Bethanechol Chloride Tablets
» Bethanechol Chloride Tablets contain not less than 90.0 percent and not more than 110.0 percent of the labeled amount of bethanechol chloride (C7H17ClN2O2).
Packaging and storage—
Preserve in tight containers.
USP Reference standards 
11
—
11—
USP Bethanechol Chloride RS 
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Identification—
Pulverize a quantity of Tablets, equivalent to about 100 mg of bethanechol chloride, add 15 mL of ether, and allow to digest for 15 minutes. Decant the ether, again extract the residue with 10 mL of ether, and discard the ether extracts. To the residue add 30 mL of alcohol, shake for 10 minutes, and allow to stand for 1 hour with frequent agitation. Filter with suction, and evaporate the filtrate on a steam bath to dryness: the bethanechol chloride so obtained, recrystallized from alcohol and dried at 105
for 2 hours, responds to Identification test A under Bethanechol Chloride.
for 2 hours, responds to Identification test A under Bethanechol Chloride.
Dissolution 711—
711—
Medium:
0.1 N hydrochloric acid; 900 mL.
Apparatus 2:
50 rpm.
Time:
30 minutes.
Determine the amount of bethanechol chloride (C7H17ClN2O2) dissolved using the following method.
Buffer solution, Mobile phase, and Chromatographic system—
Proceed as directed in Assay.
Standard solution—
Dissolve an accurately weighed quantity of USP Bethanechol Chloride RS in Medium, and dilute quantitatively, and stepwise if necessary, with Medium to obtain a solution having a known concentration of USP Bethanechol Chloride RS approximately corresponding to the concentration of the solution under test.
Procedure—
Separately inject equal volumes (about 100 µL) of a filtered portion of the solution under test and the Standard solution into the chromatograph, record the chromatograms, and measure the responses for the major peaks. Calculate the quantity of bethanechol chloride (C7H17ClN2O2) dissolved based on the peak responses obtained from the solution under test and the Standard solution.
Tolerances—
Not less than 80% (Q) of the labeled amount of C7H17ClN2O2 is dissolved in 30 minutes.
Uniformity of dosage units 905:
meet the requirements.
905:
meet the requirements.
Related compounds—
Buffer solution—
Transfer about 0.48 g of methanesulfonic acid to a 1000-mL volumetric flask. Dissolve in and dilute with water to volume.
Mobile phase—
Prepare a filtered and degassed mixture of Buffer solution and acetonitrile (95:5). Make adjustments if necessary (see System Suitability under Chromatography 621).
621).
Standard solution—
Dissolve an accurately weighed quantity of USP Bethanechol Chloride RS in Mobile phase, and dilute quantitatively and stepwise if necessary, with Mobile phase to obtain a solution having a known concentration of about 1 µg of USP Bethanechol Chloride RS per mL.
Test solution—
Weigh and finely powder not fewer than 20 Tablets. Transfer an accurately weighed portion of the powder, equivalent to 1 Tablet, to a suitable volumetric flask so that the final solution yields a concentration of about 0.1 mg per mL of bethanechol chloride. Add an amount of Mobile phase, about 60% to 70% of the total volume of the flask. Sonicate for 20 minutes. Shake by mechanical means for about 15 minutes. Dilute with Mobile phase to volume, and mix. Allow to stand for 10 minutes, and pass the solution through a 1-µm glass filter, discarding the first 3 mL of the filtrate.
System suitability solution—
Transfer about 25 mg of bethanechol chloride, accurately weighed, to a 250-mL volumetric flask. Add 10 mL of 0.1 N sodium hydroxide, and allow to stand for about 15 minutes. Add 10 mL of 0.1 N hydrochloric acid. Dissolve in and dilute with Mobile phase to volume, and mix.
Chromatographic system (see Chromatography 621)—
The liquid chromatograph is equipped with a conductivity detector and a 3.9- × 150-mm column containing packing L55. The flow rate is about 1.0 mL per minute. The detector and column temperatures are maintained at 35 and 30, respectively. Chromatograph the System suitability solution, and record the peak responses as directed for Procedure: the relative retention times are about 0.9 for 2-hydroxypropyltrimethyl ammonium chloride and 1.0 for bethanechol; and the resolution, R, between 2-hydroxypropyltrimethyl ammonium chloride and bethanechol is not less than 0.8. Chromatograph the Standard solution, and record the peak responses as directed for Procedure: the relative standard deviation for replicate injections is not more than 10.0% for bethanechol chloride.
621)—
The liquid chromatograph is equipped with a conductivity detector and a 3.9- × 150-mm column containing packing L55. The flow rate is about 1.0 mL per minute. The detector and column temperatures are maintained at 35 and 30, respectively. Chromatograph the System suitability solution, and record the peak responses as directed for Procedure: the relative retention times are about 0.9 for 2-hydroxypropyltrimethyl ammonium chloride and 1.0 for bethanechol; and the resolution, R, between 2-hydroxypropyltrimethyl ammonium chloride and bethanechol is not less than 0.8. Chromatograph the Standard solution, and record the peak responses as directed for Procedure: the relative standard deviation for replicate injections is not more than 10.0% for bethanechol chloride.
Procedure—
Separately inject equal volumes (about 50 µL) of the Standard solution and Test solution into the chromatograph, record the chromatograms, and measure the responses for all of the peaks. Calculate the percentage of each impurity in the portion of Tablets taken by the formula:
100V(F/W)C(ri / rS)
in which C is the concentration, in mg per mL, of USP Bethanechol Chloride RS in the Standard solution; F is the relative response factor and is equal to 0.79 for 2-hydroxypropyltrimethyl ammonium chloride and 1.0 for any other impurity; ri is the peak response for any impurity in the Test solution; rS is the peak response of USP Bethanechol Chloride RS in the Standard solution; and W is the amount, in mg, of bethanechol chloride based on the average weight, labeled dose, and amount taken to prepare the Test solution. Not more than 1.0% of 2-hydroxypropyltrimethyl ammonium chloride is found; not more than 0.2% of any other impurity is found; and the sum of all the impurities is not more than 1.5%.
Assay—
Buffer solution—
Transfer about 29 mg of edetic acid to a 1000-mL volumetric flask, and dissolve in 500 mL of water. Add 300 µL of nitric acid to the volumetric flask, and dilute with water to volume. Pass through a 0.45-µm nylon membrane filter.
Mobile phase—
Prepare a filtered and degassed mixture of Buffer solution and acetonitrile (95:5). Make adjustments if necessary (see System Suitability under Chromatography 621).
621).
Standard preparation—
Dissolve an accurately weighed quantity of USP Bethanechol Chloride RS in Mobile phase, and dilute quantitatively, and stepwise if necessary, with Mobile phase to obtain a solution having a known concentration of about 0.1 mg of USP Bethanechol Chloride RS per mL.
Assay preparation—
Weigh and finely powder not fewer than 20 Tablets. Transfer an accurately weighed portion of the powder, equivalent to 1 Tablet, to a suitable volumetric flask so that the final solution yields a concentration of about 0.1 mg per mL of bethanechol chloride. Add an amount of Mobile phase, about 60% to 70% of the total volume of the flask. Sonicate for 20 minutes. Shake by mechanical means for about 15 minutes. Dilute with Mobile phase to volume, and mix. Allow to stand for 10 minutes, and pass the solution through a 1-µm glass filter, discarding the first 3 mL of the filtrate.
System suitability solution—
Transfer about 25 mg of bethanechol chloride, accurately weighed, to a 250-mL volumetric flask. Add 10 mL of 0.1 N sodium hydroxide, and allow to stand for about 15 minutes. Add 10 mL of 0.1 N hydrochloric acid. Dissolve in and dilute with Mobile phase to volume, and mix.
Chromatographic system (see Chromatography 621)—
The liquid chromatograph is equipped with a conductivity detector and a 3.9- × 150-mm column containing packing L55. The flow rate is about 1.0 mL per minute. The detector and column temperatures are maintained at 35 and 30, respectively. Chromatograph the System suitability solution, and record the peak responses as directed for Procedure: the relative retention time is about 0.9 for 2-hydroxypropyltrimethyl ammonium chloride and 1.0 for bethanechol; and the resolution, R, between 2-hydroxypropyltrimethyl ammonium chloride and bethanechol is not less than 0.8. Chromatograph the Standard preparation, and record the peak responses as directed for Procedure: the tailing factor is not more than 3.5; and the relative standard deviation for replicate injections is not more than 3.0%.
621)—
The liquid chromatograph is equipped with a conductivity detector and a 3.9- × 150-mm column containing packing L55. The flow rate is about 1.0 mL per minute. The detector and column temperatures are maintained at 35 and 30, respectively. Chromatograph the System suitability solution, and record the peak responses as directed for Procedure: the relative retention time is about 0.9 for 2-hydroxypropyltrimethyl ammonium chloride and 1.0 for bethanechol; and the resolution, R, between 2-hydroxypropyltrimethyl ammonium chloride and bethanechol is not less than 0.8. Chromatograph the Standard preparation, and record the peak responses as directed for Procedure: the tailing factor is not more than 3.5; and the relative standard deviation for replicate injections is not more than 3.0%.
Procedure—
Separately inject equal volumes (about 50 µL) of the Standard preparation and the Assay preparation into the chromatograph, record the chromatograms, and measure the peak responses. Calculate the quantity, in mg, of bethanechol chloride (C7H17ClN2O2) in the portion of Tablets taken by the formula:
VC(rU / rS)
in which C is the concentration, in mg per mL, of USP Bethanechol Chloride RS in the Standard preparation; V is the volume, in mL, of the flask used to prepare the Assay preparation; and rU and rS are the bethanechol chloride peak responses obtained from the Assay preparation and the Standard preparation, respectively.
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 |
| Reference Standards | RS Technical Services 1-301-816-8129 rstech@usp.org |
|
| 711 |
Margareth R.C. Marques, Ph.D.
Senior Scientific Liaison 1-301-816-8106 |
(GCDF2010) General Chapters - Dosage Forms |
USP35–NF30 Page 2353
Pharmacopeial Forum: Volume No. 30(5) Page 1587