碘克沙醇USP34翻译.docx
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碘克沙醇USP34翻译.docx
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碘克沙醇USP34翻译
Iodixanol
碘克沙醇
(eye''ohdix'anol).
C35H44I6N6O15
1550.18
1,3-Benzenedicarboxamide,5,5'-[(2-hydroxy-1,3-propanediyl)bis(acetylimino)]bis[N,N'-bis(2,3-dihydroxypropyl)-2,4,6-triiodo-.5,5'-[(2-Hydroxytrimethylene)bis(acetylimino)]bis[N,N'-bis(2,3-dihydroxypropyl)-2,4,6-triiodoisophthalamide]
»Iodixanolcontainsnotlessthan98.6percentandnotmorethan101.0percentofC35H44I6N6O15,calculatedontheanhydrousbasis.
Packagingandstorage—Preserveinwell-closed,light-resistantcontainers.Storeat25
excursionspermittedbetween15
and30
.
本品为1,3-苯二甲酰胺,5,5'-[(2-羟基-1,3-丙二基)双(乙酰亚胺基)]双[N,N'-双(2,3-二羟丙基)-2,4,6-三碘-;5,5'-[(2-羟基丙烷基)双(乙酰亚胺基)]双[N,N'-双(2,3-二羟丙基)-2,4,6-三碘异酞酰胺]
[92339-11-2]
按无水物计算,本品含C35H44I6N6O15应为98.6%~101.0%。
【包装和贮藏】密闭容器保存,避光。
温度为25℃,允许在15℃~30℃范围内变化。
USPReferencestandards
11
—
USPIodixanolRS
USPIohexolRelatedCompoundBRS
5-Amino-N,N'-bis(2,3-dihydroxypropyl)-2,4,6-triiodo-1,3-benzenedicarboxamide.
USPIodixanolRelatedCompoundCRS
5-[Acetyl[3-[[3,5-bis[[(2,3-dihydroxypropyl)amino]carbonyl]-2,4,6-triiodophenyl]amino]-2-hydroxypropyl]amino]N,N'-bis(2,3-dihydroxypropyl)-2,4,6-triiodo-1,3-benzenedicarboxamide.
USPIodixanolRelatedCompoundDRS
5-[Acetyl(2-hydroxy-3-methoxypropyl)amino]-N,N'-bis(2,3-dihydroxypropyl)-2,4,6-triiodo-1,3-benzenedicarboxamide.
USPIodixanolRelatedCompoundERS
5-[[3-[[3-[[(2,3-Dihydroxypropyl)amino]carbonyl]-5-[[amino]carbonyl]-2,4,6-triiodophenyl](acetylimino)]-2-hydroxypropyl]-(acetylimino)]-N,N'-bis(2,3-dihydroxypropyl)-2,4,6-triiodo-1,3-benzenedicarboxamide.
【USP对照品】<11>
碘克沙醇对照品
碘克沙醇相关物质B对照品
5-氨基-N,N'-双(2,3-二羟丙基-2,4,6-三碘-1,3-苯二甲酰胺
碘克沙醇相关物质C对照品
5-[乙酰基[3-[[3,5-双[[(2,3-二羟丙基)氨基]羰基]-2,4,6-三碘苯基]氨基]-2-羟丙基]氨基]N,N'-双(2,3-二羟丙基)-2,4,6-三碘-1,3-苯二甲酰胺
碘克沙醇相关物质D对照品
5-[乙酰基(2-羟基-3-甲氧基丙基)氨基]-N,N'-双(2,3-二羟丙基)-2,4,6-三碘-1,3-苯二甲酰胺
碘克沙醇相关物质E对照品
5-[[3-[[3-[[(2,3-二羟丙基)氨基]羰基]-5-[[氨基]羰基]-2,4,6-三碘苯基](乙酰亚胺基)]-2-羟丙基]-(乙酰亚胺基)]-N,N'-双(2,3-二羟丙基)-2,4,6-三碘-1,3-苯二甲酰胺
Identification—
A:
InfraredAbsorption
197K
.
B:
TheretentiontimesofthetwoprincipalpeaksinthechromatogramoftheTestsolutioncorrespondtothoseinthechromatogramofStandardsolution2,asobtainedinRelatedcompounds,Test2.[note—Athirdisomermayappearasaminorpeak.]
C:
Heat0.5ginacrucible:
violetvaporsareevolved.
【鉴别】
(1)红外吸收<197K>
(2)在有关物质测试2项下记录的色谱图中,供试品溶液的两个主峰保留时间应与对照品溶液2的两个主峰保留时间一致。
(注:
可能出现第三个异构体小峰)
(3)取本品0.5g,置坩埚中加热:
有紫色碘蒸汽产生。
Specificrotation
781S
:
between–0.5
and+0.5
.
Testsolution:
50mgpermL.
Microbialenumerationtests
61
andTestsforspecifiedmicroorganisms
62
—ProceedasdirectedforPlateMethodunderTotalAerobicMicrobialCount:
notmorethan100cfuperg.
【检查】比旋度<781S>应为–0.5°至+0.5°。
供试品溶液:
50mg/mL的水溶液。
微生物计数试验<61>和特定微生物检查<62>照需氧菌总数下的平皿法进行操作:
不得过100cfu/g。
Water,MethodI
921
:
notmorethan4.0%.
Heavymetals,MethodI
231
:
0.001%.
Freeiodine—Transfer2gtoaglass-stopperedtube,addabout20mLofwater,5mLoftoluene,and5mLof2Nsulfuricacid,shakevigorously,andallowthephasestoseparate:
thetoluenelayershowsnoredorpinkcolor.
水分(<921>:
方法I)不得过4.0%。
重金属(<231>:
方法I)不得过0.001%。
游离碘取本品2g,置具塞管中,加水约20mL,甲苯5mL和2N硫酸溶液5mL,强烈振摇,静置使分层:
甲苯层不得显红色或粉红色。
Limitoffreeiodide—Transfer5.0gtoasuitablecontainer,addabout30mLofwater,andtitratewith0.001NsilvernitrateVS,determiningtheendpointpotentiometrically.EachmLof0.001Nsilvernitrateisequivalentto126.9µgofiodine.Notmorethan0.39mLof0.001Nsilvernitrateisrequired:
notmorethan10µgofiodidepergisfound.
游离碘化物取本品5.0g,置适宜容器中,加水约30mL,照电位滴定法,用0.001N硝酸银滴定液滴定。
每mL0.001N硝酸银滴定液相当于126.9µg的碘。
消耗0.001N硝酸银滴定液不得过0.39mL:
碘化物不得过10µg/g。
Limitoffreearomaticamine—
N-(1-Naphthyl)ethylenediaminedihydrochloridesolution—PrepareafreshsolutionofN-(1-naphthyl)ethylenediaminedihydrochloride(3in1000)inamixtureofpropyleneglycolandwater(70:
30).
Blanksolution—Add15mLofwatertoa25-mLvolumetricflask.
Standardstocksolution—DissolveanaccuratelyweighedquantityofUSPIohexolRelatedCompoundBRS,andquantitativelydilutewithwatertoobtainasolutionhavingaknownconcentrationofabout10µgpermL.
Standardsolution—Transfer10.0mLoftheStandardstocksolutionand5mLofwatertoa25-mLvolumetricflask.
Testsolution—Transferabout200mgofIodixanol,accuratelyweighed,toa25-mLvolumetricflask,add15mLofwater,andmix.
游离芳香胺
N-(1-萘基)乙二胺二盐酸盐溶液取N-(1-萘基)乙二胺二盐酸盐,加丙二醇与水的混合溶液(70:
30)制成3→1000的溶液(新配制)。
空白溶液取水15mL,置25mL量瓶中。
对照品储备液取USP碘海醇有关物质B对照品适量,精密称定,加水溶解并定量稀释制成每mL中约含10µg的溶液。
对照品溶液取对照品储备液10.0mL和水5mL,置25mL量瓶中。
供试品溶液取本品约200mg,精密称定,置25mL量瓶中,加水15mL,摇匀。
Procedure—TreattheStandardsolution,theTestsolution,andtheBlanksolutionasfollows.Placetheflaskinanicebathfor5minutes.Add1.5mLof6Nhydrochloricacid,mixbyswirling,add1.0mLofsodiumnitritesolution(2in100),mix,andallowtostandintheicebathfor4minutes.Removetheflaskfromtheicebath,add1.0mLof4%sulfamicacidsolution,andswirlgentlyuntilgasevolutionceases.Add1.0mLofN-(1-Naphthyl)ethylenediaminedihydrochloridesolution,mix,dilutewithwatertovolume,mix,andallowtostandfor5minutes.TransferthesolutionobtainedfromtheTestsolutionandthesolutionobtainedfromtheStandardsolutiontoseparatecolor-comparisontubes.ThesolutionobtainedfromtheTestsolutionislighterthanthesolutionobtainedfromtheStandardsolution:
notmorethan0.05%isfound.IfthesolutionobtainedfromtheTestsolutionisaboutthesamecolorordarkerthanthesolutionobtainedfromtheStandardsolution,proceedasfollows.ConcomitantlydeterminetheabsorbancesofthesolutionobtainedfromtheTestsolution,thesolutionobtainedfromtheStandardsolution,andthesolutionobtainedfromtheBlanksolutionin5-cmcells,atthewavelengthofmaximumabsorbanceatabout495nm,usingthesolutionobtainedfromtheBlanksolutiontozerothespectrophotometer.CalculatethepercentageoffreearomaticamineintheportionofIodixanoltakenbytheformula:
测定
取对照品溶液,供试品溶液和空白溶液按下述同法操作。
将量瓶置冰浴中5分钟,加6N盐酸溶液1.5mL,涡旋混匀,加亚硝酸钠溶液(2→100)1.0mL,混匀,并置冰浴中4分钟。
从冰浴中取出量瓶,加4%的氨基磺酸溶液1.0mL,并缓慢涡旋直至气体停止逸出。
加N-(1-萘基)乙二胺二盐酸盐溶液1.0mL,混匀,用水稀释至刻度,摇匀,并静置5分钟。
取供试品溶液和对照品溶液分别置比色管中,供试品溶液所显颜色应浅于对照品溶液:
不得过0.05%。
若供试品溶液所显颜色约等于或深于对照品溶液,按下述操作。
用5-cm吸收池盛溶液在495nm波长处测定供试品溶液、对照品溶液和空白溶液的吸光度,分光光度计用空白溶液归零。
按以下公式计算碘克沙醇中游离芳香胺的百分含量:
(C/W)[(AU–AB)/(AS–AB)]
inwhichCistheconcentration,inµgpermL,ofUSPIohexolRelatedCompoundBRSintheStandardsolution;Wistheweight,inmg,ofIodixanoltakentopreparetheTestsolution;andAU,AB,andASaretheabsorbancesofthefinalsolutionsobtainedfromtheTestsolution,theBlanksolution,andtheStandardsolution,respectively:
notmorethan0.05%isfound.
结果=(C/W)[(AU–AB)/(AS–AB)]
C
=
对照品溶液中USP碘海醇有关物质B对照品的浓度(µg/mL)
W
=
供试品溶液中碘克沙醇的重量(mg)
AU
=
供试品溶液的吸光度
AB
=
空白溶液的吸光度
AS
=
对照品溶液的吸光度
限度
不得过0.05%。
Limitofcalcium—
Internalstandardsolution—Accuratelyweighabout3.067gofscandiumoxide,anddissolvein1Lofwater(eachmLcontains2.0mgofscandium).Transfer10.0mLofthissolutiontoa100-mLvolumetricflask,dilutewithwatertovolume,andmix.
Blanksolution—Transfer5.0mLofInternalstandardsolutiontoa50-mLvolumetricflask,dilutewithwatertovolume,andmix.
Standardsolutions—Prepareasolutionhavingaconcentrationof10µgofcalciumpermL.Add0.5,2.5,5.0,and10.0mLofthissolutiontoseparate50-mLvolumetricflasks.Toeachflask,add5.0mLofInternalstandardsolution,dilutewithwatertovolume,andmix.
钙
内标溶液:
取氧化钪约3.067g,精密称定,加水1L使溶解(每mL中含钪2.0mg)。
取该溶液10.0mL,置100mL量瓶中,加水稀释至刻度,摇匀。
空白溶液:
取内标溶液5.0mL,置50mL量瓶中,加水稀释至刻度,摇匀。
对照品溶液:
配制每mL中含钙10µg的溶液,取该溶液0.5mL、2.5mL、5.0mL和10.0mL,分别置50mL量瓶中,每个量瓶中加入内标溶液5.0mL,加水稀释至刻度,摇匀。
Testsolution—Transferabout2gofIodixanol,accuratelyweighed,toa20-mLvolumetricflask,addabout10mLofwater,andmix.Add2.0mLofInternalstandardsolution,dilutewithwatertovolume,andmix.
Procedure—ConcomitantlydeterminetheabsorbancesofeachStandardsolutionandtheTestsolutionat393.366nm,thecalciumemissionline,andat361.38nm,thescandiumemissionline,withanatomicabsorptionspectrophotometer,usingtheBlanksolutionastheblank.Plotastandardcurveoftheratioofthecalciumabsorptiontothescandiumabsorptionversustherespectivecalciumconcentrations.Fromthegraphsoobtained,determinethecalciumconcentration,C,inµgpermL,intheTestsolution.Calculatethecontentofcalcium,inµgperg,intheportionofIodixanoltakenbytheformula:
20(C/W)
inwhichCisasobtainedabove;andWistheweight,ing,ofIodixanoltakentopreparetheTestsolution:
notmorethan5µgpergisfound.
供试品溶液取本品约2g,精密称定,置20mL量瓶中,加水约10mL,混匀。
加内标溶液2.0mL,用水稀释至刻度,摇匀。
测定
用原子吸收分光光度计,以空白溶液作空白,在393.366nm(钙的发射谱线)和361.38nm(钪的发射谱线)处同时测定对照品溶液和供试品溶液的吸光度。
以钙与钪的吸光度比值和钙的各个浓度作标准曲线。
从图表中获得供试品溶液中的钙浓度C,µg/mL;按以下公式计算碘克沙醇中钙的含量,µg/g:
结果=20(C/W)
C
=
由上述图表获得
W
=
供试品溶液中碘克沙醇的重量(g)
限度
不得过5µg/g。
Limitofioniccompounds—[note—Rinseallglasswarewithwater.]PrepareasolutionofIodixanolinwater(2in100).Thespecificconductanceofthissolutionisnotgreaterthanthatofasodiumchloridesolutionhavingaconcentrationof4µgpermL(equivalenttonotmorethan0.02%ofioniccompounds,asNaCl).
离子化合物(注:
用水清洗所有的玻璃仪器)
取本品,加水制成水溶液(2→100)。
该溶液电导率不得大于浓度为4µg/mL的氯化钠溶液(相当于0.02%的离子化合物,以氯化钠计)。
Limitofmethanol,isopropylalcohol,andmethoxyethanol—
Internalstandardstocksolution—Transferabout500mgofsecondarybutylalcoholtoa500-mLvolumetricflask,dilutewithwatertovolume,andmix.
Internalstandardsolution—Transfer1.0mLofIn
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