supplement ii to the japanese pharmacopoeia fifteenth edition - NIHS

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2066 General Tests, Process and Apparatus Supplement II, JP XVLoss on drying : Not more than 1.5% (0.5 g, 105ºC, 4hours).Heart infusion agar medium Prepared for biochemicaltests.Heptyl parahydroxybenzoate C 14 H 20 O 3 White crystalsor crystalline powder.Melting point : 45 - 50ºC.Content: Not less than 98.0% Assay—Weigh accuratelyabout 3.5 g of heptyl parahydroxybenzoate, dissolve in 50 mL ofdiluted N,N-dimethylformamide (4 in 5), and titrate with1 mol/L sodium hydroxide VS (potentiometric titration). Performa blank determination in the same manner, and make anynecessary correction.Each mL of 1 mol/L sodium hydroxide VS= 236.3 mg of C 14 H 20 O 3Hexyl parahydroxybenzoate C 13 H 18 O 3 White crystals orcrystalline powder.Melting point : 49 - 53ºCContent: Not less than 98.0%. Assay—Proceed as directedin the Assay under Ethyl Parahydroxybenzoate.Each mL of 1 mol/L sodium hydroxide VS= 222.3 mg of C 13 H 18 O 3Hyodeoxycholic acid for thin-layer chromatographyC 24 H 40 O 4 White to pale brown crystalline powder or powder.Freely soluble in methanol an in ethanol (99.5), and practicallyinsoluble in water.Identification Determine the infrared absorption spectrumof hyodeoxycholic acid for thin-layer chromatography as directedin the potassium bromide disk method under InfraredSpectrophotometry : it exhibits absorption at the wavenumbers of about 2940 cm -1 , 2840 cm -1 , 2360 cm -1 , 1740 cm -1 ,1460 cm -1 , 1340 cm -1 , 1200 cm -1 , 1160 cm -1 , 1040 cm -1 and 600cm -1 .Optical rotation [α] 20D: +7 - +10º (0.4 g, ethanol(99.5), 20 mL, 100 mm).Melting point : 198 - 205ºCPurity Related substances—Dissolve 20 mg of hyodeoxycholicacid for thin-layer chromatography in 1 mL of methanol,and use this solution as the sample solution. Pipet 0.2 mL of thissolution, add methanol to make exactly 10 mL, and use this solutionas the standard solution. Perform the test as directed underThin-layer Chromatography . Spot 5 µL each of thesample solution and standard solution on a plate of silica gel forthin-layer chromatography. Develop the plate with a mixture ofchloroform, acetone and acetic acid (100) (7:2:1) to a distanceof about 10 cm, and air-dry the plate. Splay evenly dilute sulfuricacid on the plate, and heat at 105ºC for 10 minutes: the spotsother than the principal spot at the R f value of about 0.3 obtainedfrom the sample solution are not more intense than thespot from the standard solution.10-Hydroxy-2-(E)-decenoic acid for component determination10-hydroxy-2-(E)-decenoic acid for thin-layer chromatographymeeting the following additional specifications.Purity Related substances—Dissolve 10 mg of10-hydroxy-2-(E)-decenoic acid for component determination in100 mL of methanol, and use this solution as the sample solution.Pipet 1 mL of this solution, add methanol to make exactly100 mL, and use this solution as the standard solution. Performthe test with exactly 10 µL each of the sample solution andstandard solution as directed under Liquid Chromatography according to the following conditions. Determine eachpeak from both solutions by the automatic integration method:the total area of the peaks other than the peak of10-hydroxy-2-(E)-decenoic acid is not larger than the peak areaof 10-hydroxy-2-(E)-decenoic acid from the standard solution.Operating conditionsDetector, column, column temperature, mobile phase andflow rate: Proceed as directed in the operating conditions in theComponent determination under Royal Jelly.Time span of measurement: About 4 times as long as the retentiontime of 10-hydroxy-2-(E)-decenoic acid beginning afterthe solvent peak.System suitabilitySystem performance and system repeatability: Proceed as directedin the system suitability in the Component determinationunder Royal Jelly.Test for required detectability: Pipet 1 mL of the standard solution,and add methanol to make exactly 20 mL. Confirm thatthe peak area of 10-hydroxy-2-(E)-decenoic acid obtained from10 µL of this solution is equivalent to 3.5 to 6.5% of that of10-hydroxy-2-(E)-decenoic acid from the standard solution.10-Hydroxy-2-(E)-decenoic acid for thin-layer chromatographyC 10 H 18 O 3 White crystalline powder. Very solublein methanol, freely soluble in ethanol (99.5), soluble in diethylether, and slightly soluble in water.Identification Determine the absorption spectrum of a solutionof 10-hydroxy-2-(E)-decenoic acid for thin-layer chromatographyin ethanol (99.5) (1 in 125000) as directed under Ultraviolet-visibleSpectrophotometry : it exhibits a maximumbetween 206 nm and 210 nm.Melting point : 63 - 66ºC.Purity Related substances—Dissolve 5.0 mg of10-hydroxy-2-(E)-decenoic acid for thin-layer chromatographyin 1 mL of diethyl ether. Perform the test with 20 µL of this solutionas directed in the Identification under Royal Jelly: no spotother than the principal spot at around R f 0.5 appears.Imidapril hydrochloride C 20 H 27 N 3 O 6·HCl [Same as themonograph Imidapril Hydrochloride.]Imidapril hydrochloride for assay C 20 H 27 N 3 O 6·HCl[Same as the monograph Imidapril Hydrochloride. When dried,it contains not less than 99.0% of imidapril hydrochloride(C 20 H 27 N 3 O 6·HCl).]Irsogladine maleate C 9 H 7 Cl 2 N 5·C 4 H 4 O 4 [Same as themonograph Irsogladine Maleate.]Irsogladine maleate for assay C 9 H 7 Cl 2 N 5·C 4 H 4 O 4 [Same
Supplement II, JP XV General Tests, Process and Apparatus 2067as the monograph Irsogladine Maleate. When dried, it containsnot less than 99.5% of irsogladine maleate(C 9 H 7 Cl 2 N 5·C 4 H 4 O 4 ).]Isosorbide dinitrate for assay C 6 H 8 N 2 O 8 [Same as themonograph Isosorbide Dinitrate. It contains not less than 99.0%of isosorbide dinitrate (C 6 H 8 N 2 O 8 ) meeting the following additionalspecifications.]Purity Related substances—Dissolve 50 mg of isosorbidedinitrate for assay in 50 mL of a mixture of water and methanol(1:1), and use this solution as the sample solution. Pipet 1 mL ofthis solution, add a mixture of water and methanol (1:1) to makeexactly 200 mL, and use this solution as the standard solution.Perform the test with exactly 10 µL each of the sample solutionand standard solution as directed under Liquid Chromatography, and determine each peak area of both solutions by theautomatic integration method: the total area of the peaks otherthan the peak of isosorbide dinitrate obtained from the samplesolution is not larger than the peak area of isosorbide dinitratefrom the standard solution.Operating conditionsDetector, column, column temperature, mobile phase andflow rate: Proceed as directed in the operating procedures in theAssay under Isosorbide Dinitrate Tablets.Time span of measurement: About 2 times as long as the retentiontime of isosorbide dinitrate beginning after the solventpeak.System suitabilityTest for required detectability: Pipet 5 mL of the standard solution,and add a mixture of water and methanol (1:1) to makeexactly 50 mL. Confirm that the peak area of isosorbide dinitrateobtained from 10 µL of this solution is equivalent to 7 to13% of that of isosorbide dinitrate from the standard solution.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 isosorbide dinitrate are not less than 3000 and not morethan 1.5, 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 isosorbidedinitrate is not more than 2.0%.Ketoconazolemonograph.]C 26 H 28 Cl 2 N 4 O 4 [Same as the namesakeKetoconazole for assay C 26 H 28 Cl 2 N 4 O 4 [Same as themonograph Ketoconazole. When dried, it contains not less than99.5% of ketoconazole (C 26 H 28 Cl 2 N 4 O 4 ).]4-methoxybenzaldehyde-sulfuric acid-acetic acid-ethanolTS for spray To 9 mL of ethanol (95) add 0.5 mL of4-methoxybenzaldehyde, mix gently, add gently 0.5 mL of sulfuricacid and 0.1 mL of acetic acid (100) in this order, and mixwell.Loganin for component determination Loganin forthin-layer chromatography meeting the following additionalspecifications.1%Absorbance E 1cm (235 nm): 275 - 303 (dried in adesiccator (silica gel) for 24 hours, 5 mg, methanol, 500 mL).Purity Related substances—Dissolve 2 mg of loganin forcomponent determination in 5 mL of the mobile phase, and usethis solution as the sample solution. Pipet 1 mL of this solution,add the mobile phase to make exactly 100 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. Determine each peak area of both solutions bythe automatic integration method: the total area of the peaksother than the peak of loganin is not larger than the peak area ofloganin from the standard solution.Operating conditionsDetector, column, column temperature, mobile phase andflow rate: Proceed as directed in the operating conditions in theAssay (1) under Goshajinkigan Extract.Time span of measurement: About 3 times as long as the retentiontime of loganin.System suitabilitySystem performance and system repeatability: Proceed as directedin the system suitability in the Assay (1) under GoshajinkiganExtract.Test for required detectability: Pipet 1 mL of the standard solution,and add the mobile phase to make exactly 20 mL. Confirmthat the peak area of loganin obtained from 10 µL of thissolution is equivalent to 3.5 to 6.5% of that of loganin from thestandard solution.Lovastatin C 24 H 36 O 5 White crystals or crystalline powder.Soluble in acetonitrile and in methanol, sparingly soluble inethanol (99.5), and practically insoluble in water.Optical rotation [α] 20D: +325 - +340º (50 mg calculatedon the anhydrous basis, acetonitrile, 10 mL, 100 mm).Loss on drying : Not more than 1.0% (1 g, under reducedpressure not exceeding 0.67 kPa, 60ºC, 3 hours).Mebendazole C 16 H 13 N 3 O 3 White powder. Practically insolublein water and in ethanol (95).Mercaptoethanesulfonic acid C 2 H 6 O 3 S 2 Prepared foramino acid analysis or biochemistry.2-Methoxy-4-methylphenol C 8 H 10 O 2 Colorless to paleyellow liquid. Miscible with methanol and with ethanol (99.5),and slightly soluble in water. Congealing point: 3 - 8ºC.Identification Determine the infrared absorption spectrumof 2-methoxy-4-methylphenol as directed in the ATR methodunder Infrared Spectrophotometry : it exhibits absorptionat the wave numbers of about 1511 cm -1 , 1423 cm -1 , 1361 cm -1 ,1268 cm -1 , 1231 cm -1 , 1202 cm -1 , 1148 cm -1 , 1120 cm -1 , 1031cm -1 , 919 cm -1 , 807 cm -1 and 788 cm -1 .Purity Related substances—Perform the test with 0.2 µL of2-methoxy-4-methylphenol as directed under Gas Chromatography according to the following conditions. Determineeach peak by the automatic integration method: the total area ofthe peaks other than the peak of 2-methoxy-4-methylphenol is
Page 1 and 2: SUPPLEMENT IITOTHE JAPANESEPHARMACO
Page 3: The Ministry of Health, Labour andW
Page 7 and 8: PREFACEThe 15th Edition of the Japa
Page 9 and 10: Supplement II, JP XV Preface iii(6)
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Page 13: Supplement II, JP XV Preface viiYuj
Page 17: GENERAL RULES FORCRUDE DRUGSChange
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Crude DrugsApricot Kernelキョウ
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Add the following:GENERAL INFORMATI
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INDEXPage citations refer to the pa
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INDEX IN LATIN NAMEAAchyranthis Rad
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INDEX IN JAPANESEア亜鉛華デ
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Supplement II, JP XV Index in Japan
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