supplement ii to the japanese pharmacopoeia fifteenth edition - NIHS

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2058 General Tests, Process and Apparatus Supplement II, JP XVAdd the following to (1):Reference StandardAciclovirCalcitonin (Salmon)DanazolDiflucortolone ValerateDoxazosin MesilateFludrocortisone AcetateFlutamideGefarnateD-glucuronolactoneIndapamideIpriflavoneLosartan PotassiumPioglitazone HydrochloridePrazosin HydrochlorideProbucolSevofluraneSimvastatinTacrolimusTeprenoneTosufloxacin TosilateTroxipideAdd the following to (2):Reference StandardTazobactamIntended Use*I, AAI, AI, AI, AI, AI, AI, AAI, U, D, AI, AI, AI, AI, AI, AI, AI, AI, AI, AI, U, D, AI, U, D, AIntended Use*I, A9.41 Reagents, Test SolutionsChange the following to read:Benzoylmesaconine hydrochloride for thin-layer chromatographyC 31 H 43 NO 10·HCl·xH 2 O White crystals or crystallinepowder. Soluble in water and in ethanol (99.5) and sparinglysoluble in methanol. Melting point: about 250ºC (withdecomposition).1%Absorbance E 1cm (230 nm): 217 - 231 (5 mg calculatedon the anhydrous basis, methanol, 200 mL)Purity Related substances—Dissolve 1.0 mg of benzoylmesaconinehydrochloride for thin-layer chromatography in exactly1 mL of ethanol (99.5). Perform the test with 5 µL of thissolution as directed in the Identification under Processed AconiteRoot: no spot other than the principal spot at around R f 0.4appears.Bergenin for thin-layer chromatography C 14 H 16 O 9·xH 2 OWhite crystals or crystalline powder. Slightly soluble in ethanol(99.5), very slightly soluble in water, and practically insoluble indiethyl ether.Identification Determine the absorption spectrum of a solutionof bergenin for thin-layer chromatography in methanol (1 in50000) as directed under Ultraviolet-visible Spectrophotometry: it exhibits maxima between 217 nm and 221 nm, andbetween 273 nm, and 277 nm, and a minimum between 241nmand 245 nm.Purity Related substances—Dissolve 1.0 mg of bergenin forthin-layer chromatography in 1 mL of methanol. Perform thetest with 20 µL of this solution as directed in the Identificationunder Mallotus Bark: no spot other than the principal spot at theR f value of about 0.5 appears.(E)-Capsaicin for thin-layer chromatography C 18 H 27 NO 3White crystals, having a strong irritative odor. Very soluble inmethanol, freely soluble in ethanol (95) and in diethyl ether, andpractically insoluble in water.Melting point : 65-70ºC.Purity Related substances—Dissolve 20 mg of(E)-capsaicin for thin-layer chromatography in 2 mL of methanol,and use this solution as the sample solution. Pipet 1 mL ofthis solution, add methanol to make exactly 100 mL, and usethis solution as the standard solution. Perform the test with 10µL each of the sample solution and standard solution as directedin the Identification under Capsicum: any spot other than theprincipal spot at the R f value of about 0.5 from the sample solutionis not more intense than the spot from the standard solution.Add the following:Acemetacin C 21 H 18 ClNO 6 [Same as the namesake monograph]Acemetacin for assay C 21 H 18 ClNO 6 [Same as the monographAcemetacin. When died, it contains no less than 99.5% ofacemetacin (C 21 H 18 ClNO 6 ) meeting the following additionalspecifications.]Purity Dissolve 40 mg of acemetacin for assay in 10 mL ofmethanol, and use this solution as the sample solution. Pipet 1mL of this solution, and add methanol to make exactly 10 mL.Pipet 1 mL of this solution, add methanol to make exactly 20mL, and use this solution as the standard solution. Perform thetest with exactly 10 µL each of the sample solution and standardsolution as directed under Liquid Chromatography accordingto the following conditions. Determine each peak areaof both solutions by the automatic integration method: the areaof each peak other than acemetacin is not larger than 1/2 timesthe peak area of acemetacin obtained from the standard solution,and the total area of the peaks other than the peak of acemetacinis not larger than the peak area of acemetacin from the standardsolution.Operating conditionsDetector, column, column temperature, mobile phase, andflow rate: Proceed as directed in the operating conditions in theAssay under Acemetacin Tablets.Time span of measurement: About 4 times as long as the retentiontime of Acemetacin.System SuitabilityTest for required detectability: Pipet 1 mL of the standard solution,and add methanol to make exactly 20 mL. Confirm thatthe peak area of acemetacin obtained from 10 µL of this solutionis equivalent to 3 to 7% of that of acemetacin from the standardsolution.System performance: Dissolve 75 mg of acemetacin and 75
Supplement II, JP XV General Tests, Process and Apparatus 2059mg of indometacin in 50 mL of methanol. To 4 mL of this solutionadd 1 mL of a solution of hexyl parahydroxybenzoate inmethanol (1 in 250), and add methanol to make 50 mL. Whenthe procedure is run with 10 µL of this solution under the aboveoperating conditions, acemetacin, indometacin and hexyl parahydroxybenzoateare eluted in this order with the resolutionsbetween the peaks of acemetacin and indometacin and betweenthe peaks of indometacin and hexyl parahydroxybenzoate beingnot less than 3, 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 ofacemetacin is not more than 1.5%.Acetic acid buffer solution containing 0.1% bovine serumalbumin Dissolve 0.1 g of bovine serum albumin in sodiumacetate trihydrate solution (1 in 100) to make exactly 100 mL,and adjust the pH to 4.0 with 1 mol/L hydrochloric acid TS.Acetic acid-sodium acetate TS, pH 7.0 Dissolve 4.53 g ofsodium acetate trihydrate in water to make 100 mL, and adjustthe pH to 7.0 with diluted acetic acid (100) (1 in 50).Achyranthes root for thin-layer chromatography Aheat-dried, pulverized root of Achyranthes fauriei Leveillé etVaniot (Amaranthaceae) meeting the following additionalspecifications.Identification (1) To 2 g of pulverized achyranthes root forthin-layer chromatography add 10 mL of water, shake for 10minutes, add 5 mL of 1-butanol, shake for 10 minutes, centrifuge,and use the supernatant liquid as the sample solution.Separately, dissolve 1 mg of chikusetsusaponin IV for thin-layerchromatography in 1 mL of methanol, and use this solution asthe standard solution. Perform the test with these solutions asdirected under Thin-layer Chromatography . Spot 10 µLeach of the sample solution and standard solution on a plate ofsilica gel for thin-layer chromatography. Develop the plate witha mixture of ethyl acetate, water and formic acid (5:1:1) to adistance of about 10 cm, and air-dry the plate. Spray evenly dilutesulfuric acid on the plate, and heat the plate at 105ºC for 10minutes: the standard solution shows a deep purplish red spot ataround R f 0.35, and the sample solution shows spots equivalentto those described below:R f valueAround 0Around 0.1Around 0.2Around 0.25Around 0.35Around 0.45Around 0.5Around 0.75Around 0.9Color and shape of the spotA weak spot, blackA weak spot, strong purplish redA weak, tailing spot, strong purplish redA strong spot, deep purplish redA leading spot, deep purplish redA weak spot, dull yellowA weak spot, grayish purplish redA weak spot, grayish redA weak spot, dull red(2) Perform the test as directed in the operating conditionsunder (1), except using a mixture of 1-propanol, ethyl acetateand water (4:4:3) as the developing solvent: the standard solutionshows a deep purplish red spot at around R f 0.45, and thesample solution shows spots equivalent to those described below:R f valueAround 0.25Around 0.25- 0.3Around 0.35Around 0.4Around 0.42Around 0.45Around 0.65Around 0.7Around 0.85Around 0.95Color and shape of the spotA weak spot, strongly purplish redA leading spot or two strong spots, stronglypurplish redA deep purplish red spotA weak spot, dull redA dark red spotA weak spot, grayish redA weak spot, dull greenish yellowA weak spot, grayish redA weak spot, grayish redA weak spot, dull yellow-redAconitum monoester alkaloids standard TS for componentdetermination Weigh accurately about 20 mg of benzoylmesaconinehydrochloride for component determination(separately, determine the water content), about 10 mg of benzoylhypaconinehydrochloride for component determination(separately, determine the water content) and about 20 mg of14-anisoylaconine hydrochloride for component determination(separately, determine the water content), dissolve in a mixtureof phosphate buffer solution for processed aconite root and tetrahydrofuran(183:17) to make exactly 1000 mL. Perform thetest with 20 µL of this solution as directed in the Purity underbenzoylmesaconine hydrochloride for component determination:the peaks of benzoylmesaconine, benzoylhypaconine and14-anisoylaconine appear with a peak area ratio of about 2:1:2.Alcian blue 8 GX C 56 H 68 Cl 14 CuN 16 S 4 Dark blue-purplepowder.Alcian blue staining solution Dissolve 0.5 g of alcian blue8 GX in 100 mL of diluted acetic acid (100) (3 in 100).C 5 H 4 N 4 O [Same as the namesake mono-Allopurinolgraph.]Allopurinol for assay C 5 H 4 N 4 O [Same as the monographAllopurinol. When dried, it contains not less than 99.0% of allopurinol(C 5 H 4 N 4 O).]Alkaline copper (II) TS Dissolve 20 g of anhydrous sodiumcarbonate in dilute sodium hydroxide TS to make 1000mL, and use this solution as solution A. Dissolve 0.5 g of copper(II) sulfate pentahydrate in potassium sodium tartarate tetrahydratesolution (1 in 100) to make 100 mL, and use this solutionas solution B. To 50 mL of solution A add 1 mL of solution B.Prepare before use.Alkaline phosphatase Obtained from bovine small intestine,a white to grayish white or yellow-brown, freeze-driedpowder having no odor.Alkaline phosphatase contains not less than 1 unit per mg andno salts. One unit of alkaline phosphatase indicates an amountof the enzyme which produces 1 µmol of 4-nitrophenol in 1
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)
Page 11 and 12: Supplement II, JP XV Preface vStrep
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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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