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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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