» Dimenhydrinate Tablets contain not less than 90.0 percent and not more than 110.0 percent of the labeled amount of dimenhydrinate (C17H21NO·C7H7ClN4O2).
Packaging and storage Preserve in well-closed containers.
USP Reference standards 11
Identification The relative retention times of the 8-chlorotheophylline and diphenhydramine peaks in the chromatogram of the Assay preparation correspond to those in the chromatogram of the Standard preparation, as obtained in the Assay.
Medium: water; 900 mL.
Apparatus 2: 50 rpm.
Time: 45 minutes.
Procedure Determine the amount of C17H21NO·C7H7ClN4O2 dissolved by employing UV absorption at the wavelength of maximum absorbance at about 276 nm on filtered portions of the solution under test, suitably diluted with Dissolution Medium, if necessary, in comparison with a Standard solution having a known concentration of USP Dimenhydrinate RS in the same Medium.
Tolerances Not less than 75% (Q) of the labeled amount of C17H21NO·C7H7ClN4O2 is dissolved in 45 minutes.
Uniformity of dosage units 905: meet the requirements, the following procedure being used where the test for Content Uniformity is required. Transfer 1 Tablet to a 50-mL volumetric flask, add about 5 mL of Ammonium bicarbonate solution obtained from the Assay, and shake gently to disperse, sonicating, if necessary. Add 20.0 mL of Internal standard solution obtained from the Assay, shake by mechanical means for 30 minutes, and centrifuge. To 1 mL of the clear supernatant add about 9 mL of Diluent obtained from the Assay, and mix. Continue as directed for Procedure in the Assay.
Content of 8-chlorotheophylline
Ammonium bicarbonate solution, Diluent, Solution A, Solution B, Mobile phase, Internal standard solution, and Chromatographic system Prepare as directed in the Assay.
Standard solution Prepare as directed for Standard preparation in the Assay.
Test solution Prepare as directed for Assay preparation in the Assay.
Procedure Separately inject equal volumes (about 10 µL) of the Standard solution and the Test solution into the chromatograph, record the chromatograms, and measure the areas for the major peaks. Calculate the quantity, in mg, of 8-chlorotheophylline (C7H7ClN4O2) per Tablet taken by the formula:
(214.61/469.96)W(RU / RS)in which 214.61 and 469.96 are the molecular weights of 8-chlorotheophylline and dimenhydrinate, respectively; W is the weight, in mg, of USP Dimenhydrinate RS in the Standard solution; and RU and RS are peak area ratios of 8-chlorotheophylline to the internal standard obtained from the Test solution and the Standard solution, respectively. An amount of 8-chlorotheophylline that is between 43.4% and 47.9% of the amount of dimenhydrinate obtained in the Assay is found.
Ammonium bicarbonate solution Dissolve 4 g of ammonium bicarbonate in 250 mL of water.
Diluent Dissolve 4 g of ammonium bicarbonate in 200 mL of water. Add 50 mL of methanol, and mix.
Solution A Dissolve 0.8 g of ammonium bicarbonate in 800 mL of water. Add 200 mL of methanol, filter, and degas.
Solution B Dissolve 0.8 g of ammonium bicarbonate in 150 mL of water. Add 850 mL of methanol, filter, and degas.
Mobile phase Use variable mixtures of Solution A and Solution B as directed for Chromatographic system. Make adjustments if necessary (see System Suitability under Chromatography 621).
Internal standard solution Prepare a solution in methanol containing 2.0 mg of 2-hydroxybenzyl alcohol per mL.
Standard preparation Accurately weigh about 50 mg of USP Dimenhydrinate RS, add about 5 mL of Ammonium bicarbonate solution and 20.0 mL of Internal standard solution, and mix. To 1 mL of this solution add about 9 mL of Diluent, and mix.
Assay preparation Transfer 5 Tablets into a 250-mL volumetric flask, add 25 mL of Ammonium bicarbonate solution, and shake gently to disperse, sonicating if necessary. Add 100.0 mL of Internal standard solution, shake vigorously for 30 minutes, and centrifuge. To 1 mL of the clear supernatant add about 9 mL of Diluent, and mix.
Chromatographic system (see Chromatography 621) The liquid chromatograph is equipped with a 229-nm detector and a 4.6-mm × 25-cm column that contains packing L7. The flow rate is about 1.5 mL per minute. The chromatograph is programmed as follows.
Procedure Separately inject equal volumes (about 10 µL) of the Standard preparation and the Assay preparation into the chromatograph, record the chromatograms, and measure the areas for the major peaks. Calculate the quantity, in mg, of dimenhydrinate (C17H21NO·C7H7ClN4O2) per Tablet taken by the formula:
W(RU / RS)in which W is the weight, in mg, of USP Dimenhydrinate RS in the Standard preparation; and RU and RS are the peak area ratios of diphenhydramine to the internal standard obtained from the Assay preparation and the Standard preparation, respectively.
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USP35NF30 Page 2923Pharmacopeial Forum: Volume No. 30(4) Page 1191