENTS
Test preparation: Dissolve 0.5 g of Calcium Citrate in 20 PACKAGING AND STORAGE: Preserve in well-closed containers.
mL of 3 N hydrochloric acid. Evaporate this solution on a USP REFERENCE STANDARDS 11
steam bath to 10 mL, dilute with water to 20 mL, and cool. USP Sodium Fluoride RS
Use 5 mL of Diluted Standard Lead Solution (5 g of Pb) for
the test.
Acceptance criteria: NMT 10 ppm
LIMIT OF FLUORIDE
.
[NOTEPrepare and store all solutions in plastic containers.] Calcium Glubionate Syrup
Standard stock solution: 1000 g/mL of fluoride ion from
USP Sodium Fluoride RS in water DEFINITION
Standard solution: 5 g/mL of fluoride ion from Standard Calcium Glubionate Syrup is a solution containing equimolar
stock solution. [NOTEPrepare on the day of use.] amounts of Calcium Gluconate and Calcium Lactobionate or
Linearity solution A: Transfer 1.0 mL of the Standard solu- with Calcium Lactobionate predominating. It contains NL T
tion to a 250-mL plastic beaker. Add 50 mL of water, 5 mL 95.0% and NMT 105.0% of the labeled amount of calcium
of 1 N hydrochloric acid, 10 mL of 1.0 M sodium citrate, (Ca).