Compound Sodium Picosulfate Powder for Oral Solution

Sodium Picosulfate Oral Powder

Compound Sodium Picosulfate Powder for Oral Solution contains Sodium Picosulfate, Light Magnesium Oxide and Anhydrous Citric Acid. On reconstitution the powder produces Sodium Picosulfate and Magnesium Citrate in solution; heat is evolved during the reconstitution.

The powder complies with the requirements stated under Powders and Granules for Oral Solutions and Suspensions under Oral Liquids and with the following requirements.

90.0 to 110.0% of the stated amount.

90.0 to 110.0% of the stated amount.

90.0 to 110.0% of the stated amount.

A. In the test for Uniformity of content, the chromatogram obtained with solution (1) shows a peak with the same retention time as the peak in the chromatogram obtained with solution (2).

B. Dissolve the contents of one sachet in water; heat is evolved.

C. Add 100 mL of water to the contents of one sachet and allow to cool. Centrifuge and dilute 10 mL of the supernatant liquid to 100 mL with water. 5 mL of the resulting solution yields reaction A characteristic of citrates, Appendix VI.

D. Place about 1 g of the oral powder in a silica crucible, moisten with sulfuric acid, ignite gently, again moisten with sulfuric acid and ignite at 800° until a carbon-free residue is obtained. Disperse about 0.1 g of the residue obtained in 10 mL of water, adjust the pH to about 3 with 2m sulfuric acid, shake and filter. The filtrate yields the reactions characteristic of magnesium salts, Appendix VI.

Carry out the method for liquid chromatography, Appendix III D, using the following solutions. For solution (1) disperse the contents of one sachet in about 70 mL of water, allow to stand until effervescence has ceased, cool to room temperature, add sufficient water to produce a solution containing 0.01% w/v Sodium Picosulfate, mix and centrifuge; use the clear supernatant liquid. Solution (2) contains 0.0002% w/v of sodium picosulfate BPCRS in water. For solution (3) dissolve 10 mg of sodium picosulfate BPCRS in 2 mL of 0.1m hydrochloric acid, bring rapidly to the boil and heat for 1 minute. Cool in ice-water, add 2 mL of 0.1m sodium hydroxide and dilute to 10 mL with the mobile phase. Dilute 2 volumes to 50 volumes with the mobile phase.

The chromatographic procedure may be carried out using (a) a stainless steel column (10 cm × 4.6 mm) packed with octadecylsilyl silica gel for chromatography (5 µm) (Nucleosil C18 is suitable), (b) a guard column (2.5 cm × 4.5 mm) packed with octadecylsilyl silica gel for chromatography, (c) as the mobile phase with a flow rate of 1.5 mL per minute a mixture of 15 volumes of acetonitrile and 85 volumes of 0.067m mixed phosphate buffer pH 7.0 and (d) a detection wavelength of 263 nm.

Inject 50 µL of each solution. The test is not valid unless the chromatogram obtained with solution (3) closely resembles the appropriate reference chromatogram supplied with sodium picosulfate BPCRS.

In the chromatogram obtained with solution (1) the area of any peak due to impurity A (4-[(pyridin-2-yl)(4-hydroxyphenyl)methyl] phenyl sodium sulfate) is not greater than the area of the principal peak in the chromatogram obtained with solution (2) (2%).

Complies with the requirements stated under Powders with respect to the content of Sodium Picosulfate using the following method of analysis. Carry out the method for liquid chromatography, Appendix III D, using the following solutions. For solution (1) dissolve the contents of one sachet in about 70 mL of water, allow to stand until effervescence has ceased, cool to room temperature, add sufficient water to produce 100 mL, mix and centrifuge; use the clear supernatant liquid. Solution (2) contains 0.01% w/v of sodium picosulfate BPCRS in water.

The chromatographic procedure described under Impurity A may be used.

Calculate the content of C₁₈H₁₃NNa₂O₈S₂ using the declared content of C₁₈H₁₃NNa₂O₈S₂ in sodium picosulfate BPCRS.

Use the average of the 10 individual results obtained in the test for Uniformity of content.

To a quantity of the powder containing 30 mg of Light Magnesium Oxide add 4 mL of 3m hydrochloric acid, dissolve by warming on a water bath, cool and add 50 mL of water. Carry out the complexometric titration of magnesium, Appendix VIII D, beginning at the words 'To the resulting solution…', but using 0.05m disodium edetate VS as titrant. Each mL of 0.05m disodium edetate VS is equivalent to 2.015 mg of MgO.

During the titration take care to exclude carbon dioxide. Dissolve a quantity of the powder containing 0.8 g of Anhydrous Citric Acid in 60 mL of dimethylformamide and carry out Method II for non-aqueous titration, Appendix VIII A, using 0.1m tetrabutylammonium hydroxide VS as titrant, determining the end point potentiometrically and taking the second inflection as the end point. Each mL of 0.1m tetrabutylammonium hydroxide VS is equivalent to 96.05 mg of C₆H₈O₇.

The label states (1) the total weights, in grams, of the constituents in each sachet and (2) that heat is evolved when the contents of the sachet are added to water.

4-[(pyridin-2-yl)(4-hydroxyphenyl)methyl]phenyl sodium sulfate.