supplement ii to the japanese pharmacopoeia fifteenth edition - NIHS

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2158 Official Monographs Supplement II, JP XVerence Standard, equivalent to 20 mg (potency), dissolve in themobile phase to make exactly 20 mL, and use this solution asthe standard solution. Then, proceed as directed in the Assayunder Lincomycin Hydrochloride Hydrate.Amount [mg (potency)] of lincomycin (C 18 H 34 N 2 O 6 S)= W S × (A T /A S ) × 15W S : Amount [mg (potency)] of Lincomycin HydrochlorideReference StandardContainers and storage Containers—Hermetic containers.Add the following:Losartan PotassiumロサルタンカリウムC 22 H 22 ClKN 6 O: 461.00Monopotassium 5-{[4´-(2-butyl-4-chloro-5-hydroxymethyl-1H-imidazol-1-yl)methyl]biphenyl-2-yl}-1H-tetrazol-1-ide[124750-99-8]Losartan Potassium contains not less than 98.5%and not more than 101.0% of C 22 H 22 ClKN 6 O, calculatedon the anhydrous basis.Description Losartan Potassium occurs as a white crystallinepowder.It is very soluble in water, and freely soluble in methanol andin ethanol (99.5).Identification (1) Determine the absorption spectrum of asolution of Losartan Potassium in methanol (1 in 100000) as directedunder Ultraviolet-visible Spectrophotometry , andcompare the spectrum with the Reference Spectrum or the spectrumof a solution of Losartan Potassium Reference Standardprepared in the same manner as the sample solution: both spectraexhibit similar intensities of absorption at the same wavelengths.(2) Determine the infrared absorption spectrum of LosartanPotassium as directed in the potassium bromide disk methodunder Infrared Spectrophotometry , and compare thespectrum with the Reference Spectrum or the spectrum ofLosartan Potassium Reference Standard: both spectra exhibitsimilar intensities of absorption at the same wave numbers.(3) Losartan Potassium responds to the Qualitative Tests (1) for potassium salt.(4) Perform the test with Losartan Potassium as directed underFlame Coloration Test (2): a green color appears.Purity (1) Heavy metals —Proceed with 2.0 g ofLosartan Potassium according to Method 2, and perform the test.Prepare the control solution with 2.0 mL of Standard Lead Solution(not more than 10 ppm).(2) Related substances—Dissolve 30 mg of Losartan Potassiumin 100 mL of methanol, and use this solution as the samplesolution. Pipet 1 mL of this solution, add methanol to make exactly100 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 according to the following conditions. Determine eachpeak area of both solutions by the automatic integration method:the area of each peak other than the peaks of solvent and losartanobtained from the sample solution is not larger than 1/10times the peak area of losartan from the standard solution, andthe total area of the peaks other than the peak of losartan fromthe sample solution is not larger than 3/10 times the peak area oflosartan from the standard solution.Operating conditions—Detector: An ultraviolet absorption photometer (wavelength:220 nm).Column: A stainless steel column 4 mm in inside diameterand 25 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: Diluted phosphoric acid (1 in 1000).Mobile phase B: Acetonitrile.Flowing of the mobile phase: Control the gradient by mixingthe mobile phases A and B as directed in the following table.Time after injectionof sample(min)Mobile phase A(vol%)Mobile phase B(vol%)0 – 25 75 → 10 25 → 9025 – 35 10 90Flow rate: 1.0 mL per minute.Time span of measurement: 35 minutes after injection of thesample.System suitability—Test for required detectability: Pipet 1 mL of the standard solution,and add methanol to make exactly 10 mL. Confirm thatthe peak area of losartan obtained from 10 µL of this solution isequivalent to 7 to 13% of that of losartan 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 losartan are not less than 10000 and not more than 1.3,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 of losartanis not more than 2.0%.
Supplement II, JP XV Official Monographs 2159(3) Residual solvent—Being specified separately.Water Not more than 0.5% (0.25 g, volumetric titration,direct titration)Assay Weigh accurately about 25 mg each of Losartan Potassiumand Losartan Potassium Reference Standard (separately,determine the water content in the same manner asLosartan Potassium), dissolve separately in methanol to makeexactly 100 mL, and use these solutions as the sample solutionand standard solution, respectively. Perform the test with exactly10 µL each of the sample solution and standard solution as directedunder Liquid Chromatography according to thefollowing conditions, and calculate the peak areas, A T and A S , oflosartan in each solution.Amount (mg) of losartan potassium (C 22 H 22 ClKN 6 O)= W S × (A T /A S )W S : Amount (mg) of Losartan Potassium Reference Standard,calculated on the anhydrous basis.Operating conditions—Detector: An ultraviolet absorption photometer (wavelength:254 nm).Column: A stainless steel column 4 mm in inside diameterand 25 cm in length, packed with octadecylsilanized silica gelfor liquid chromatography (5 µm in particle diameter).Column temperature: A constant temperature of about 35ºC.Mobile phase: A mixture of diluted phosphoric acid (1 in1000) and acetonitrile (3:2)Flow rate: Adjust the flow rate so that the retention time oflosartan is about 6 minutes.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 losartan are not less than 5500 and not more than 1.4,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 losartanis not more than 1.0%.Containers and storage Containers—Tight containers.Add the following:L-Lysine AcetateL‐リジン酢酸塩C 6 H 14 N 2 O 2·C 2 H 4 O 2 : 206.24(2S)-2,6-Diaminohexanoic acid monoacetate[57282-49-2]L-Lysine Acetate, when dried, contains not less than98.5% and not more than 101.0% ofC 6 H 14 N 2 O 2·C 2 H 4 O 2 .Description L-Lysine Acetate occurs as white crystals orcrystalline powder. It has a characteristic odor and a slightlyacid taste.It is very soluble in water, freely soluble in formic acid, andpractically insoluble in ethanol (99.5).It is deliquescent.Identification (1) Determine the infrared absorption spectrumof L-Lysine Acetate as directed in the potassium bromidedisk method under Infrared Spectrophotometry , andcompare the spectrum with the Reference Spectrum: both spectraexhibit similar intensities of absorption at the same wavenumbers.(2) A solution of L-Lysine Acetate (1 in 20) responds to theQualitative Tests (2) for acetate.Optical rotation [α] 20D: +8.5 - +10.0º (after drying,2.5 g, water, 25 mL, 100 mm).pH Dissolve 1.0 g of L-Lysine Acetate in 10 mL ofwater: the pH of the solution is between 6.5 and 7.5.Purity (1) Clarity and color of solution—Dissolve 1.0 g ofL-Lysine Acetate in 10 mL of water: the solution is colorless andclear.(2) Chloride —Perform the test with 0.5 g ofL-Lysine Acetate. Prepare the control solution with 0.30 mL of0.01 mol/L hydrochloric acid VS (not more than 0.021%).(3) Sulfate —Perform the test with 0.6 g of L-LysineAcetate. Prepare the control solution with 0.35 mL of 0.005mol/L sulfuric acid VS (not more than 0.028%).(4) Ammonium —Perform the test with 0.25 g ofL-Lysine Acetate. Prepare the control solution with 5.0 mL ofStandard Ammonium Solution (not more than 0.02%).(5) Heavy metals —Proceed with 1.0 g of L-LysineAcetate according to Method 4, and perform the test. Preparethe control solution with 1.0 mL of Standard Lead Solution (notmore than 10 ppm).(6) Iron —Prepare the test solution with 1.0 g ofL-Lysine Acetate according to Method 1, and perform the testaccording to Method A. Prepare the control solution with 1.0
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SUPPLEMENT IITOTHE JAPANESEPHARMACO
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The Ministry of Health, Labour andW
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PREFACEThe 15th Edition of the Japa
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Supplement II, JP XV Preface iii(6)
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Supplement II, JP XV Preface vStrep
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Supplement II, JP XV Preface viiYuj
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GENERAL RULES FORCRUDE DRUGSChange
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2044 General Tests, Process and App
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Supplement II, JP XV General Tests,
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Official MonographsAdd the followin
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Supplement II, JP XV Official Monog
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Crude DrugsApricot Kernelキョウ
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Supplement II, JP XV Infrared Refer
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Ultraviolet-visible Reference Spect
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2264 Ultraviolet-visible Reference
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Add the following:GENERAL INFORMATI
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Supplement II, JP XV General Inform
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INDEXPage citations refer to the pa
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Supplement II, JP XV Index 2295Pant
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Supplement II, JP XV Index 2297Tabl
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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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