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JP XV

O‹cial Monographs / Propranolol Hydrochloride

1037

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). Identiˆcation (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 xanthone—Dissolve 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
プロプラノロール塩酸塩

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. Identiˆcation (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. Containers—Well-closed contain-

Purity (1) Clarity and color of solution—Dissolve 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 substances—Dissolve 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,

Pipet 1 mL of this solution. System suitability— Test for required detectability: Measure exactly 5 mL of the standard solution. Separately. AT and AS.1z (1 g).5z (1 g.45 mm.3 with 2 mol/L sodium hydroxide TS. respectively. Add 50 mL of methanol. Uniformity of dosage units <6. and adjust to pH 3.0z of the labeled amount of propranolol hydrochloride (C16H21NO2.24>. and shake until the tablet is completely disintegrated. Determine the absorbances.44> Assay Weigh accurately about 0. The dissolution rate in 15 minutes is not less than 80z. dissolove in 50 mL of a mixture of acetic anhydride and acetic acid (100) (7:3).24>: it exhibits maxima between 288 nm and 292 nm. and use this solution as the standard solution. Discard the ˆrst 20 mL of the ˆltrate. of the sample solution and standard solution at 290 nm as directed under Ultraviolet-visible Spectrophotometry <2. Storage—Light-resistant. Not more than 0. add water to make exactly V? mL so that each mL contains about 10 mg of propranolol hydrochloride (C16H21NO2. and between 317 nm and 321 nm. add methanol to make exactly V? mL so that each mL contains about 20 mg of propranolol hydrochloride (C16H21NO2. weigh accurately about 50 mg of propranolol hydrochloride for assay.HCl). 259 Mobile phase: Dissolve 1. and make any necessary correction.58 mg of C16H21NO2.6 g of sodium lauryl sulfate and 0. Withdraw 20 mL or more of the dissolution medium 15 minutes after starting the test. System repeatability: When the test is repeated 6 times with 20 mL of the standard solution under the above operating conditions. and ˆlter through a membrane ˆlter with pore size of not more than 0.HCl) according to the labeled amount. Perform a blank determination in the same manner. Column: A stainless steel column 4.HCl) =WS×(AT/AS)×(V?/V)×(1/25) WS: Amount (mg) of propranolol hydrochloride for assay Dissolution <6.02> Perform the test according to the following method: it meets the requirement of the Content uniformity test. the number of theoretical plates and the symmetry factor of the peak of propranolol is not less than 3000 and not more than 2.10> 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. Identiˆcation Determine the absorption spectrum of the sample solution obtained in the Assay as directed under Ultraviolet-visible Spectrophotometry <2.24>. using 900 mL of water as the dissolution medium. System performance: When the procedure is run with 20 mL of the standard solution under the above operating conditions.0.5 g of Propranolol Hydrochloride. Pipet 2 mL of this solution. pipet V mL of the subsequent ˆltrate. Operating conditions— Detector: An ultraviolet absorption photometer (wavelength: 292 nm).1 mol/L perchloric acid VS =29.80). the relative standard deviation of the peak area of propranolol is not more than 2. add water to make exactly 100 mL. then add methanol to make exactly 100 mL.31 g of tetrabutylammonium phosphate in 450 mL of water. with Propranolol Hydrochloride. and use this solution as the sample solution.0z. shake vigorously for 10 minutes. and ˆlter. Determine the absorbances. pipet V mL of the subsequent ˆltrate. add 1 mL of sulfuric acid and 550 mL of acetonitrile for liquid chromatography. Amount (mg) of propranolol hydrochloride (C16H21NO2. Discard the ˆrst 10 mL of the ˆltrate. and titrate <2.50> with 0. and use this solution as the standard solution. and use this solution as the sample solution. 1059 4 C. Dissolution rate (z) with respect to the labeled amount of propranolol hydrochloride (C16H21NO2. add methanol to make exactly 100 mL. Loss on drying <2. and add the mobile phase to make exactly 20 mL. previously dried at 1059 for 4 hours. 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. of the sample solution and the standard solution at 290 nm as directed under Ultraviolet-visible Spectrophotometry <2.6 mm in inside diameter and 25 cm in length. and dissolve in water C to make exactly 50 mL. and dissolve in methanol to make exactly C 50 mL. Conˆrm 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.HCl Containers and storage Containers—Well-closed containers. Each mL of 0. Not more than 0. previously dried at 1059 for 4 hours. Method of preparation Prepare as directed under Tablets. Separately. Flow rate: Adjust the ‰ow rate so that the retention time of propranolol is about 4 minutes. Column temperature: A constant temperature of about C.1038 Propranolol Hydrochloride Tablets / O‹cial 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. Propranolol Hydrochloride Tablets プロプラノロール塩酸塩錠 Propranolol Hydrochloride Tablets contain not WS: Amount (mg) of propranolol hydrochloride for assay C: Labeled amount (mg) of propranolol hydrochloride . weigh accurately about 50 mg of propranolol hydrochloride for assay.HCl: 295. To 1 tablet of Propranolol Hydrochloride Tablets add 20 mL of water.HCl) =WS×(AT/AS)×(V?/V)×(1/C)×18 Residue on ignition <2.41> hours). less than 95.1 mol/L perchloric acid VS (potentiometric titration).0z and not more than 105. Time span of measurement: About 5 times as long as the retention time of propranolol. AT and AS. previously dried. packed with octadecylsilanized silica gel for liquid chromatography (5 mm in particle diameter).