supplement ii to the japanese pharmacopoeia fifteenth edition - NIHS

2064 General Tests, Process and Apparatus Supplement II, JP XVphy Prepared for gas chromatography.Demethoxycurcumin C 20 H 18 O 5 Yellow to orange crystallinepowder or powder. Sparingly soluble in methanol and inethanol (99.5), and practically insoluble in water. Melting point:166 - 170ºC.Identification Determine the absorption spectrum of a solutionof demethoxycurcumin in methanol (1 in 400000) as directedunder Ultraviolet-visible Spectrophotometry : itexhibits a maximum between 416 nm and 420 nm.Purity Related substances—(1) Dissolve 4 mg of demethoxycurcuminin 2 mL of methanol, and use this solution asthe sample solution. Pipet 1 mL of this solution, add methanol tomake exactly 20 mL, and use this solution as the standard solution.Perform the test as directed under Thin-layer Chromatography. Spot 5 µL each of the sample solution and standardsolution on a plate of silica gel for thin-layer chromatography.Develop the plate with a mixture of dichloromethane andmethanol (19:1) to a distance of about 10 cm, and air-dry theplate. Examine under ultraviolet light (main wavelength: 365nm): the spots other than the principal spot at the R f value ofabout 0.3 obtained from the sample solution are not more intensethan the spot from the standard solution.(2) Dissolve 1.0 mg of demethoxycurcumin in 5 mL ofmethanol, and use this solution as the sample solution. Pipet 1mL of this solution, add methanol to make exactly 20 mL, anduse this solution as the standard solution. Perform the test withexactly 10 µL each of the sample solution and standard solutionas directed under Liquid Chromatography according tothe following conditions. Determine each peak from both solutionsby the automatic integration method: the total area of thepeaks other than the peak of demethoxycurcumin obtained fromthe sample solution is not larger than the peak area of demethoxycurcuminfrom the standard solution.Operating conditionsColumn, column temperature, mobile phase and flow rate:Proceed as directed in the operating conditions in the Componentdetermination under TurmericDetector: A visible absorption photometer (wavelength: 422nm)Time span of measurement: About 4 times as long as the retentiontime of demethoxycurcumin beginning after the solventpeak.System suitabilitySystem performance and system repeatability: Proceed as directedin the system suitability in the Component determinationunder Turmeric.Test for required detectability: Pipet 1 mL of the standard solution,and add methanol to make exactly 20 mL. Confirm thatthe peak area of demethoxycurcumin obtained from 10 µL ofthis solution is equivalent to 3.5 to 6.5% of that of demethoxycurcuminfrom the standard solution.Dibenz[a,h]anthracene C 22 H 14 Very pale yellow togreen-yellow crystalline powder or powder. Practically insolublein water, in methanol and in ethanol (99.5). Melting point:265 - 270ºC.Identification Perform the test with dibenz[a,h]anthraceneas directed in the Purity: the mass spectrum of the main peakshows a molecular ion peak (m/z 278) and a fragment ion peak(m/z 139).Purity Related substances—Dissolve 3.0 mg ofdibenz[a,h]anthracene in methanol to make 100 mL, and usethis solution as the sample solution. Perform the test with 1 µLof this solution as directed under Gas Chromatography according to the following conditions, and determine each peakarea by the automatic integration method. Calculate the amountsof these peaks by the area percentage method: the total amountof the peaks other than dibenz[a,h]anthracene is not more than7.0%.Operating conditionsDetector: A mass spectrophotometer (EI)Mass scan range: 15.00 - 300.00Time of measurement: 12 - 30 minutesColumn: A fused silica column 0.25 mm in inside diameterand 30 m in length, coated inside with 5% diphenyl-95% dimethylpolysiloxanefor gas chromatography in thickness of 0.25- 0.5 µm.Column temperature: Inject at a constant temperature of about45ºC, raise the temperature to 240ºC at a rate of 40ºC per minute,maintain at 240ºC for 5 minutes, raise to 300ºC at a rate of 4ºCper minute, raise to 320ºC at a rate of 10ºC per minute, andmaintain at 320ºC for 3 minutes.Injection port temperature: A constant temperature of about250ºC.Interface temperature: A constant temperature of about 300ºC.Carrier gas: HeliumFlow rate: Adjust the flow rate so that the reaction time of thepeak of dibenz[a,h]anthracene is about 27 minutes.Split ratio: SplitlessSystem suitabilityTest for required detectability: Pipet 1 mL of the sample solution,and add methanol to make exactly 10 mL. Confirm that thepeak area of dibenz[a,h]anthracene obtained from 1 µL of thissolution is equivalent to 5 to 15% of that ofdibenz[a,h]anthracene from the standard solution.Dibutylamine C 8 H 19 N Colorless, clear liquid.Refractive index n 20D: 1.415 - 1.419Density (20ºC): 0.756 - 0.761 g/mL2,6-Dichloroindophenol sodium-sodium acetate TS Mixequal volumes of 2,6-dichloroindophenol sodium dihydrate solution(1 in 20) and acetic acid-sodium acetate TS, pH 7.0. Preparebefore use.Diisopropylamine [(CH 3 ) 2 CH] 2 NH Colorless, clear liquid,having an amine-like odor. Miscible with water and withethanol (95). The solution in water is alkaline.Refractive index n 20D: 1.391 - 1.394Specific gravity d 2020: 0.715 - 0.722Dimenhydrinate for assay C 17 H 21 NO·C 7 H 7 ClN 4 O 2[Same as the monograph Dimenhydrinate. When dried, it containsnot less than 53.8% and not more than 54.9% of diphen-