O‹cial Monographs

460 Pages·2007·8.49 MB·English

O‹cial Monographs
AsolutionofAcebutololHydrochloride(1in20)showsno
opticalrotation.
Absorptive Ointment
Identiˆcation (1) Determinetheabsorptionspectrumofa
solution of Acebutolol Hydrochloride in 0.01mol/L
吸水軟膏
hydrochloricacidTS(1in100,000)asdirectedunderUltrav-
iolet-visible Spectrophotometry <2.24>, and compare the
Method of preparation spectrum with the Reference Spectrum: both spectra exhibit
similarintensitiesofabsorption at the same wavelengths.
White Petrolatum 400g
(2) Determine the infrared absorption spectrum of
Cetanol 100g
Acebutolol Hydrochloride, previously dried, as directed in
White Beeswax 50g
the potassium bromide disk method under Infrared
Sorbitan Sesquioleate 50g
Spectrophotometry <2.25>, and compare the spectrum with
Lauromacrogol 5g
theReferenceSpectrum:bothspectraexhibitsimilarintensi-
EthylParahydroxybenzoateor Methyl
ties ofabsorption atthe same wavenumbers.
Parahydroxybenzoate 1g
(3) A solution of Acebutolol Hydrochloride (1 in 100)
ButylParahydroxybenzoateor Propyl
responds to the Qualitative Tests <1.09>forchloride.
Parahydroxybenzoate 1g
Puriˆed Water a su‹cientquantity Melting point <2.60> 141–1459C
To make 1000g Purity (1) Heavy metals <1.07>—Proceed with 1.0g of
Acebutolol Hydrochloride according to Method 2, and per-
MeltWhitePetroleum,Cetanol,WhiteBeeswax,Sorbitan
form the test. Prepare the control solution with 1.0mL of
SesquioleateandLauromacrogolbyheatingonawaterbath,
Standard Lead Solution (notmore than 10ppm).
mix and maintain at about 759C. Add Methyl Parahydrox-
(2) Arsenic <1.11>—Prepare the test solution with 1.0g
ybenzoate or Ethyl Parahydroxybenzoate and Propyl Para-
of Acebutolol Hydrochloride according to Method 3, and
hydroxybenzoate or Butyl Parahydroxybenzoate to Puriˆed
perform the test (not more than 2ppm).
Water, dissolve by warming at 809C. Combine both solu-
(3) Related substances—Dissolve 40mg of Acebutolol
tions,mixtomakeemulsion,cool,andstirthoroughlyuntil
Hydrochloridein2mLofmethanol,andusethissolutionas
itcongeals.
thesamplesolution.Pipet1mLofthesamplesolution,add
Description Absorptive Ointment is white in color and is methanol to make exactly 25mL, and pipet 1mL of this
lustrous. Ithas a slightly characteristic odor. solution,addmethanoltomakeexactly20mL,andusethis
solutionasthestandardsolution.Performthetestwiththese
Containers and storage Containers—Tightcontainers.
solutions as directed under Thin-layer Chromatography
<2.03>. Spot 5mL each of the sample solution and standard
Acebutolol Hydrochloride solution on a plate of silica gel for thin-layer chro-
matography. Develop the plate with the upper layer of a
mixtureofwater,1-butanolandaceticacid(100)(5:4:1)toa
アセブトロール塩酸塩
distance of about 10cm, and air-dry the plate. Examine
under ultraviolet light (main wavelength:365nm):the spots
otherthantheprincipalspotfromthesamplesolutionarenot
more intense than the spotfrom the standard solution.
Loss on drying <2.41> Not more than 1.0z (0.5g, 1059C,
3 hours).
C H NO.HCl: 372.89 Residue on ignition <2.44> Not morethan 0.2z(1g).
18 28 2 4
N-s3-Acetyl-4-[(2RS)-2-hydroxy-
Assay Weigh accurately about 0.25g of Acebutolol
3-(1-methylethyl)aminopropyloxy]phenyltbutanamide
Hydrochloride,previouslydried,dissolvein20mLofacetic
monohydrochloride [34381-68-5]
acid(100),add80mLofaceticanhydride,andtitrate<2.50>
with0.1molWLperchloricacidVS(potentiometrictitration).
AcebutololHydrochloride,whendried,containsnot
Performablankdetermination,andmakeanynecessarycor-
less than 98.0z and not more than 102.0z of
rection.
C H N O .HCl.
18 28 2 4
Each mL of 0.1molWL perchloric acid VS
Description Acebutolol Hydrochloride occurs as white to
＝37.29mg ofC H N O.HCl
pale yellowish white crystalsor crystalline powder. 18 28 2 4
It is freely soluble in water, in methanol, in ethanol (95) Containers and storage Containers—Well-closed contain-
and in acetic acid (100), and practically insoluble in diethyl ers.
ether.
226655
226666 Aceglutamide Aluminum / O‹cial Monographs JP XV
ppm).
(2) Arsenic <1.11>—Prepare the test solution with 1.0g
Aceglutamide Aluminum
of Aceglutamide Aluminum according to Method 1, and
perform the test (not more than 2ppm).
アセグルタミドアルミニウム (3) Relatedsubstances—Dissolve0.10gofAceglutamide
Aluminuminthemobilephasetomakeexactly100mL,and
use this solution as the sample solution. Pipet 1mL of the
sample solution, add the mobile phase to make exactly 100
mL, and use this solution as the standard solution (1).
Separately, dissolve 10mg of 2-acetamidoglutarimide in the
mobile phase to make exactly 100mL. Pipet 3mL of this
solution,addthemobilephasetomakeexactly100mL,and
usethissolutionasthestandardsolution(2).Performthetest
C H AlN O : 1084.84
35 59 3 10 24 withexactly20mLeachofthesamplesolutionandstandard
Pentakis[(2S)-2-acetylamino-4-
solutions (1) and (2) as directed under Liquid Chro-
carbamoylbutanoato]tetrahydroxotrialuminium
matography <2.01> according to the following conditions,
[12607-92-0]
and determine each peak area by the automatic integration
method: the peak area of 2-acetamidoglutarimide from the
Aceglutamide Aluminum contains not less than
samplesolutionisnotmorethanthatfromthestandardsolu-
85.4z and not more than 87.6z of aceglutamide
tion (2), the peak areas other than aceglutamide and 2-
(C H N O : 188.18), and not less than 7.0z and not
7 12 2 4 acetamidoglutarimidefromthesamplesolutionarenotmore
more than 8.0z of aluminum (Al: 26.98), calculated
than 3/10 times the peak area of aceglutamide from the
on the dried basis.
standard solution (1), and the total of the peak areas other
Description Aceglutamide Aluminum occurs as a white than aceglutamide and 2-acetamidoglutarimide from the
powder, having astringentbittertaste. sample solution is not more than the peak area of
It is freely soluble in water, and practically insoluble in aceglutamidefrom the standard solution (1).
ethanol(99.5). Operating conditions—
Itdissolves in dilute hydrochloric acid. Detector,column,columntemperature,mobilephase,and
Itis hygroscopic. ‰ow rate: Proceed as directed in the operating conditionsin
the Assay.
Identiˆcation (1) Dissolve 0.03g each of Aceglutamide
Time span of measurement: About 3 times as long as the
AluminumandAceglutamideReferenceStandardin5mLof
retention timeofaceglutamide.
water, and use these solutions as the sample solution and
System suitability—
standard solution. Perform the test with these solutions as
Test for required detection: To exactly 5mL of the
directedunderThin-layerChromatography<2.03>.Spot5mL
standardsolution(1)addthemobilephasetomakeexactly50
eachofthesamplesolutionandstandardsolutiononaplate
mL. Conˆrm that the peak area of aceglutamide obtained
ofcelluloseforthin-layerchromatography.Developtheplate
from20mLofthissolutionisequivalentto7to13zofthat
with a mixture of 1-propanol, water and acetic acid (100)
of aceglutamide obtained from 20mL of the standard solu-
(16:8:1) to a distance of about 10cm, and air-dry the plate.
tion.
Sprayevenlyasolutionofbromocresolgreeninethanol(95)
System performance: Proceed as directed in the system
(1in1000),thensprayevenlydilutedammoniasolution(28)
suitability in the Assay (1).
(1 in 100): the spots from the sample solution and the stan-
Systemrepeatability:Whenthetestisrepeated6timeswith
dardsolutionshowalightyellowandhavethesameRfvalue.
20mLofthestandardsolution(1)undertheaboveoperating
(2) A solution of Aceglutamide Aluminum in dilute
conditions,therelativestandarddeviationofthepeakareaof
hydrochloric acid(1 in 20)respondstotheQualitativeTests
aceglutamideis notmore than 2.0z.
<1.09>for aluminum salt.
Loss on drying <2.41> Not more than 5.0z (1g, 1309C,
Opticalrotation<2.49> [a]20:－5.5–－7.59(2gcalculated
D 5hours).
on the dried basis,water,50mL,100mm).
Assay (1) Aceglutamide—Weigh accurately about 50mg
Purity (1) Heavy metals < 1.07 > —Put 1.0g of
ofAceglutamideAluminum,dissolveinasuitableamountof
Aceglutamide Aluminum in a porcelain crucible, cover the
themobilephase,addexactly10mLoftheinternalstandard
crucibleloosely,andheatgentlytocarbonize.Aftercooling,
solution and the mobile phase to make 50mL, and use this
add2mLofnitricacidand1mLofsulfuricacid,heatgently
solutionasthesamplesolution.Separately,weighaccurately
untilthewhitefumesnomoreevolve,andheattoincinerate
about 45mg of Aceglutamide Reference Standard, dissolve
at500to6009C.Iftheincinerationisnotaccomplished,add
inasuitableamountofthemobilephase,addexactly10mL
2mL of nitric acid and 1mL of sulfuric acid, heat in the
of the internal standard solution and the mobile phase to
samemannerasabove,thenigniteat500to6009Ctoinciner-
make50mL,andusethis solutionasthe standard solution.
ate. After cooling, add 2mL of hydrochloric acid, proceed
Performthetestwith10mLeachofthesamplesolutionand
with this solution according to Method 2, and perform the
standardsolutionasdirectedunderLiquidChromatography
test. Prepare the control solution as follows: proceed in the
<2.01>according to the following conditions, and determine
samemannerasthepreparationofthetestsolutionwiththe
the ratios, Q and Q , of the peak area of aceglutamide to
same amount of the reagents, and add 2.0mL of Standard T S
that of theinternal standard.
Lead Solution and water to make 50mL (not more than 20
Amount (mg) of aceglutamide (C H N O)
7 12 2 4
JP XV O‹cial Monographs / Acetaminophen 226677
＝W ×(Q /Q ) crystalline powder.
S T S
Itisfreelysolubleinmethanolandinethanol(95),sparing-
W : Amount(mg)ofAceglutamide Reference Standard
S lysolubleinwater,andveryslightly,solubleindiethylether.
Internal standard solution—A solution of thymine in It dissolves in sodium hydroxide TS.
methanol(1 in 4000).
Identiˆcation Determinetheinfraredabsorptionspectraof
Operating conditions—
Acetaminophen,previouslydried,asdirectedinthepotassi-
Detector: An ultraviolet absorption photometer (wave-
umbromidediskmethodunderInfraredSpectrophotometry
length:210nm).
<2.25>, and compare the spectrum with the Reference Spec-
Column: A stainless steel column 4.6mm in inside
trum or the spectrum of dried Acetaminophen Reference
diameterand25cminlength,packedwithoctadecylsilanized
Standard: both spectra exhibit similar intensities of absorp-
silica gel for liquid chromatography (5mm in particle
tion at the samewave numbers.
diameter).
Column temperature: A constant temperature of about Melting point <2.60> 169–1729C
259C.
Purity (1) Chloride < 1.03 > —Dissolve 4.0g of
Mobile phase: A mixture of diluted perchloric acid (1 in
Acetaminophen in 100mL of water by heating, cool with
1000) and methanol(99:1).
shaking in ice water, allow to stand until ordinary tempera-
Flowrate:Adjustthe‰owratesothattheretentiontimeof
tureisattained,addwatertomake100mL,andˆlter.To25
aceglutamideis about5minutes.
mLoftheˆltrateadd6mLofdilutenitricacidandwaterto
Systemsuitability—
make50mL,andperformthetestusing thissolution asthe
System performance: When the procedure is run with
test solution. Prepare the control solution with 0.40mL of
10mL of the standard solution under the above operating
0.01molWL hydrochloric acid VS (not more than 0.014z).
conditions,aceglutamideandtheinternalstandardareeluted
(2) Sulfate <1.14>—To 25mL of the ˆltrate obtained in
in this order with the resolution between these peaks being
(1)add 1mL of dilute hydrochloric acid and water to make
notless than 11.
50mL, and perform the test using this solution as the test
Systemrepeatability:Whenthetestisrepeated6timeswith
solution.Preparethecontrolsolutionwith0.40mLof0.005
10mL of the standard solution under the above operating
molWL sulfuric acid VS (not more than 0.019z).
conditions,therelativestandarddeviationoftheratiosofthe
(3) Heavy metals <1.07>—Proceed with 2.0g of
peakareaofaceglutamidetothatoftheinternalstandardis
Acetaminophen according to Method 4, and perform the
notmore than 1.0z.
test. Prepare the control solution with 2.0mL of Standard
(2) Aluminum—Weigh accurately about 3.0g of
Lead Solution (not more than 10ppm).
Aceglutamide Aluminum, add 20mL of dilute hydrochloric
(4) Arsenic <1.11>—Prepare the test solution with 1.0g
acid,andheatonawaterbathfor60minutes.Aftercooling,
of Acetaminophen according to Method 3,and perform the
addwatertomakeexactly200mL.Pipet20mLofthissolu-
test(not more than 2ppm).
tion,addexactly25mLof0.05mol/Ldisodiumdihydrogen
(5) Related substances—Dissolve 50mg of
ethylenediamine tetraacetate VS and 20mL of acetic acid-
Acetaminophenin1mLofmethanol,addthemobilephase-
ammonium acetate buŠer solution, pH4.8, and boil for
tomake50mL,andusethissolutionasthesamplesolution.
5 minutes. After cooling, add 50mL of ethanol (95), and
Pipet 1mL of the sample solution, add the mobile phase to
titrate<2.50>with0.05mol/LzincacetateVSuntilthecolor
make exactly 200mL, and use this solution as the standard
ofthesolutionchangesfromlightdarkgreentolightred(in-
solution.Performthetestwithexactly10mLeachofthesam-
dicator:2mLofdithizoneTS).Performablankdetermina-
ple solution and standard solution as directed under Liquid
tion in the same manner.
Chromatography <2.01> according to the following condi-
EachmL of 0.05mol/L disodium dihydrogen tions. Determine each peak area of both solutions by the
ethylenediamine tetraacetateVS＝1.349mg ofAl automatic integration method: the total area of all peaks
otherthanthepeakareaofacetaminophenfromthesample
Containers and storage Containers—Tightcontainers.
solution is not larger than the peak area of acetaminophen
from thestandard solution.
Acetaminophen Operating conditions—
Detector: An ultraviolet absorption photometer
(wavelength: 225nm).
Paracetamol
Column: A stainless steel column about 4mm in inside
diameterand about 15cm in length,packed with octadecyl-
アセトアミノフェン
silanizedsilicagelforliquidchromatography(5mminparti-
cle diameter).
Column temperature: A constant temperature of about
409C.
Mobile phase: A mixture of 0.05molWL potassium di-
C HNO :151.16
8 9 2
hydrogenphosphate, pH 4.7 and methanol(4:1)
N-(4-Hydroxyphenyl)acetamide [103-90-2]
Flowrate:Adjustthe‰owratesothattheretentiontimeof
acetaminophen is about 5 minutes.
Acetaminophen, when dried, contains not less than
Selection of column: Dissolve 0.01g each of
98.0z of C H NO .
8 9 2 Acetaminophen and p-aminophenol in 1mL of methanol,
Description Acetaminophen occurs as white crystals or addthemobilephasetomake50mL,to1mLofthissolution
226688 Acetazolamide / O‹cial Monographs JP XV
addthemobilephasetomake10mL.Proceedwith10mLof (2) To 0.02g of Acetazolamide add 2mL of dilute
this solution under the above operating conditions, and hydrochloricacid,boilfor10minutes,cool,andadd8mLof
calculate the resolution. Use a column giving elution of p- water: this solution responds to the Qualitative Tests <1.09>
aminophenol and acetaminophen in this order with the for primary aromatic amines.
resolution between these peaksbeing not lessthan 7. (3) To 0.2g of Acetazolamide add 0.5g of granulated
Detection sensitivity: Adjust the detection sensitivity so zinc and 5mL of diluted hydrochloric acid (1 in 2): the gas
thatthepeakheightofacetaminophenobtainedfrom10mL evolved darkens moistened lead (II) acetatepaper.
of the standard solution is about 15zofthefullscale.
Purity (1) Clarityandcolorofsolution—Dissolve1.0gof
Time span of measurement: About 6 times as long as the
Acetazolamide in 10mL of sodium hydroxide TS: the
retention time of acetaminophen beginningafterthesolvent
solution is clearand colorless to pale yellow.
peak.
(2) Chloride <1.03>—To 1.5g of Acetazolamide add 75
Loss on drying <2.41> Not more than 0.3z (0.5g, 1059C, mL of water, and warm at 709C for 20 minutes with
2 hours). occasional shaking. After cooling, ˆlter, and to 25mL of
theˆltrateadd6mL ofdilutenitricacid andwaterto make
Residueon ignition <2.44> Not more than 0.1z(1g).
50mL. Perform the test using this solution as the test solu-
Assay Weigh accurately about 20mg each of tion.Preparethecontrolsolutionwith0.20mLof0.01molW
Acetaminophen and Acetaminophen Reference Standard, L hydrochloricacid VS (notmore than 0.014z).
previously dried, dissolve in 2mL of methanol, and add (3) Sulfate <1.14>—To 25mL of the ˆltrate obtained in
water to make exactly 100mL. Pipet 3mL each of these (2)add 1mL of dilute hydrochloric acid and water to make
solutions, add water to make exactly 100mL, and use these 50mL. Perform the test using this solution as the test solu-
solutions as the sample solution and standard solution, tion.Preparethecontrolsolutionwith0.40mLof0.005mol
respectively. Determine the absorbances, A and A , of the WL sulfuric acid VS (notmore than 0.038z).
T S
sample solution and standard solution at the wavelength of (4) Heavy metals <1.07>—Proceed with 1.0g of
maximum absorption at about 244nm as directed under AcetazolamideaccordingtoMethod2,andperformthetest.
Ultraviolet-visible Spectrophotometry <2.24>,using water as Prepare the control solution with 2.0mL of Standard Lead
the blank. Solution (not more than 20ppm).
(5) Silver-reducing substances—Wet 5g of
Amount(mg)of CHNO ＝W ×(A /A )
8 9 2 S T S Acetazolamidewith5mLofaldehyde-freeethanol,andadd
W :Amount(mg)of Acetaminophen ReferenceStandard 125mL of water, 10mL of nitric acid and exactly 5mL of
S
0.1molWLsilvernitrateVS.Stirfor30minutesbyprotecting
Containers and storage Containers—Tightcontainers.
from light, ˆlter through a glass ˆlter (G3), and wash the
Storage—Light-resistant.
residueontheglassˆlterwithtwo10-mLportionsofwater.
Combine the ˆltrate with the washings, to the solution add
Acetazolamide 5mLofferricammoniumsulfaceTS,andtitrate<2.50>with
0.1molWL ammoniumthiocyanate VS:notless than 4.8mL
of 0.1molWL ammonium thiocyanate VS is consumed.
アセタゾラミド
Loss on drying <2.41> Not more than 0.5z (0.5g, 1059C,
3 hours).
Residue on ignition <2.44> Not morethan 0.1z(0.5g).
Assay Weigh accurately about 0.15g of Acetazolamide,
and dissolve in 400mL of waterin a waterbath byheating.
After cooling, add water to make exactly 1000mL. Pipet
C4H6N4O3S2:222.25 5mL of the solution, add 10mL of 1molWL hydrochloric
N-(5-Sulfamoyl-1,3,4-thiadiazol-2-yl)acetamide [59-66-5]
acidTS,andthenaddwatertomakeexactly100mL.Deter-
minetheabsorbanceAofthissolutionatthewavelengthof
Acetazolamidecontainsnotlessthan98.0zandnot
maximum absorption at about 265nm as directed under
more than 102.0z of C H N O S , calculated on the
4 6 4 3 2 Ultraviolet-visible Spectrophotometry <2.24>.
dried basis.
Description Acetazolamide occurs as a white to pale Amount(mg)of C4H6N4O3S2＝(A/474)×200,000
yellowishwhite,crystallinepowder.Itisodorless,andhasa
slight bitter taste. Containers and storage Containers—Well-closed contain-
Itisslightlysolubleinethanol(95),veryslightlysolublein ers.
water, and practically insolublein diethyl ether. Storage—Light-resistant.
Melting point: about2559C (with decomposition).
Identiˆcation (1) To0.1gofAcetazolamideadd5mLof Acetic Acid
sodiumhydroxideTS,thenadd5mLofasolutionof0.1gof
hydroxylammonium chloride and 0.05g of copper (II)
酢酸
sulfate pentahydrate in 10mL of water:a lightyellow color
develops.Thenheatthissolutionfor5minutes:adeepyellow
coloris produced gradually.
Acetic Acid contains not less than 30.0wWvz and
JP XV O‹cial Monographs / Acetohexamide 226699
not more than 32.0wWvz of C H O : 60.05.
2 4 2 Purity (1) Chloride—To 10mL of Glacial Acetic Acid
Description AceticAcidisaclear,colorlessliquid.Ithasa addwatertomake100mL,andusethissolutionasthesam-
pungent, characteristicodor and an acid taste. plesolution.To10mLofthesamplesolutionadd5dropsof
It is miscible with water, with ethanol (95) and with silvernitrate TS:no opalescence isproduced.
glycerin. (2) Sulfate—To10mLofthesamplesolutionobtainedin
Speciˆc gravity d20: about1.04 (1) add 1mL of barium chloride TS: no turbidity is
20
produced.
Identiˆcation AceticAcidchangesbluelitmuspapertored,
(3) Heavy metals <1.07>—Evaporate 2.0mL of Glacial
and responds to the QualitativeTests <1.09>foracetate.
AceticAcidonawaterbathtodryness.Dissolvetheresidue
Purity (1) Chloride—To20mLofAceticAcidadd40mL in 2mL ofdiluteaceticacid and waterto make 50mL, and
ofwater,andusethissolutionasthesamplesolution.To10 performthetestusingthissolutionasthetestsolution.Pre-
mLofthesamplesolutionadd5dropsofsilvernitrateTS:no parethecontrolsolutionwith2.0mLofStandardLeadSolu-
opalescence is produced. tionbyadding2.0mLofdiluteaceticacidandwatertomake
(2) Sulfate—To10mLofthesamplesolutionobtainedin 50mL (notmore than 10ppm).
(1) add 1mL of barium chloride TS: no turbidity is (4) Potassium permanganate-reducing substances—To
produced. 20mLofthesamplesolutionobtainedin(1)add0.10mLof
(3) Heavy metals <1.07>—Evaporate 10mL of Acetic 0.1molWL potassium permanganate VS: the red color does
Acidonawaterbathtodryness,andtotheresidueadd2mL notdisappear within 30minutes.
of diluteacetic acid and waterto make 50mL. Perform the (5) Non-volatile residue—Evaporate 10mL of Glacial
testwiththissolutionasthetestsolution.Preparethecontrol AceticAcidonawaterbathtodryness,anddryat1059Cfor
solutionwith3.0mLofStandardLeadSolutionbyadding2 1hour: the mass ofthe residueis notmore than 1.0mg.
mLofdiluteaceticacidandwatertomake50mL(notmore
Assay Place10mLofwaterinaglass-stoppered‰ask,and
than 3ppm).
weigh accurately. Add about 1.5g of Glacial Acetic Acid,
(4) Potassium permanganate-reducing substances—To
weighaccuratelyagain,thenadd30mLofwater,andtitrate
20mLofthesamplesolutionobtainedin(1)add0.02molWL
<2.50>with1molWLsodiumhydroxideVS(indicator:2drops
potassium permanganate VS: the red color does not disap-
of phenolphthalein TS).
pearwithin 30 minutes.
(5) Non-volatile residue—Evaporate 30mL of Acetic Each mL of1molWL sodium hydroxide VS
Acidonawaterbathtodryness,anddryat1059Cfor1hour: ＝60.05mg of C HO
2 4 2
the massofthe residueis notmore than 1.0mg.
Containers and storage Containers—Tightcontainers.
Assay Measureexactly5mLofAceticAcid,add30mLof
water,andtitrate<2.50>with1molWLsodiumhydroxideVS
Acetohexamide
(indicator:2drops of phenolphthalein TS).
Each mL of1molWL sodium hydroxide VS
アセトヘキサミド
＝60.05mg of C HO
2 4 2
Containers and storage Containers—Tightcontainers.
Glacial Acetic Acid
氷酢酸
C H NOS:324.40
15 20 2 4
4-Acetyl-N-(cyclohexylcarbamoyl)benzenesulfonamide
C HO :60.05 [968-81-0]
2 4 2
Acetic acid [64-19-7]
Acetohexamide, when dried, contains not less than
Glacial Acetic Acid contains not less than 99.0z of 98.0z and not more than 101.0z of C15H20N2O4S.
C H O .
2 4 2 Description Acetohexamide occurs as a white to yellowish
Description GlacialAceticAcidisaclear,colorless,volatile whitepowder.
liquid, or colorless or white, crystalline masses. It has a It is freely soluble in N,N-dimethylformamide, sparingly
pungent, characteristicodor. solubleinacetone,slightlysolubleinmethanolandinethanol
Itismisciblewithwater,withethanol(95)andwithdiethyl (99.5), and practically insoluble in water.
ether. Melting point: about 1859C (with decomposition).
Boiling point:about 1189C
Identiˆcation (1) Dissolve0.10gofAcetohexamidein100
Speciˆc gravity d20: about1.049
20 mLofmethanol.To 5mLofthesolutionadd 20mL of0.5
Identiˆcation A solution of Glacial Acetic Acid (1 in 3) mol/LhydrochloricacidTSand75mLofmethanol,anduse
changes blue litmus paper to red, and responds to the thesolutionasthesamplesolution(1).Determinetheabsorp-
Qualitative Tests <1.09>for acetate. tion spectrum of the sample solution (1) as directed under
Ultraviolet-visible Spectrophotometry <2.24>, using
Congealing point<2.42> Not below 14.59C.
methanol as the blank, and compare the spectrum with the
227700 Acetohexamide / O‹cial Monographs JP XV
ReferenceSpectrum1:bothspectraexhibitsimilarintensities 2109C.
ofabsorptionatthesamewavelengths.Separately,toexactly Carriergas:Helium
10mL of the sample solution (1) add methanol to make ex- Flowrate:Adjustthe‰owratesothattheretentiontimeof
actly50mL,andusethesolutionasthesamplesolution(2). cyclohexylamine is about 4 minutes.
Determinetheabsorptionspectrumofthesamplesolution(2) Splitratio:1:1
as directed under Ultraviolet-visible Spectrophotometry System suitability—
<2.24>, using methanol as the blank, and compare the spec- Systemperformance:Whentheprocedureisrunwith2mL
trum with the Reference Spectrum 2: both spectra exhibit of the standard solution under the above operating
similarintensitiesof absorption at the samewavelengths. conditions, the number of theoretical plates of the peak of
(2) Determine the infrared absorption spectrum of cyclohexylamine is notless than 8000.
Acetohexamide, previously dried, as directed in the potassi- Systemrepeatability:Whenthetestisrepeated6timeswith
umbromidediskmethodunderInfraredSpectrophotometry 2mLofthestandardsolutionundertheaboveoperatingcon-
<2.25>, and compare the spectrum with the Reference Spec- ditions,therelativestandarddeviationofthepeakareaofcy-
trum:bothspectraexhibitsimilarintensitiesofabsorptionat clohexylamine is not morethan 5z.
the samewave numbers. (ii) Dicyclohexylurea—Dissolve exactly 1.0g of Aceto-
hexamide in exactly 10mL of 0.5mol/L sodium hydroxide
Purity (1) Chloride <1.03>—Dissolve 1.5g of Acetohex-
TS,addexactly20mLofmethanol,shake,thenaddexactly5
amidein40mLofN,N-dimethylformamide,add6mLofdi-
mL of diluted hydrochloric acid (1 in 10), shake vigorously
lutenitricacidandN,N-dimethylformamidetomake50mL.
for 15 minutes, and centrifuge. Filter 10mL or more of the
Performthetestusingthissolutionasthetestsolution.Pre-
supernatant liquid through a membrane ˆlter with pore size
parethecontrolsolutionasfollows:to0.45mLof0.01molW
of not larger than 0.5mm. Discard the ˆrst 5mL of the
L hydrochloric acid VS add 6mL of dilute nitric acid and
ˆltrate,andusethesubsequentˆltrateasthesamplesolution.
N,N-dimethylformamide to make 50mL (not more than
Separately, dissolve exactly 50mg of dicyclohexylurea in
0.011z).
methanol to make exactly 100mL. Pipet 2mL of this solu-
(2) Sulfate <1.14>—Dissolve 2.0g of Acetohexamide in
tion,andaddmethanoltomakeexactly100mL.Pipet20mL
40mL of N,N-dimethylformamide, and add 1mL of dilute
of this solution, add exactly 10mL of 0.5mol/L sodium
hydrochloric acid and N,N-dimethylformamide to make 50
hydroxide TS, shake, then add exactly 5mL of diluted
mL.Performthetestusingthissolutionasthetestsolution.
hydrochloricacid(1in10),shake,andusethissolutionasthe
Preparethecontrolsolutionasfollows:to0.40mLof0.005
standard solution. Perform the test with exactly 50mL each
molWL sulfuric acid VS add 1mL of dilute hydrochloric
ofthesamplesolutionandstandardsolutionasdirectedun-
acidandN,N-dimethylformamidetomake50mL(notmore
der Liquid Chromatography <2.01> according to the follow-
than 0.010z).
ing conditions, and determine the peak area of dicyclohex-
(3) Heavy metals <1.07>—Proceed with 1.0g of Aceto-
ylureabytheautomaticintegrationmethod:thepeakareaof
hexamideaccordingtoMethod2,andperformthetest.Pre-
dicyclohexylureaisnotmorethanthatwiththestandardso-
pare the control solution with 2.0mL of Standard Lead
lution.
Solution (not more than 20ppm).
Operating conditions—
(4) Relatedsubstances(i)Cyclohexylamine—Dissolveex-
Detector: An ultraviolet absorption photometer
actly1.0gofAcetohexamidein exactly30mLof0.5mol/L
(wavelength: 210nm).
sodium hydroxide TS, add exactly 5mL of hexane, shake
Column: A stainless steel column 4.6mm in inside
vigorouslyfor60minutes,allowtostandfor5minutes,and
diameterand25cminlength,packedwithoctadecylsilanized
use the upper layer as the sample solution. Separately, dis-
silica gel for liquid chromatography (5mm in particle di-
solveexactly50mgofcyclohexylaminein0.5mol/Lsodium
ameter).
hydroxideTStomakeexactly50mL.Pipet2mLofthissolu-
Column temperature: A constant temperature of about
tion, and add 0.5mol/L sodium hydroxide TS to make ex-
259C.
actly300mL.Pipet30mLofthissolution,addexactly5mL
Mobilephase:Dissolve0.5gofsodiumhydroxidein1000
of hexane, shake vigorously for 60 minutes, allow to stand
mL of 0.05mol/L sodium dihydrogen phosphate TS, and
for 5 minutes,and use the upper layer as the standard solu-
adjust the pH to 6.5 with 0.5mol/L sodium hydroxide TS.
tion. Perform the test with exactly 2mL each of the sample
To 500mL ofthis solution add 500mL of acetonitrile.
solution and standard solution as directed under Gas Chro-
Flowrate:Adjustthe‰owratesothattheretentiontimeof
matography <2.02> according to the following conditions,
dicyclohexylurea is about10 minutes.
anddeterminethepeakareaofcyclohexylaminebytheauto-
System suitability—
maticintegrationmethod:thepeakareaofcyclohexylamine
System performance: When the procedure is run with
isnot morethan that with thestandard solution.
50mL of the standard solution under the above operating
Operating conditions—
conditions, the number of theoretical plates of the peak of
Detector: Ahydrogen ‰ame-ionization detector.
dicyclohexylurea is notless than 10,000.
Column:Afused-silicacolumn0.53mmininsidediameter
Systemrepeatability:Whenthetestisrepeated6timeswith
and30minlength,coatedtheinnersurfacewithmethylsili-
50mL of the standard solution under the above operating
cone polymer for gaschromatography 1.5mm in thickness.
conditions,therelativestandarddeviationofthepeakareaof
Column temperature: A constant temperature of about
dicyclohexylurea is notmore than 2.0z.
909C.
(iii) Other related substances—Dissolve 0.10g of Aceto-
Injection port temperature: A constant temperature of
hexamide in 10mL of acetone, and use this solution as the
about1509C.
samplesolution.Pipet1mLofthesamplesolution,andadd
Detector temperature: A constant temperature of about
acetone to makeexactly 20mL. Pipettwo 1mL portions of
JP XV O‹cial Monographs / Acetylcholine Chloride for Injection 227711
thissolution,addacetonetomakeexactly10mLand25mL, It isextremely hygroscopic.
respectively,andusethesesolutionsasthestandardsolution
Identiˆcation (1) Determine the infrared absorption
(1)andthestandardsolution(2).Performthetestwiththese
spectrumofAcetylcholineChlorideforInjection,previously
solutions as directed under Thin-layer Chromatography
dried, as directed in the potassium bromide disk method
<2.03>.Spot10mLeachofthesamplesolutionandstandard
under Infrared Spectrophotometry <2.25>, and compare the
solutions (1) and (2) on a plate of silica gel with ‰uorescent
spectrum with the Reference Spectrum: both spectra exhibit
indicator for thin-layer chromatography. Develop the plate
similarintensitiesofabsorption at the same wave numbers.
withamixtureofethylacetate,methanol,ammoniasolution
(2) A solution of Acetylcholine Chloride for Injection
(28)andcyclohexane(6:2:1:1)toa distanceofabout10cm,
(1in10)respondstotheQualitativeTests<1.09>(2)forchlo-
and air-dry the plate. Examine under ultraviolet light (main
ride.
wavelength:254nm):thespotsotherthantheprincipalspot
fromthesamplesolutionarenotmoreintensethanspotfrom Melting point <2.60> 149–1529C. Seal Acetylcholine
thestandardsolution(1),andthenumberofthemwhichare Chloride for Injection in a capillary tube for melting point
moreintense than the spotfrom the standard solution (2)is immediatelyafterdryingbothofthesampleandthetubeat
notmore than 4. 1059C for 3 hours, and determine the melting point.
Loss on drying <2.41> Not more than 1.0z (1g, 1059C, Purity (1) Clarityandcolorofsolution—Dissolve1.0gof
4 hours). Acetylcholine Chloride for Injection in 10mL of water: the
solution is clearand colorless.
Residueon ignition <2.44> Not more than 0.1z(1g).
(2) Acidity—Dissolve 0.10g of Acetylcholine Chloride
Assay Weigh accurately about 0.3g of Acetohexamide, for Injection in 10mL of freshly boiled and cooled water,
previously dried, dissolve in 30mL of N,N-dimethylfor- and add 1 drop of bromothymol blue TS, and 0.30mL of
mamide,add10mLofwater,andtitrate<2.50>with0.1mol 0.01molWL sodium hydroxide VS: the solution is blue in
WLsodiumhydroxideVS(potentiometrictitration).Perform color.
ablankdeterminationusingasolutionpreparedbyadding19 (3) Heavy metals <1.07>—Proceed with 2.0g of Acetyl-
mL of water to 30mL of N,N-dimethylformamide, and choline Chloride for Injection according to Method 1, and
make any necessary correction. performthetest.Preparethecontrolsolutionwith2.0mLof
Standard Lead Solution (notmore than 10ppm).
Each mL of0.1molWL sodium hydroxide VS
＝32.44mg ofC H N OS Loss on drying <2.41> Not more than 1.0z (1g, 1059C, 3
15 20 2 4
hours).
Containers and storage Containers—Well-closed contain-
ers. Residue on ignition <2.44> Not morethan 0.1z(1g).
Assay (1) Acetylcholine chloride—Weigh accurately the
Acetylcholine Chloride for contentsofnotlessthan10AcetylcholineChlorideforInjec-
tions.Weighaccuratelyabout0.5gofthecontents,dissolve
Injection in15mLofwater,thenaddexactly40mLof0.1molWLsodi-
umhydroxideVS,stopperloosely,andheatonawaterbath
注射用アセチルコリン塩化物 for30minutes.Coolquickly,andtitrate<2.50>theexcessso-
diumhydroxidewith0.05molWLsulfuricacidVS(indicator:
3dropsofphenolphthaleinTS).Performablankdetermina-
tion.
Each mL of 0.1molWL sodium hydroxide VS
＝18.17mg ofC H ClNO
7 16 2
C H ClNO :181.66
7 16 2
2-Acetoxy-N,N,N-trimethylethylaminium chloride (2) Chlorine—Titrate<2.50>thesolution,whichhasbeen
[60-31-1] titrated in (1),with 0.1molWL silver nitrateVS (indicator:3
drops of ‰uorescein sodium TS).
AcetylcholineChlorideforInjectionisapreparation
Each mL of0.1molWL silver nitrate VS
for injection which is dissolved before use.
＝3.545mg of Cl
It contains not less than 98.0z and not more than
102.0z of acetylcholine chloride (C H ClNO ), and Containers and storage Containers—Hermeticcontainers.
7 16 2
notlessthan19.3zandnotmorethan19.8zofchlo-
rine (Cl: 35.45), calculated on the dried basis.
Itcontainsnotlessthan93zandnotmorethan107
z of the labeled amount of acetylcholine chloride
(C H ClNO ).
7 16 2
Method of preparation Prepare as directed under Injec-
tions.
Description Acetylcholine Chloride for Injection occurs as
white crystals or crystallinepowder.
It is very soluble in water, and freely soluble in ethanol
(95).
227722 Aclarubicin Hydrochloride / O‹cial Monographs JP XV
Purity (1) Clarity and color of solution－Dissolve 0.10g
Aclarubicin Hydrochloride ofAclarubicinHydrochloridein10mLofwater:thesolution
is clear and yellow to pale orange-yellow.
(2) Heavymetals<1.07>—Proceedwith1.0gofAclarubi-
アクラルビシン塩酸塩
cin Hydrochloride according to Method 2, and perform the
test. Prepare the control solution with 2.0mL of Standard
Lead Solution (not more than 20ppm).
(3) Related substances—Dissolve 10mg of Aclarubicin
Hydrochloride in 10mL of the mobile phase, and use this
solutionasthesamplesolution.Performthetestwith20mL
of the sample solution as directed under Liquid Chro-
matography <2.01> according to the following conditions,
and determine each peak area by the automatic integration
method. Calculate the amount of the related substances by
the area percentage method: the amount of aklavinone
havingtherelativeretentiontimeofabout0.6toaclarubicin
isnotmorethan0.2z,aclacinomycinL1havingtherelative
retention timeofabout0.75to aclarubicinisnotmore than
0.5z, 1-deoxypyrromycin having the relative retention time
of about 1.7 to aclarubicin is not more than 1.5z and
C H NO .HCl: 848.33 aclacinomycinS1havingtherelativeretentiontimeofabout
42 53 15
Methyl (1R,2R,4S)-4-s2,6-dideoxy-4-O-[(2R,6S)-6- 2.3 to aclarubicin is not more than 0.5z, and the total
methyl-5-oxo-3,4,5,6-tetrahydro-2H-pyran-2-yl]- amount of the peaks other than aclarubicin and the peaks
a-L-lyxo-hexopyranosyl-(1ª4)-2,3,6-trideoxy-3- mentionedaboveisnotmorethan1.0zofthepeakareaof
dimethylamino-a-L-lyxo-hexopyranosyloxyt-2-ethyl-2,5,7- aclarubicin.
trihydroxy-6,11-dioxo-1,2,3,4-tetrahydrotetracene- Operating conditions—
1-carboxylate monohydrochloride [75443-99-0] Detector: A visible absorption photometer (wavelength:
436nm).
Aclarubicin Hydrochloride is the hydrochloride of Column: A stainless steel column 3.9mm in inside
an anthracycline substance having antitumor activity diameterand30cminlength,packedwithsilicagelforliquid
produced by the growth of Streptomyces galilaeus. chromatography (10mm in particle diameter).
It contains not less than 920mg (potency) and not Column temperature: A constant temperature of about
more than 975mg (potency) per mg, calculated on the 259C.
anhydrous basis. The potency of Aclarubicin Mobilephase:Amixtureofchloroform,methanol,acetic
Hydrochloride is expressed as mass (potency) of acid (100),waterand triethylamine (6800:2000:1000:200:1).
aclarubicin (C H NO : 811.87). Flowrate:Adjustthe‰owratesothattheretentiontimeof
42 53 15
aclarubicin isabout 5minutes.
Description Aclarubicin Hydrochloride occurs as a yellow
Timespanofmeasurement:Aslongasabout4timesofthe
to pale orange-yellow powder.
retention time of aclarubicin beginning after the solvent
It is very soluble in chloroform and in methanol, freely
peak.
soluble in water,and slightly soluble in ethanol(95).
System suitability—
Identiˆcation (1) Determinetheabsorptionspectrumofa Test for required detectability: Pipet 1mL of the sample
solution of Aclarubicin Hydrochloride in diluted methanol solution,addthemobilephasetomakeexactly100mL,and
(4 in 5) (3 in 100,000) as directed under Ultraviolet-visible use this solution as the solution for system suitability test.
Spectrophotometry <2.24>, and compare the spectrum with Pipet1mLofthesolutionforsystemsuitabilitytest,andadd
theReferenceSpectrum:bothspectraexhibitsimilarintensi- the mobile phase to make exactly 10mL. Conˆrm that the
tiesofabsorption at the same wavelengths. peakareaofaclarubicinobtainedfrom20mLofthissolution
(2) Determine the infrared absorption spectrum of isequivalentto7to13zofthatfrom20mL ofthesolution
Aclarubicin Hydrochloride as directed in the potassium for system suitability test.
bromide disk method under Infrared Spectrophotometry System performance: Dissolve 5mg of Aclarubicin
<2.25>, and compare the spectrum with the Reference Hydrochloridein10mLof0.1mol/LhydrochloricacidTS,
Spectrum:both spectra exhibit similar intensities of absorp- andallowtostandfor60minutes.To1.0mLofthissolution
tion at the same wave numbers. add 1.0mL of 0.2mol/L sodium hydroxide TS, 1.0mL of
(3) AsolutionofAclarubicinHydrochlorideinmethanol phosphate buŠer solution, pH8.0 and 1.0mL of chlo-
(1 in 200) responds to the Qualitative Tests <1.09> (2) for roform, shake vigorously, and take the chloroform layer.
chloride. When the procedure is run with 20mL of the chloroform
under the above operating conditions, aclarubicin and 1-
Opticalrotation<2.49>[a]20:－146–－1629(50mgcalculat-
D deoxypyrromycinareelutedinthisorderwiththeresolution
ed on the anhydrous basis,water, 10mL, 100 mm).
between these peaks being notless than 3.0.
pH <2.54> The pH of a solution obtained by dissolving Systemrepeatability:Whenthetestisrepeated5timeswith
0.05g of Aclarubicin Hydrochloride in 10mL of water is 20mL of the sample solution under the above operating
between 5.5 and 6.5. conditions,therelativestandarddeviationofthepeakareaof
JP XV O‹cial Monographs / Compound Acrinol and Zinc Oxide Oil 227733
aclarubicin is notmore than 2.0z. and 2.5mL ofacetic acid (100),and use thissolution asthe
standard solution. Perform the test with these solutions as
Water <2.48> Not more than 3.5z (0.1g, volumetric
directedunderThin-layerChromatography<2.03>.Spot5mL
titration, direct titration).
eachofthesamplesolutionandstandardsolutiononaplate
Residueon ignition <2.44> Not more than 0.1z(1g). ofsilicagelforthin-layerchromatography.Developtheplate
withamixtureof2-propanolandaceticacid(100)(9:1)toa
Assay Weigh accurately an amount of Aclarubicin
distanceofabout10cm,andair-drytheplate.Examineun-
Hydrochloride,equivalenttoabout20mg(potency),anddis-
der ultraviolet light (main wavelength: 365nm): the spots
solve in diluted methanol (4 in 5) to make exactly 100mL.
fromthesamplesolutionandstandardsolutionexhibitablue
Pipet15mLofthissolution,adddilutedmethanol(4in5)to
‰uorescence and show the same Rfvalue.
make exactly 100mL, and use this solution as the sample
solution. Separately, weigh accurately an amount of Containers and storage Containers—Tightcontainers.
Aclarubicin Reference Standard, equivalent to about 20mg Storage—Light-resistant.
(potency),add0.6mLofdilutedhydrochloricacid(1in250)
anddilutedmethanol(4in5)tomakeexactly100mL.Pipet
Compound Acrinol and Zinc Oxide
15mLofthissolution,adddilutedmethanol(4in5)tomake
exactly 100mL, and use this solution as the standard solu- Oil
tion.Performthetestwiththesamplesolutionandstandard
solution as directed under Ultraviolet-visible Spectrophoto-
複方アクリノール・チンク油
metry<2.24>,anddeterminetheabsorbances,A andA ,at
T S
433nm.
Method of preparation
Amount[mg (potency)] of aclarubicin (C H NO )
42 53 15
＝WS×(AT/AS)×1000 Acrinol, very ˆnely powdered 10g
Zinc Oxide Oil 650g
W : Amount [mg (potency)] of Aclarubicin Reference
S
EthylAminobenzoate, ˆnely powdered 50g
Standard
White Beeswax 20g
Containers and storage Containers—Tightcontainers. Hydrophilic Petrolatum 270g
Storage—Light-resistantand at59C or below.
To make 1000g
Prepare by mixing the above ingredients.
Acrinol and Zinc Oxide Oil
Description CompoundAcrinolandZincOxideOilislight
yellow to yellow in color.
アクリノール・チンク油
Identiˆcation (1) Shake well 1g of Compound Acrinol
and Zinc Oxide Oil with 10mL of diethyl ether, 2mL of
Method of preparation
aceticacid(100)and10mLofwater,andseparatethewater
Acrinol, very ˆnely powdered 10g layer.Shake the layer with 5mL ofhydrochloricacid and 2
ZincOxide Oil 990g to 3 drops of sodium nitrite TS, and allow to stand: a dark
red color is produced (acrinol).
To make 1000g
(2) Place1gofCompoundAcrinolandZincOxideOilin
Prepare by mixing theabove ingredients. acrucible,meltbywarming,heat,graduallyraisingthetem-
peratureuntilthemassisthoroughlycharred,andthenignite
Description Acrinol and Zinc Oxide Oil is a yellowish
strongly: a yellow color is produced, and disappears on
white,slimysubstance.Separationofapartofitsingredients
cooling. To the residue add 10mL of water and 5mL of
occurs on prolonged standing.
dilutehydrochloricacid,shakewell,andˆlter.Totheˆltrate
Identiˆcation (1) Shake well 1g of Acrinol and Zinc add 2 to 3 drops of potassium hexacyanoferrate (II) TS: a
Oxide Oil with 10mL of diethyl ether, 2mL of acetic acid whiteprecipitate is produced (zinc oxide).
(100) and 10mL of water, and separate the water layer. (3) Shake well 0.2g of Compound Acrinol and Zinc
Shake the layer with 5mL of hydrochloric acid and 2 to 3 OxideOilwith20mLofethanol(95)and1mLofaceticacid
drops of sodium nitrite TS, and allow to stand: a dark red (100), centrifuge, ˆlter, and use the ˆltrate as the sample
coloris produced (acrinol). solution. Separately, dissolve 5mg of acrinol and 25mg of
(2) Place1gofAcrinolandZincOxideOilinacrucible, ethylaminobenzoatein50mLofethanol(95)andin2.5mL
melt by warming, heat, gradually raising the temperature of acetic acid (100), respectively, and use both solutions as
untilthemassisthoroughlycharred,andthenignitestrongly: thestandardsolutions(1)and(2).Performthetestwiththese
ayellowcolorisproduced,anddisappearsoncooling.Tothe solutionsasdirectedunderThin-layerChromatography<2.03
residueadd10mLofwaterand5mLofdilutehydrochloric >.Spot5mLeachofthesamplesolutionand standard solu-
acid,ˆlterafterthoroughshaking,andtotheˆltrateadd2to tions on a plate of silica gel with ‰uorescent indicator for
3 drops of potassium hexacyanoferrate (II) TS: a white thin-layerchromatography.Developtheplatewithamixture
precipitateis formed (zinc oxide). of 2-propanol and acetic acid (100) (9:1) to a distance of
(3) Shake well 0.2g of Acrinol and Zinc Oxide Oil with about10cm,andair-drytheplate.Examineunderultraviolet
20mL of ethanol (95) and 1mL of acetic acid (100), cen- light (main wavelength: 365nm): the spots from the sample
trifuge, ˆlter, and use the ˆltrate as the sample solution. solutionandstandardsolution(1)exhibitablue‰uorescence,
Separately,dissolve5mgofacrinolin50mLofethanol(95) andshowthesameRfvalue.Alsoexamineunderultraviolet
227744 Acrinol and Zinc Oxide Ointment / O‹cial Monographs JP XV
light (main wavelength: 254nm): the spots from the sample
solutionandstandardsolution(2)exhibitapurplecolor,and
show the same Rfvalue. Acrinol Hydrate
Containers and storage Containers—Tightcontainers.
Ethacridine Lactate
Storage—Light-resistant.
アクリノール水和物
Acrinol and Zinc Oxide Ointment
アクリノール・亜鉛華軟膏
Method of preparation C H NO.C H O.HO: 361.39
15 15 3 3 6 3 2
2-Ethoxy-6,9-diaminoacridine monolactate monohydrate
Acrinol, very ˆnely powdered 10g
ZincOxide Ointment 990g [1837-57-6]
To make 1000g
Acrinol Hydrate contains not less than 98.5z and
Prepare as directed under Ointments, with the above notmorethan101.0zofacrinol(C15H15N3O.C3H6O3:
ingredients. 343.38), calculated on the anhydrous basis.
Description Acrinol and Zinc oxide Ointment is yellow in Description AcrinolHydrateoccursasayellow,crystalline
color. powder.
Itissparinglysolubleinwater,inmethanolandinethanol
Identiˆcation (1) Shake 0.5g of Acrinol and Zinc Oxide
(99.5).
Ointment with 5mL of diethyl ether, 5mL of dilute
Melting point: about 2459C (with decomposition).
hydrochloricacidand2to3dropsofsodiumnitriteTS,and
ThepH of a solution of AcrinolHydrate(1 in 100)is be-
allow to stand: a dark red color develops in the water layer
tween 5.5 and 7.0.
(acrinol).
(2) Ignite 0.5g of Acrinol and Zinc Oxide Ointment to Identiˆcation (1) Determinetheabsorptionspectrumofa
char,anddissolvetheresiduein5mLofdilutehydrochloric solutionofAcrinolHydrate(3in250,000)asdirectedunder
acid:thesolutionrespondstotheQualitativeTests<1.09>for Ultraviolet-visible Spectrophotometry <2.24>, and compare
zinc salt. the spectrum with the Reference Spectrum:both spectra ex-
(3) Shake0.5gofAcrinolandZincOxideOintmentwith hibit similar intensities of absorption at the same
5mLofdiethylether,1mLofaceticacid(100)and5mLof wavelengths.
water,separatethewaterlayer,andusethewaterlayerasthe (2) Determine the infrared absorption spectrum of
sample solution. Dissolve 5mg of acrinol in 1mL of acetic Acrinol Hydrate as directed in the potassium bromide disk
acid (100) and 5mL of water, and use this solution as the methodunderInfraredSpectrophotometry<2.25>,andcom-
standard solution. Perform the test with these solutions as parethespectrumwiththeReferenceSpectrum:bothspectra
directedunderThin-layerChromatography<2.03>.Spot5mL exhibit similar intensities of absorption at the same wave
eachofthesamplesolutionandstandardsolutiononaplate numbers.
ofsilicagelforthin-layerchromatography.Developtheplate (3) To 5mL of a solution of Acrinol Hydrate (1 in 100)
with a mixture of diethyl ether, ethanol (95) and acetic acid add 5mL of dilute sulfuric acid, shake well, allow to stand
(100)(40:10:1)toadistanceofabout10cm,andair-drythe for about 10 minutes at room temperature, and ˆlter: the
plate.Examineunderultravioletlight(mainwavelength:365 ˆltrate responds to the QualitativeTests <1.09>forlactate.
nm):thespotsfromthesamplesolutionandthestandardso-
Purity (1) Chloride<1.03>—Dissolve1.0gofAcrinolHy-
lution exhibit a blue ‰uorescence and show the same Rf
drate in 80mL of water by warming on a water bath, cool,
value.
and add 10mL of sodium hydroxide TS and water to make
Containers and storage Containers—Tightcontainers. 100mL.Shakewell,allow tostandfor30minutes,ˆlter,to
Storage—Light-resistant. 40mLoftheˆltrateadd7mLofdilutenitricacidandwater
to make 50mL, and perform the test using this solution as
thetestsolution.Prepare50mLofthecontrolsolutionwith
4mL of sodium hydroxide TS, 7mL of dilute nitric acid,
0.30mL of 0.01mol/L hydrochloric acid VS and su‹cient
water (not more than 0.026z).
(2) Heavy metals <1.07>—Proceed with 1.0g of Acrinol
Hydrate according to Method 2, and perform the test. Pre-
parethecontrolsolutionwith2.0mLofStandardLeadSolu-
tion (notmore than 20ppm).
(3) Volatile fatty acids—Dissolve 0.5g of Acrinol Hy-
drateinamixtureof20mLofwaterand5mLofdilutesul-
furicacid,shakewell,ˆlter,andheattheˆltrate:noodorof
volatile fatty acidsis perceptible.
(4) Related substances—Dissolve 10mg of Acrinol Hy-