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Ocial Monographs / Propranolol Hydrochloride

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Propantheline Bromide, when dried, contains not less than 98.0z and not more than 102.0z of C23H30BrNO3.
Description Propantheline Bromide occurs as a white to yellowish white, crystalline powder. It is odorless and has a very bitter taste. It is very soluble in water, in ethanol (95), in acetic acid (100) and in chloroform, soluble in acetic anhydride, and practically insoluble in diethyl ether. The pH of a solution of Propantheline Bromide (1 in 50) is between 5.0 and 6.0. Melting point: about 1619 (with decomposition, after C drying). Identication (1) To 5 mL of a solution of Propantheline Bromide (1 in 20) add 10 mL of sodium hydroxide TS, heat to C, boil for 2 minutes. Cool to 609 and add 5 mL of dilute hydrochloric acid. After cooling, collect the precipitates, and wash with water. Recrystallize from dilute ethanol, and dry at 1059 for 1 hour: the crystals melt <2.60> between 2179 C C and 2229 C. (2) Dissolve 0.01 g of the crystals obtained in (1) in 5 mL of sulfuric acid: a vivid yellow to yellow-red color develops. (3) To 5 mL of a solution of Propantheline Bromide (1 in 10) add 2 mL of dilute nitric acid: this solution responds to the Qualitative Tests <1.09> (1) for bromide. Purity Xanthene-9-carboxylic acid and xanthoneDissolve 10 mg of Propantheline Bromide in exactly 2 mL of chloroform, and use this solution as the sample solution. Separately, dissolve 1.0 mg of xanthene-9-carboxylic acid and 1.0 mg of xanthone in exactly 40 mL of chloroform, and use this solution as the standard solution. Perform the test immediately with these solutions as directed under Thin-layer Chromatography <2.03>. Spot 25 mL each of the sample solution and standard solution on a plate of silica gel with uorescent indicator for thin-layer chromatography, and air-dry the plate for 10 minutes. Develop the plate with a mixture of 1,2dichloroethane, methanol, water and formic acid (56:24:1:1) to a distance of about 12 cm, and air-dry the plate. Examine under ultraviolet light: the spots from the sample solution corresponding to the spots from the standard solution are not more intense than those from the standard solution. Loss on drying <2.41> 4 hours). Not more than 0.5z (2 g, 1059 C, Not more than 0.1z (1 g).

Propranolol Hydrochloride

C16H21NO2.HCl: 295.80 (2 RS )-1-(1-Methylethyl)amino-3-(naphthalen1-yloxy)propan-2-ol monohydrochloride [318-98-9 ]

Propranolol Hydrochloride, when dried, contains not less than 99.0z and not more than 101.0z of C16H21NO2.HCl.
Description Propranolol Hydrochloride occurs as a white, crystalline powder. It is freely soluble in methanol, soluble in water and in acetic acid (100), and sparingly soluble in ethanol (99.5). A solution of Propranolol Hydrochloride in methanol (1 in 40) shows no optical rotation. It is gradualy colored to yellowish white to light brown by light. Identication (1) Determine the absorption spectrum of a solution of Propranolol Hydrochloride in methanol (1 in 50,000) as directed under Ultraviolet-visible Spectrophotometry <2.24>, and compare the spectrum with the Reference Spectrum: both spectra exhibit similar intensities of absorption at the same wavelengths (2) Determine the infrared absorption spectrum of Propranolol Hydrochloride, previously dried, as directed in the potassium chloride disk method under Infrared Spectrophotometry <2.25>, and compare the spectrum with the Reference Spectrum: both spectra exhibit similar intensities of absorption at the same wave numbers. (3) A solution of Propranolol Hydrochloride (1 in 50) responds to the Qualitative Tests <1.09> (2) for chloride. pH <2.54> The pH of a solution prepared by dissolving 0.5 g of Propranolol Hydrochloride in 50 mL of water is 5.0 6.0. Melting point <2.60> 163 1669 C

Residue on ignition <2.44>

Assay Weigh accurately about 1 g of Propantheline Bromide, previously dried, dissolve in 50 mL of a mixture of acetic anhydride and acetic acid (100) (7:3), and titrate <2.50> with 0.1 mol W perchloric acid VS (potentiometric titration). L Perform a blank determination, and make any necessary correction. Each mL of 0.1 mol W perchloric acid VS L 44.84 g of C23H30BrNO3 Containers and storage ers. ContainersWell-closed contain-

Purity (1) Clarity and color of solutionDissolve 1.0 g of Propranolol Hydrochloride in 20 mL of water: the solution is clear and colorless. (2) Heavy metals < 1.07 > Proceed with 1.0 g of Propranolol Hydrochloride according to Method 4, and perform the test. Prepare the control solution with 2.0 mL of Standard Lead Solution (not more than 20 ppm). (3) Related substancesDissolve 20 mg of Propranolol Hydrochloride in 10 mL of the mobile phase, and use this solution as the sample solution. Pipet 2 mL of the sample solution, and add the mobile phase to make exactly 100 mL. Pipet 1 mL of this solution, add the mobile phase to make exactly 10 mL, and use this solution as the standard solution. Perform the test with exactly 20 mL each of the sample solution and standard solution as directed under Liquid Chromatography <2.01> according to the following conditions,

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Propranolol Hydrochloride Tablets / Ocial Monographs

JP XV

and determine each peak area by the automatic integration method: the area of the peak other than propranolol is not larger than 1/2 times the peak area of propranolol from the standard solution, and the total area of the peaks other than the peak of propranolol is not larger than 2 times the peak area of propranolol from the standard solution. Operating conditions Detector: An ultraviolet absorption photometer (wavelength: 292 nm). Column: A stainless steel column 4.6 mm in inside diameter and 25 cm in length, packed with octadecylsilanized silica gel for liquid chromatography (5 mm in particle diameter). Column temperature: A constant temperature of about C. 259 Mobile phase: Dissolve 1.6 g of sodium lauryl sulfate and 0.31 g of tetrabutylammonium phosphate in 450 mL of water, add 1 mL of sulfuric acid and 550 mL of acetonitrile for liquid chromatography, and adjust to pH 3.3 with 2 mol/L sodium hydroxide TS. Flow rate: Adjust the ow rate so that the retention time of propranolol is about 4 minutes. Time span of measurement: About 5 times as long as the retention time of propranolol. System suitability Test for required detectability: Measure exactly 5 mL of the standard solution, and add the mobile phase to make exactly 20 mL. Conrm that the peak area of propranolol obtained with 20 mL of this solution is equivalent to 17 to 33z of that with 20 mL of the standard solution. System performance: When the procedure is run with 20 mL of the standard solution under the above operating conditions, the number of theoretical plates and the symmetry factor of the peak of propranolol is not less than 3000 and not more than 2.0, respectively. System repeatability: When the test is repeated 6 times with 20 mL of the standard solution under the above operating conditions, the relative standard deviation of the peak area of propranolol is not more than 2.0z. Loss on drying <2.41> hours). Not more than 0.5z (1 g, 1059 4 C, Not more than 0.1z (1 g).

less than 95.0z and not more than 105.0z of the labeled amount of propranolol hydrochloride (C16H21NO2.HCl: 295.80).
Method of preparation Prepare as directed under Tablets, with Propranolol Hydrochloride. Identication Determine the absorption spectrum of the sample solution obtained in the Assay as directed under Ultraviolet-visible Spectrophotometry <2.24>: it exhibits maxima between 288 nm and 292 nm, and between 317 nm and 321 nm. Uniformity of dosage units <6.02> Perform the test according to the following method: it meets the requirement of the Content uniformity test. To 1 tablet of Propranolol Hydrochloride Tablets add 20 mL of water, and shake until the tablet is completely disintegrated. Add 50 mL of methanol, shake vigorously for 10 minutes, then add methanol to make exactly 100 mL, and lter. Discard the rst 20 mL of the ltrate, pipet V mL of the subsequent ltrate, add methanol to make exactly V? mL so that each mL contains about 20 mg of propranolol hydrochloride (C16H21NO2.HCl), and use this solution as the sample solution. Separately, weigh accurately about 50 mg of propranolol hydrochloride for assay, previously dried at 1059 for 4 hours, and dissolve in methanol to make exactly C 50 mL. Pipet 2 mL of this solution, add methanol to make exactly 100 mL, and use this solution as the standard solution. Determine the absorbances, AT and AS, of the sample solution and the standard solution at 290 nm as directed under Ultraviolet-visible Spectrophotometry <2.24>. Amount (mg) of propranolol hydrochloride (C16H21NO2.HCl) WS(AT/AS)(V?/V)(1/25)

WS: Amount (mg) of propranolol hydrochloride for assay

Dissolution <6.10> Perform the test according to the following method: it meets the requirement. Perform the test with 1 tablet of Propranolol Hydrochloride Tablets at 50 revolutions per minute according to the Paddle method, using 900 mL of water as the dissolution medium. Withdraw 20 mL or more of the dissolution medium 15 minutes after starting the test, and lter through a membrane lter with pore size of not more than 0.45 mm. Discard the rst 10 mL of the ltrate, pipet V mL of the subsequent ltrate, add water to make exactly V? mL so that each mL contains about 10 mg of propranolol hydrochloride (C16H21NO2.HCl) according to the labeled amount, and use this solution as the sample solution. Separately, weigh accurately about 50 mg of propranolol hydrochloride for assay, previously dried at 1059 for 4 hours, and dissolve in water C to make exactly 50 mL. Pipet 1 mL of this solution, add water to make exactly 100 mL, and use this solution as the standard solution. Determine the absorbances, AT and AS, of the sample solution and standard solution at 290 nm as directed under Ultraviolet-visible Spectrophotometry <2.24>. The dissolution rate in 15 minutes is not less than 80z. Dissolution rate (z) with respect to the labeled amount of propranolol hydrochloride (C16H21NO2.HCl) WS(AT/AS)(V?/V)(1/C)18

Residue on ignition <2.44>

Assay Weigh accurately about 0.5 g of Propranolol Hydrochloride, previously dried, dissolove in 50 mL of a mixture of acetic anhydride and acetic acid (100) (7:3), and titrate <2.50> with 0.1 mol/L perchloric acid VS (potentiometric titration). Perform a blank determination in the same manner, and make any necessary correction. Each mL of 0.1 mol/L perchloric acid VS 29.58 mg of C16H21NO2.HCl Containers and storage ContainersWell-closed containers. StorageLight-resistant.

Propranolol Hydrochloride Tablets

Propranolol Hydrochloride Tablets contain not

WS: Amount (mg) of propranolol hydrochloride for assay C: Labeled amount (mg) of propranolol hydrochloride