干燥失重藥典比較

干燥失重中國(guó)藥典：供試品，混合均勻(如為較大的結(jié)晶，應(yīng)先迅速搗碎使成2mm以下的小粒)。取約1g或各藥品項(xiàng)下規(guī)定的重量，置與供試品同樣條件下干燥至恒重的扁形稱瓶中，精密稱定，除另有規(guī)定外，在105r干燥至恒重。從減失的重量和取樣量計(jì)算供試品的干燥失重。供試品干燥時(shí)，應(yīng)平鋪在扁形稱量瓶中，厚度不可超過(guò)5mm，如為疏松物質(zhì)，厚度不可超過(guò)10mm。放入烘箱或干燥器進(jìn)行干燥時(shí)，應(yīng)將瓶蓋取下，置稱量瓶旁，或?qū)⑵可w半開(kāi)進(jìn)行干燥；取出時(shí)，須將稱量瓶蓋好。置烘箱內(nèi)干燥的供試品，應(yīng)在干燥后取出置干燥器中放冷至室溫，然后稱定重量。供試品如未達(dá)規(guī)定的干燥溫度即融化時(shí)，應(yīng)先將供試品于較低的溫度下干燥至大部分水分除去后，再按規(guī)定條件干燥。當(dāng)用減壓干燥器或恒溫減壓干燥器時(shí)，除另有規(guī)定外，壓力應(yīng)在2.67kPa(20mmHg)以下；干燥器中常用的干燥劑為無(wú)水氯化鈣、硅膠或五氧化二磷，恒溫減壓干燥器中常用的干燥劑為五氧化二磷，除另有規(guī)定外，溫度為60r。干燥劑應(yīng)保持在有效狀態(tài)。美國(guó)藥典-731?；LOSSONDRYINGTheproceduresetforthinthischapterdeterminestheamountofvolatilematterofanykindthatisdrivenoffundertheconditionsspecified.Forsubstancesappearingtocontainwaterastheonlyvolatileconstituent,theproceduregiveninthechapter,WaterDetermination'?921；,isappropriate,andisspecifiedintheindividualmonograph.本章中給出的方法闡述了在特定的條件下任何物質(zhì)中的揮發(fā)性組分的檢測(cè)，本方法只包括揮發(fā)性成分的檢測(cè)（包括水）。水分檢測(cè)可用本方法，也可以同其他文獻(xiàn)規(guī)定的方法檢測(cè)。Unlessotherwisedirectedintheindividualmonograph,conductthedeterminationona1-to2-gtestspecimen.Mixthesubstancetobetestedand,ifitisintheformoflargeparticles,reducetheparticlesizetoabout2mmbyquicklycrushingbeforeweighingoutthetestspecimen.Tareanappropriateglass-stoppered,shallowweighingbottlethathasbeendriedforabout30minutesunderthesameconditionstobeemployedinthedeterminationandcooledtoroomtemperatureinadesiccator.Putthetestspecimeninthebottle,replacethecover,andaccuratelyweighthebottleandthecontents.Bygentle,sidewiseshaking,distributethetestspecimenasevenlyaspracticabletoadepthofabout5mmgenerally,andnotmorethan10mminthecaseofbulkymaterials.Placetheloadedbottleinthedryingchamber,removingthestopperandleavingitalsointhechamber.Drythetestspecimenatthetemperatureandforthetimespecifiedinthemonograph.[Note—Thetemperaturespecifiedinthemonographistoberegardedasbeingwithintheorangeof±2ofthestatedfigure.]When“drytoconstantweight"isspecifiedinamonograph,dryingshallbecontinueduntiltwoconsecutiveweighingsdonotdifferbymorethan0.50mgpergofsubstancetaken,thesecondweighingfollowinganadditionalhourofdrying.Uponopeningthechamber,closethebottlepromptly,andallowittocometoroomtemperatureinadesiccatorbeforeweighing.除各論中另有規(guī)定外，取混勻后（如果樣品是比較大的結(jié)晶，應(yīng)先迅速搗碎使成2mm左右的顆粒）的待測(cè)樣品，精密稱定1?2g置于與樣品相同條件下干燥30分鐘的具塞扁形稱量瓶中，稱量瓶先稱取皮重，待樣品加入后，蓋上瓶蓋，稱取總重。輕輕地平移振搖，盡可能使樣品均勻平鋪成約5mm厚，對(duì)于比較松散的、體積大的也不應(yīng)超過(guò)10mm厚。將裝有樣品的稱量瓶放在干燥室內(nèi)，瓶蓋打開(kāi)，也放入干燥室，按各論中規(guī)定的溫度和時(shí)間干燥。［注意：各論中規(guī)定的干燥溫度應(yīng)該被視為規(guī)定溫度±2°C。］打開(kāi)干燥室，立即蓋上瓶蓋，移入干燥器中冷卻到室溫，然后稱量。IfthesubstancemeltsatalowertemperaturethanthatspecifiedforthedeterminationofoLossonDryingmaintainthebottlewithitscontentsfor1to2hoursatatemperature5oto10belowthemeltingtemperature,thendryatthespecifiedtemperature.如果待測(cè)樣品在低于干燥使用的檢測(cè)溫度時(shí)就發(fā)生了溶解現(xiàn)象，可以在溫度在低于溶解溫度（上述）5-10C下，維持1—2小時(shí)，然后在升溫到指定溫度。Wherecapsulesaretobetested,useaportionofthemixedcontentsofnotfewerthan4capsules.檢測(cè)樣品是膠囊，檢測(cè)樣品應(yīng)該從至少是4個(gè)膠囊內(nèi)容物的混合樣中取出。Wheretabletsaretobetested,usepowderfromnotfewerthan4tablets.檢測(cè)樣品是片劑，應(yīng)至少壓碎4個(gè)片的粉末，從中取出優(yōu)良粉末用于檢測(cè)。Wheretheindividualmonographdirectsthatlossondryingbedeterminedbythermogravimetricanalysis,asensitiveelectrobalanceistobeused.要是按著單獨(dú)的文獻(xiàn)報(bào)道作干燥失重的檢測(cè)，應(yīng)該使用在這些文獻(xiàn)中要求采用的熱重量分析儀和高靈敏天平。Wheredryinginvacuumoveradesiccantisdirectedintheindividualmonograph,avacuumdesiccatororavacuumdryingpistol,orothersuitablevacuumdryingapparatus,istobeused.要是按著單獨(dú)文獻(xiàn)報(bào)道中做真空干燥失重，應(yīng)該使用這些文獻(xiàn)中要求采用的真空干燥器、真空干燥槍或者其他的真空干燥設(shè)備。Wheredryinginadesiccatorisspecified,exerciseparticularcaretoensurethatthedesiccantiskeptfullyeffectivebyfrequentreplacement.當(dāng)用到干燥器時(shí)，應(yīng)該特別注意及時(shí)更換干燥劑以保持其有效狀態(tài)。Wheredryinginacapillary-stopperedbottleinvacuumisdirectedintheindividualmonograph,useabottleortubefittedwithastopperhavinga225±25-pmdiametercapillary,andmaintaintheheatingchamberatapressureof5mmorlessofmercury.Attheendoftheheatingperiod,admitdryairtotheheatingchamber,removethebottle,andwiththecapillarystopperstillinplaceallowittocooltoroomtemperatureinadesiccatorbeforeweighing.在采用單獨(dú)文獻(xiàn)報(bào)道的毛細(xì)管真空干燥失重法實(shí)驗(yàn)中，應(yīng)該使用直徑為225±25um的帶塞毛細(xì)管，維持干燥室內(nèi)的壓力在5毫米汞柱或者更低。在加熱結(jié)束時(shí)，可以把干燥的空氣放進(jìn)干燥室內(nèi)，蓋上塞，把毛細(xì)管在干燥室內(nèi)冷后，稱重。歐洲藥典：Lossondryingisthelossofmassexpressedaspercentm/m.干燥失重是重量的減少，用m/m的百分比來(lái)表示。Method.Placetheprescribedquantityofthesubstancetobeexaminedinaweighingbottlepreviouslydriedundertheconditionsprescribedforthesubstancetobeexamined.Drythesubstancetoconstantmassorfortheprescribedtimebyoneofthefollowingprocedures.Wherethedryingtemperatureisindicatedbyasinglevalueratherthanarange,dryingiscarriedoutattheprescribedtemperature±2°C.方法：將規(guī)定重量的供試品放在預(yù)先干燥的稱量瓶中，按照下列要求進(jìn)行干燥，干燥供試品至恒重，或者按照下列操作之一，干燥規(guī)定的時(shí)間?！癷nadesiccator":thedryingiscarriedoutoverdiphosphoruspentoxideRatatmosphericpressureandatroomtemperature;在干燥器中：在常溫，常壓下，以無(wú)氧化二磷干燥。“invacuo":thedryingiscarriedoutoverdiphosphoruspentoxideR,atapressureof1.5kPato2.5kPaatroomtemperature;真空干燥：室溫下，在壓力為1.5?2.5kPa，放置無(wú)氧化二磷的真空干燥箱內(nèi)干燥。“invacuowithinaspecifiedtemperaturerange":thedryingiscarriedoutoverdiphosphoruspentoxideR,atapressureof1.5kPato2.5kPawithinthetemperatu