|
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;)
430.37[299-28-5].
191
.
if necessary. Similarly, prepare a Standard solution of USP Potassium Gluconate RS in water containing 10 mg per mL. Apply separate 5-µL portions of the test solution and the Standard solution to a suitable thin-layer chromatographic plate (see Chromatography 621) coated with a 0.25-mm layer of chromatographic silica gel, and allow to dry. Develop the chromatogram in a solvent system consisting of a mixture of alcohol, water, ammonium hydroxide, and ethyl acetate (50:30:10:10) until the solvent front has moved about three-fourths of the length of the plate. Remove the plate from the chamber, and dry at 110 for 20 minutes. Allow to cool, spray with a spray reagent prepared as follows. Dissolve 2.5 g of ammonium molybdate in about 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. Heat the plate at 110 for about 10 minutes: the principal spot obtained from the test solution corresponds in color, size, and RF value to that obtained from the Standard solution.
731—
Dry it at 105 for 16 hours: the anhydrous form loses not more than 3.0% of its weight; the monohydrate form, where labeled as intended for use in preparing injectable dosage forms, loses not more than 1.0% of its weight, and where labeled as not intended for use in preparing injectable dosage forms loses not more than 2.0% of its weight.
221—
A 1.0-g portion shows no more chloride than corresponds to 0.07 mL of 0.020 N hydrochloric acid (0.005%). Where it is labeled as not intended for use in the preparation of injectable dosage forms, a 1.0-g portion shows no more chloride than corresponds to 1 mL of 0.020 N hydrochloric acid (0.07%).
621).
621)—
The ion chromatograph is equipped with a conductance detector, a 4-mm × 5-cm guard column that contains 15-µm packing L12, a 4-mm × 25-cm analytical column that contains 15-µm packing L12, and a micromembrane anion suppressor column, connected in series with the guard and analytical columns. The anion suppressor column is equipped with a micromembrane that separates the Mobile phase from the Suppressor regeneration solution flowing countercurrent to the Mobile phase at a rate of about 7 mL per minute. Condition the system for about 15 minutes with Mobile phase, using a flow rate of about 2 mL per minute. Chromatograph the Standard preparation, and record the peak responses as directed for Procedure: the column efficiency determined from the analyte peak is not less than 2500 theoretical plates; the tailing factor is not more than 1.2; and the relative standard deviation for replicate injections is not more than 2.0%.
to 80), and heat to boiling, with swirling, for 10 seconds to obtain a clear solution. Dilute 1 mL of this hot solution with water to obtain 100 mL of solution (test solution). Dilute 1.0 mL of a solution containing 0.716 mg of monobasic potassium phosphate per mL with water to obtain 100 mL of solution. To 2.0 mL of this solution add 98 mL of water (Standard solution). To the test solution and the Standard solution add 4 mL of sulfomolybdic acid TS, and mix. To both solutions add 0.1 mL of a freshly prepared mixture of 3 N hydrochloric acid and stronger acid stannous chloride TS (10:1), and mix. After 10 minutes any color observed in the test solution is not more intense than that obtained from the Standard solution (0.01%). [NOTE—Calcium Gluconate labeled as not intended for use in the preparation of injectable dosage forms is exempt from this requirement.]
221—
A 2.0-g portion dissolved in boiling water shows no more sulfate than corresponds to 0.1 mL of 0.020 N sulfuric acid (0.005%). Where it is labeled as not intended for use in the preparation of injectable dosage forms, a 2.0-g portion dissolved in boiling water shows no more sulfate than corresponds to 1 mL of 0.020 N sulfuric acid (0.05%).
211—
Dissolve 1.0 g in a mixture of 10 mL of hydrochloric acid and 20 mL of water, and dilute with water to 55 mL: the resulting solution meets the requirements of the test, the addition of 20 mL of 7 N sulfuric acid specified under Procedure being omitted. The limit is 3 ppm.
231:
0.001%. [NOTE—Where Calcium Gluconate is labeled as not intended for use in the preparation of injectable dosage forms, the limit is 0.002%.]
to 80, ammonium oxalate TS. Allow to stand for 4 hours, dilute with water to 200 mL, and filter. Evaporate 100 mL of the filtrate to dryness, and ignite to constant weight. The weight of the residue does not exceed 2 mg (0.4%). [NOTE—Calcium Gluconate labeled as not intended for use in preparing injectable dosage forms is exempt from this requirement.]
241, to 100-mL volumetric flasks, each containing 1.37 g of calcium chloride, previously tested and shown to contain less than 5 ppm of iron, dilute with 2 N hydrochloric acid to volume, and mix. These solutions contain, respectively, 0.2, 0.4, and 1.0 µg of iron per mL.
or evaporate to dryness because of danger of explosion.
] Transfer this solution to a 25-mL volumetric flask, dilute with 2 N hydrochloric acid to volume, and mix.
851) equipped with an iron hollow-cathode lamp and an air–acetylene flame, using the Blank solution as the blank and making deuterium background corrections. Plot the absorbances of the Standard preparations versus concentration, in µg per mL, of iron, and draw the straight line best fitting the three plotted points. From the graph so obtained, determine the concentration, C, in µg per mL, of iron in the Test preparation. Calculate the concentration of iron, in ppm, in the specimen taken by the formula:
467:
meets the requirements.
467:
meets the requirements.