Biperiden Hydrochloride Tablets
DEFINITION
Biperiden Hydrochloride Tablets contain NLT 93.0% and NMT 107.0% of the labeled amount of C21H29NO·HCl.
IDENTIFICATION
• Thin-Layer Chromatographic Identification Test 
201
201
Standard solution:
Dissolve 10 mg of USP Biperiden Hydrochloride RS in 5 mL of water, mix, and sonicate to disperse the powder. Add 5 mL of methanol to the flask, mix, and sonicate for 15 min. Filter the solution into a separator, add 2 mL of 1 N sodium hydroxide and 10 mL of chloroform, and shake for 3 min. Filter the chloroform layer into a stoppered flask, and use the chloroform filtrate.
Sample solution:
To a quantity of finely powdered Tablets, equivalent to 10 mg of biperiden hydrochloride, add 5 mL of water, mix, and sonicate to disperse the powder. Add 5 mL of methanol to the flask, mix, and sonicate for 15 min. Filter the solution into a separator, add 2 mL of 1 N sodium hydroxide and 10 mL of chloroform, and shake for 3 min. Filter the chloroform layer into a stoppered flask, and use the chloroform filtrate.
Adsorbent:
0.25-mm layer of chromatographic silica gel mixture. Condition by heating the plate at 105
for 1 h and allowing to cool.
for 1 h and allowing to cool.
Application volume:
20 µL
Developing solvent system:
Methanol and ammonium hydroxide (100:1.5)
Visualization:
Iodine vapor, 10 min
Analysis:
Separately apply the Sample solution and the Standard solution to the chromatographic plate. Allow the applications to dry, and develop the chromatogram in the Developing solvent system until the solvent front has moved about three-fourths of the length of the plate. Remove the plate from the chamber, mark the solvent front, and allow the solvent to evaporate. Locate the spots on the plate by exposing the plate for 10 min to iodine vapors in a preequilibrated closed chamber, on the bottom of which there are iodine crystals.
Acceptance criteria:
The RF value of the principal spot of the Sample solution corresponds to that of the Standard solution.
ASSAY
• Procedure
Solution A:
38 g/L of monobasic sodium phosphate and 2 g/L of anhydrous dibasic sodium phosphate in water. Adjust to a pH of 5.3 ± 0.1, if necessary.
Solution B:
Dissolve 400 mg of bromocresol purple in 30 mL of water, add 6.3 mL of 0.1 N sodium hydroxide, and dilute with water to 500 mL.
Phosphate buffer–bromocresol purple solution:
Mix equal volumes of Solution A, Solution B, and chloroform, shake in a separator, and discard the chloroform. If appreciable color is extracted, repeat with additional portions of chloroform until no color is extracted.
Standard stock solution:
0.8 mg/mL of USP Biperiden Hydrochloride RS in methanol
Standard solution:
40 µg/mL of USP Biperiden Hydrochloride RS, prepared as follows: Transfer a suitable volume of Standard stock solution to a suitable volumetric flask, add 25% of the flask volume of water, and dilute with methanol to volume.
Sample solution:
Nominal concentration of 40 µg/mL of biperiden hydrochloride from NLT 20 Tablets, prepared as follows: Transfer a portion of finely powdered Tablets, to obtain the final nominal concentration, to a suitable volumetric flask; add 25% of the volume of water; and heat on a steam bath for 15 min. Cool, and dilute with methanol to volume.
Blank:
Methanol and water (3:1)
Analysis
Samples:
Standard solution, Sample solution, and Blank
Transfer 5.0 mL each of the Standard solution, the Sample solution, and the Blank to individual separators, each containing 10.0 mL of Phosphate buffer–bromocresolpurple solution. Extract the solution in each separator with 20.0 mL of chloroform for 2 min. After the layers have separated, pass each chloroform extract through filter paper (Whatman No. 31 or equivalent) into separate glass-stoppered, 50-mL volumetric flasks. In the same manner, extract the solution in each separator with another 20.0-mL portion of chloroform, filter, and wash each filter with 8 mL of chloroform, collecting each combined filtrate and washing, respectively, in the 50-mL volumetric flask containing the first extract. Dilute each with chloroform to volume. Concomitantly determine the absorbances of the solutions in 1-cm cells at the wavelength of maximum absorbance at about 408 nm, with a suitable spectrophotometer, using the Blank to set the instrument.
Calculate the percentage of the label claim of C21H29NO·HCl in the Tablets taken:
Result = (AU/AS) × (CS/CU) × 100
| AU | = | = absorbance of the Sample solution |
| AS | = | = absorbance of the Standard solution |
| CS | = | = concentration of USP Biperiden Hydrochloride RS in the Standard solution (µg/mL) |
| CU | = | = nominal concentration of the Sample solution (µg/mL) |
Acceptance criteria:
93.0%–107.0%
PERFORMANCE TESTS
• Dissolution 711
711
Medium:
0.01 N hydrochloric acid; 500 mL
Apparatus 2:
50 rpm
Time:
45 min
[Note—Determine the amount of C21H29NO·HCl dissolved by using the following method. ]
Phosphate buffer–bromocresol purple solution:
Prepare as directed in the Assay.
Standard stock solution:
0.8 mg/mL of USP Biperiden Hydrochloride RS in methanol
Standard solution:
2 µg/mL of USP Biperiden Hydrochloride RS, prepared as follows: Pipet 5 mL of Standard stock solution into a 500-mL volumetric flask, and add 0.01 N hydrochloric acid to volume. Pipet 25 mL of this solution into a suitable beaker, and adjust with 0.01 N sodium hydroxide to a pH of 5.3. Transfer this solution to a 100-mL volumetric flask with the aid of water, and dilute with water to volume.
Sample solution:
Sample per Dissolution 711. Filter 75 mL of the solution under test, pipet 50 mL of the clear filtrate into a suitable beaker, and adjust with 0.01 N sodium hydroxide to a pH of 5.3. Transfer this solution to a 100-mL volumetric flask with the aid of water, and dilute with water to volume.
711. Filter 75 mL of the solution under test, pipet 50 mL of the clear filtrate into a suitable beaker, and adjust with 0.01 N sodium hydroxide to a pH of 5.3. Transfer this solution to a 100-mL volumetric flask with the aid of water, and dilute with water to volume.
Blank:
Water
Analysis
Samples:
Standard solution, Sample solution, and Blank
Pipet 20.0 mL each of the Standard solution, the Sample solution, and the Blank into individual separators, each containing 10.0 mL of Phosphate buffer–bromocresol purple solution. Extract the solution in each separator with 40.0 mL of chloroform for 10 min. After the layers have separated, pass each chloroform extract through filter paper into separate, glass-stoppered containers, discarding the first 10 mL of each filtrate. Determine the amount of C21H29NO·HCl dissolved from absorbances at the wavelength of maximum absorbance at about 408 nm (10-cm cells) of the extract from the Sample solution in comparison with that of the extract from the Standard solution, using the Blank to set the instrument.
Tolerances:
NLT 75% (Q) of C21H29NO·HCl is dissolved.
• Uniformity of Dosage Units 905:
Meet the requirements
905:
Meet the requirements
ADDITIONAL REQUIREMENTS
• Packaging and Storage:
Preserve in tight containers.
• USP Reference Standards 11
11
USP Biperiden Hydrochloride RS 
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Auxiliary Information—
Please check for your question in the FAQs before contacting USP.
| Topic/Question | Contact | Expert Committee |
|---|---|---|
| Monograph | Ravi Ravichandran, Ph.D.
Principal Scientific Liaison 1-301-816-8330 |
(SM42010) Monographs - Small Molecules 4 |
| 711 |
Margareth R.C. Marques, Ph.D.
Senior Scientific Liaison 1-301-816-8106 |
(GCDF2010) General Chapters - Dosage Forms |
| Reference Standards | RS Technical Services 1-301-816-8129 rstech@usp.org |
USP35–NF30 Page 2363
Pharmacopeial Forum: Volume No. 35(5) Page 1108