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BritishPharmacopoeia
BritishPharmacopoeiaVolumeI&II
Monographs:MedicinalandPharmaceuticalSubstances
Macrogols
GeneralNotices
(PhEurmonograph1444)
Actionanduse
Nonionicsurfactant.
PhEur
DEFINITION
MixturesofpolymerswiththegeneralformulaH(OCH2CH2)nOHwherenrepresentstheaverage
numberofoxyethylenegroups.Thetypeofmacrogolisdefinedbyanumberthatindicatesthe
averagerelativemolecularmass.Asuitablestabilisermaybeadded.
CHARACTERS
IDENTIFICATION
A.Itcomplieswiththetestforviscosity(seeTests).
B.To1ginatesttubeadd0.5mlofsulphuricacidR,closethetesttubewithastopper
fittedwithabentdeliverytubeandheatuntilwhitefumesareevolved.Collectthefumesviathe
deliverytubeinto1mlofmercuricchloridesolutionR.Anabundantwhite,crystalline
precipitateisformed.
C.To0.1gadd0.1gofpotassiumthiocyanateRand0.1gofcobaltnitrateRandmix
thoroughlywithaglassrod.Add5mlofmethylenechlorideRandshake.Theliquidphase
becomesblue.
TESTS
Appearanceofsolution
Thesolutionisclear(2.2.1)andnotmoreintenselycolouredthanreferencesolutionBY 6(2.2.2,
MethodII).
Dissolve12.5ginwaterRanddiluteto50mlwiththesamesolvent.
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Dissolve12.5ginwaterRanddiluteto50mlwiththesamesolvent.
Acidityoralkalinity
Dissolve5.0gin50mlofcarbondioxidefreewaterRandadd0.15mlofbromothymolblue
solutionR1.Thesolutionisyelloworgreen.Notmorethan0.1mlof0.1Msodiumhydroxideis
requiredtochangethecolouroftheindicatortoblue.
Viscosity(2.2.9)
TheviscosityiscalculatedusingadensitygiveninTable1444.1.
Formacrogolshavingarelativemolecularmassgreaterthan400,determinetheviscosityona
50percentm/msolutionofthesubstancetobeexamined.
Freezingpoint(2.2.18)
SeeTable1444.2.
Hydroxylvalue
Introducemg(seeTable1444.3)intoadryconicalflaskfittedwitharefluxcondenser.Add
25.0mlofphthalicanhydridesolutionR,swirltodissolveandboilunderarefluxcondenserona
hotplatefor60min.Allowtocool.Rinsethecondenserfirstwith25mlofpyridineRandthen
with25mlofwaterR,add1.5mlofphenolphthaleinsolutionRandtitratewith1Msodium
hydroxideuntilafaintpinkcolourisobtained(n1ml).Carryoutablanktest(n2ml).Calculate
thehydroxylvalueusingtheexpression:
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Formacrogolshavingarelativemolecularmassgreaterthan1000,ifthewatercontentismore
than0.5percent,dryasampleofsuitablemassat100105Cfor2handcarryoutthe
determinationofthehydroxylvalueonthedriedsample.
Reducingsubstances
Dissolve1gin1mlofa10g/lsolutionofresorcinolRandwarmgentlyifnecessary.Add2ml
ofhydrochloricacidR.After5minthesolutionisnotmoreintenselycolouredthanreference
solutionR3(2.2.2,MethodI).
Formaldehyde
Maximum30ppm.
TestsolutionTo1.00gadd0.25mlofchromotropicacid,sodiumsaltsolutionR,cooliniced
waterandadd5.0mlofsulphuricacidR.Allowtostandfor15minandcompleteslowlyto
10mlwithwaterR.
ReferencesolutionDilute0.860gofformaldehydesolutionRto100mlwithwaterR.Dilute
1.0mlofthissolutionto100mlwithwaterR.Ina10mlflask,mix1.00mlofthissolution
with0.25mlofchromotropicacid,sodiumsaltsolutionR,coolinicedwaterandadd5.0mlof
sulphuricacidR.Allowtostandfor15minandcompleteslowlyto10mlwithwaterR.
BlanksolutionIna10mlflaskmix1.00mlofwaterRwith0.25mlofchromotropicacid,
sodiumsaltsolutionR,coolinicedwaterandadd5.0mlofsulphuricacidR.Completeslowly
to10mlwithwaterR.
Determinetheabsorbance(2.2.25)ofthetestsolutionat567nm,againsttheblanksolution.Itis
nothigherthanthatofthereferencesolution.
Iftheuseofmacrogolswithahighercontentofformaldehydemayhaveadverseeffects,the
competentauthoritymayimposealimitofnotmorethan15ppm.
Ethyleneglycolanddiethyleneglycol
Carryoutthistestonlyifthemacrogolhasarelativemolecularmassbelow1000.
Gaschromatography(2.2.28).
TestsolutionDissolve5.00gofthesubstancetobeexaminedinacetoneRanddiluteto
100.0mlwiththesamesolvent.
ReferencesolutionDissolve0.10gofethyleneglycolRand0.50gofdiethyleneglycolRin
acetoneRanddiluteto100.0mlwiththesamesolvent.Dilute1.0mlofthissolutionto
10.0mlwithacetoneR.
Column:
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material:glass,
size:l=1.8m,=2mm,
stationaryphase:silaniseddiatomaceousearthforgaschromatographyR,impregnated
with5percentm/mofmacrogol20000R,
CarriergasnitrogenforchromatographyR.
Flowrate30ml/min.
Temperature:
column:ifnecessary,preconditionthecolumnbyheatingat200Cforabout15hadjust
theinitialtemperatureofthecolumntoobtainaretentiontimeof1416minfordiethylene
glycolraisethetemperatureofthecolumnbyabout30Catarateof2C/minbutwithout
exceeding170C
injectionportanddetector:250C.
DetectionFlameionisation.
Injection2l.
Carryout5replicateinjectionstochecktherepeatabilityoftheresponse.
LimitMaximum0.4percent,calculatedasthesumofthecontentsofethyleneglycoland
diethyleneglycol.
Ethyleneoxideanddioxan(2.4.25)
Maximum1ppmofethyleneoxideand10ppmofdioxan.
Heavymetals(2.4.8)
Maximum20ppm.
Dissolve2.0ginwaterRanddiluteto20mlwiththesamesolvent.12mlofthesolution
complieswithlimittestA.Preparethestandardusingleadstandardsolution(2ppmPb)R.
Water(2.5.12)
Maximum2.0percentformacrogolwitharelativemolecularmassnotgreaterthan1000and
maximum1.0percentformacrogolwitharelativemolecularmassgreaterthan1000,
determinedon2.00g.
Sulphatedash(2.4.14)
Maximum0.2percent,determinedon1.0g.
STORAGE
Inanairtightcontainer.
LABELLING
Thelabelstates:
thetypeofmacrogol,
thenameandtheconcentrationofanyaddedstabiliser,
thecontentofformaldehyde.
PhEur
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