supplement ii to the japanese pharmacopoeia fifteenth edition - NIHS

2124 Official Monographs Supplement II, JP XVexactly V´ mL so that each mL contains about 11 µg of emorfazone(C 11 H 17 N 3 O 3 ) according to the labeled amount, and usethis solution as the sample solution. Separately, weigh accuratelyabout 28 mg of emorfazone for assay, previously dried invacuum at 60ºC for 4 hours, and dissolve in water to make exactly100 mL. Pipet 4 mL of this solution, add water to makeexactly 100 mL, and use this solution as the standard solution.Determine the absorbances, A T and A S , of the sample solutionand standard solution at 239 nm as directed under Ultraviolet-visibleSpectrophotometry Dissolution rate (%) with respect to the labeled amount ofemorfazone (C 11 H 17 N 3 O 3 )= W S × (A T /A S ) × (V´/V) × (1/C) × 36W S : Amount (mg) of emorfazone for assayC: Labeled amount (mg) of emorfazone (C 11 H 17 N 3 O 3 ) in 1tabletAssay To 10 tablets of Emorfazone Tablets add 200 mL ofmethanol, shake well to disintegrate, add methanol to make exactly250 mL, and centrifuge. Pipet a volume of the supernatant,equivalent to about 8 mg of emorfazone (C 11 H 17 N 3 O 3 ), add exactly10 mL of the internal standard solution, add methanol tomake 50 mL, and use this solution as the sample solution.Separately, weigh accurately about 20 mg of emorfazone for assay,previously dried in vacuum at 60ºC for 4 hours, and dissolvein methanol to make exactly 25 mL. Pipet 10 mL of thissolution, add exactly 10 mL of the internal standard solution,add methanol to make 50 mL, and use this solution as the standardsolution. Perform the test with 20 µL each of the samplesolution and standard solution as directed under Liquid Chromatography according to the following conditions, andcalculate the ratios, Q T and Q S , of the peak area of emorfazoneto that of the internal standard.Amount (mg) of emorfazone (C 11 H 17 N 3 O 3 )= W S × (Q T /Q S ) × (2/5)W S : Amount (mg) of emorfazone for assayInternal standard solution—A solution of2,4-dinitrophenylhidrazine in methanol (3 in 2000). Prepare beforeuse.Operating conditions—Detector: An ultraviolet absorption photometer (wavelength:313 nm)Column: A stainless steel column 4.6 mm in inside diameterand 15 cm in length, packed with octadecylsilanized silica gelfor liquid chromatography (5 µm in particle diameter).Column temperature: A constant temperature of about 25ºC.Mobile phase: A mixture of water and methanol (11:10)Flow rate: Adjust the flow rate so that the retention time ofemorfazone is about 5 minutes.System suitability—System performance: When the procedure is run with 20 µLof the standard solution under the above operating conditions,emorfazone and the internal standard are eluted in this orderwith the resolution between these peaks being not less than 2.5.System repeatability: When the test is repeated 6 times with20 µL of the standard solution under the above operating conditions,the relative standard deviation of the ratio of the peak areaof emorfazone to that of the internal standard is not more than1.0%.Containers and storage Containers—Tight containers.Storage—Light-resistant.Ephedrine Hydrochloride Tabletsエフェドリン 塩 酸 塩 錠Add the following next to the Uniformity of dosageunits:Dissolution When the test is performed at 50 revolutionsper minute according to the Paddle method using 900 mLof water as the dissolution medium, the dissolution rate in 30minutes of Ephedrine Hydrochloride Tablets is not less than80%.Start the test with 1 tablet of Ephedrine Hydrochloride Tablets,withdraw not less than 20 mL of the medium at the specifiedminute after starting the test, and filter through a membrane filterwith a pore size not exceeding 0.45 µm. Discard the first 10mL of the filtrate, and use the subsequent filtrate as the samplesolution. Separately, weigh accurately about 28 mg of ephedrinehydrochloride for assay, previously dried at 105ºC for 3 hours,and dissolve in water to make exactly 100 mL. Pipet 5 mL ofthis solution, add water to make exactly 50 mL, and use this solutionas the standard solution. Perform the test with exactly 10µL each of the sample solution and standard solution as directedunder Liquid Chromatography according to the followingconditions, and determine the peak areas , A T and A S , ofephedrine in each solution.Dissolution rate (%) with respect to the labeled amount ofephedrine hydrochloride (C 10 H 15 NO·HCl)= W S × (A T /A S ) × (1/C) × 90W S : Amount (mg) of ephedrine hydrochloride for assayC: Labeled amount (mg) of ephedrine hydrochloride(C 10 H 15 NO·HCl) in 1 tabletOperating conditions—Detector, column, column temperature, mobile phase andflow rate: Proceed as directed in the operating conditions in thePurity (4) under Ephedrine Hydrochloride.System suitability—System performance: When the procedure is run with 10 µLof the standard solution under the above operating conditions,the number of theoretical plates and the symmetry factor of thepeak of ephedrine are not less than 10000 and not more than 2.0,respectively.System repeatability: When the test is repeated 6 times with10 µL of the standard solution under the above operating conditions,the relative standard deviation of the peak area of ephedrineis not more than 2.0%.