乙醇检测工作在试剂和药典中应用.ppt

乙醇检测在试剂和药典中的应用,斯百全化学（上海）有限公司SpectrumChinaLtd.Spectrum质检部,800.720.5720,乙醇,C2H6O46.07Ethanol.EthylalcoholCAS#:64-17-5.应用：饮料汽车燃料消毒剂有机合成原料溶剂稀释剂萃取剂洗涤剂,Spectrum乙醇品种,A2176Alcohol,Denatured,190ProofA1038Alcohol,Anhydrous,CompletelyDenaturedA1040ReagentAlcohol,Denatured,Reagent,ACSE1020EthylAlcohol,190Proof,FCCE1028EthylAlcohol,Absolute,200Proof,Reagent,ACSE1029EthylAlcohol,190Proof,Reagent,ACSE1068DehydratedAlcohol,200Proof,USP,EP,BPE1421Alcohol,190Proof,BiotechGradeE1424DehydratedAlcohol,200Proof,BiotechGradeET107DehydratedAlcohol,200Proof,Undenatured,USPET108Alcohol,190Proof,USPHP612ReagentAlcohol,Denatured,ExceedsA.C.S.Specifications,HPLCGradeHS002ReagentAlcohol,Denatured,HistologicalGradeEX0278Alcohol,Denatured,OmniSolv(R)EX0289EthylAlcohol,MultiPharm,200Proof,EP,JP,USPEX0290EthylAlcohol,Pure,190Proof,HPLCGrade*Proof:酒精纯度,一个酒精纯度相当于0.5的酒精含量.,E1028,EthylAlcohol,Absolute,200Proof,Reagent,ACS,TESTSPECIFICATIONASSAY(byVOLUME)99.5%-COLOR(APHA)10SOLUBILITYINWATERTOPASSTESTWATER-0.2%RESIDUEAFTEREVAPORATION-0.001%ACETONETOPASSTEST(limitabout0.001%)ISOPROPYLALCOHOLTOPASSTEST(limitabout0.003%)TITRABLEACID-0.0005meq/gTITRABLEBASE-0.0002meq/gMETHANOL(CH3OH)-0.1%SUBSTANCESDARKENEDBY(H2SO4)TOPASSTESTSUBSTANCESREDUCINGPERMANGANATETOPASSTEST,GB/T678-2002无水乙醇,A1040,ReagentAlcohol,Denatured,Reagent,ACS,TESTSPECIFICATIONASSAY:ETHANOL+METANOL(v/v)94.0-96.0%ISOPROPANOL(v/v)4.0-6.0%WATER-0.5%COLOR(APHA)10RESIDUEAFTEREVAPORATION-0.001%,HP612,ReagentAlcohol,Denatured,ExceedsA.C.S.Specifications,HPLCGrade,TESTSPECIFICATIONASSAY:ETHANOL+METANOL(v/v)94.0-96.0%ISOPROPYLALCOHOL(v/v)4.0-6.0%ULTRAVIOLETABSORBANCE(1cmcellvs.water)-TOPASSTEST205nm1.00210nm0.65220nm0.35230nm0.20250nm0.04270nm0.01300nm0.005COLOR(APHA)10RESIDUEAFTEREVAPORATION-4PPMWATER-0.1%,E1068,DehydratedAlcohol,200Proof,USP,EP,BP,TESTSPECIFICATIONASSAY(byVOLUME)99.5%-CLARITYOFSOLUTIONTOPASSTESTCOLOROFSOLUTIONTOPASSTESTACIDITYORALKALINITYTOPASSTESTRELATIVEDENSITY0.790-0.793SPECIFICGRAVITY15.56oC-0.7962UVABSORPTIONTOPASSTESTVOLATILEIMPURITIESTOPASSTESTNONVOLATILERESIDUETOPASSTESTIDENTIFICATIONTOPASSTESTRESIDUALSOLVENTSTOPASSTEST,乙醇含量检测的应用,相对密度法USP,SpecificGravity.ET107,Dehydratedalcohol,200proof,undenatured,USP蒸馏法USP,Method.中国药典2005版一部：附录M乙醇量测定法a,b,c气相色谱法（GC）USP,Alcoholdetermination,Method.BE115,BelladonnaTinctureACS10th,Ethylalcohol.HP612，ReagentAlcohol,Denatured,ExceedsA.C.S.Specifications,HPLCGradeUSP,Residualsolvents,class3.中国药典2010版二部：附录E乙醇量测定法中国药典2005版一部：附录M乙醇量测定法,相对密度法-USP,SpecificGravity,methodET107,Dehydratedalcohol,200proof,undenatured,USP,Alcoholcontent:99.2%,byweight;99.5%,byvolume,at15.56.原理:25下,相同体积乙醇和水的重量比值,折算成15.56下乙醇的重量含量或体积含量.方法:使用同一比重瓶，先將先将一定体积的烧开过的蒸馏水放入其中,分別称量25下空瓶和水装入后的总重量,兩者之差就是25下水的重量.同理測量25下乙醇的重量.乙醇和水的重量比为25下乙醇的比重.通过查找USPreferencetableAlcoholometrictable中的数据，确定15.56下乙醇的体积含量或者重量含量.,比重瓶,USPreferencetableAlcoholometrictable,蒸馏法-USP,Method中国药典2005版一部：附录M乙醇量测定法,适用范围USP,Method:流浸膏剂,酊剂中国药典2005版一部：附录M乙醇量测定法:流浸膏剂,酊剂,中药制剂原理根据样品的不同性质,加入不同物质,进行预处理.蒸馏,获得乙醇馏出物.测定蒸馏物的相对密度,折算出乙醇的含量.方法(中国药典2005版一部：附录M乙醇量测定法)Alcoholcontent30%:称取20下样品25ml,置于150-200ml蒸馏瓶中,加水约25ml,蒸馏.待馏出物达23ml时,停止蒸馏.加水至刻度,测量乙醇在20下的相对密度,计算出乙醇含量;Alcoholcontent30%:称取20下样品25ml,置于150-200ml蒸馏瓶中,加水约50ml,蒸馏.待馏出物达48ml时,停止蒸馏.加水至刻度,测量乙醇在20下的相对密度,计算出乙醇含量;样品含有挥发性物质,如挥发油,三氯甲烷,乙醚,樟脑等.可先加入氯化钠使之饱和,后加入乙醚,使溶液分层,取水层按常规检测.样品含有游离氨或挥发性酸.可先加入稀硫酸或氢氧化钠溶液,调节酸碱度,再按常规检测.,蒸馏法-USP,MethodB1068,BenzalkoniumChlorideSolution,50Percent,NF,Alcoholcontent10.0%25下量取样品25.0ml,加水100ml,365下蒸馏.馏出物大约23ml时,停止蒸馏,在25下定容到25ml.因馏出物浑浊,加入CaCO3振摇,过滤.使用10ml比重瓶测量25下乙醇比重,折算出乙醇含量.结果:乙醇馏出物比重25:0.9938乙醇含量:4.2%,气象色谱法(GC)-ACS10th:EthylAlcohol.HP612,ReagentAlcohol,Denatured,ExceedsA.C.S.Specification,HPLCGradeSpecifications,HPLCGrade,Application:EthylAlcoholcontent95.0%GCmethodColumn:methylsiliconecapillaryColumntemperature:40for5min,programmedto220at10/min,hold2minInjectortemperature:150-220Detectortemperature:250Samplesize:0.2lsplitlessCarriergas:heliumat3ml/minDetector:TCDMeasuretheareaunderallpeaks,andcalculatetheethylalcoholcontentinareapercent,HP612,ReagentAlcohol,Denatured,ExceedsA.C.S.Specification,HPLCGradeSpecifications,HPLCGrade,气相色谱法(GC)-USP,Alcoholdetermination,Methoda.BE115,BelladonnaTincture,Application:Alcoholcontent:65.0%-70.0%.Column:DB-624Columntemperature:120,Injectortemperature:210Detectortemperature:210Samplesize:5lCarriergas:nitrogenorheliumDetector:FIDStandardsolution:5mleachUSPAlcoholRSandUSPacetoneRStogetherdilutedbywaterto50ml.Teststocksolution:Dilutesamplestepwisetogeta2%alcoholsolution.Testsolution:5mleachteststocksolutionandUSPacetoneRStogetherdilutedbywaterto50ml.SystemSuitabilityTest:R2(alcoholtoacetone)tailingfactor:2.0(alcohol)RSD2.0%(ratioofalcoholtoacetone),BE115,BelladonnaTincture,AlcoholContent,气相色谱法(GC)-USPResidualSolvents,Application:Alcoholcontent:5000ppm.Column:DB-624Columntemperature:40for20min,programmedto240at10/min,hold20minInjectortemperature:140Detectortemperature:250Samplesize:5ml,headspaceCarriergas:heliumDetector:FIDSplitratio:5:1SystemSuitabilityTest:R1.0RSD2.0%,SU124,SulfacetamideSodium,Monohydrate,USP,ResidualSolvents-Ethanol,中国药典2005版一部：附录M乙醇量测定法,适用范围：测定制剂中在20时乙醇的含量（%，ml/ml）色谱条件与系统适应性试验：用键合交联聚乙二醇为固定液的毛细管柱；起始温度为50，维持7分钟，再以每分钟10的速率升温至110；进样口温度190；FID检测器温度220。理论板数按正丙醇峰计算应不低于8000，乙醇峰与正丙醇峰的分离度应大于2.0.校正因子测定：精密量取恒温至20的无水乙醇4ml、5ml、6ml，分別置100ml量瓶中，分別精密加入恒温至20的正丙醇（内标物质）5ml，用水稀释至刻度，摇匀，精密量取上述各溶液1ml，分別置100ml量瓶中，用水稀释至刻度，摇匀（必要时可进一步稀释），作为对照品溶液。取上述三种溶液各适量，注入气相色谱仪，分別连续进样3次，测定峰面积，计算校正因子，所得校正因子的相对标准偏差不得大于2.0%。测定法：精密量取恒温至20的供试品适量（相当于乙醇约5ml），置100ml量瓶中，精密加入恒温至20的正丙醇5ml，用水稀释至刻度，摇匀，精密量取该溶液1ml，置100ml量瓶中，用水稀释至刻度，摇匀（必要时可进一步稀释），作为供试品溶液。取1l注入气相色谱仪，测定，即得。,CNAST0546能力验证气相色谱法测定药品中乙醇含量,样品名称:T1064盲样方法:中国药典2005版一部：附录M乙醇量测定法;或实验室常用气象色谱法能力验证結果实验结果:47.92%平均值:46.39%Z绝对值:7.123,不合格结果复测结果实验结果:46.23%平均值:46.39%Z绝对值:0.21,满意结果,原因分析,CNAST0546能力验证气相色谱法测定药品中乙醇含量直接进样,CNAST0546能力驗證气相色谱法测定药品中乙醇含量顶空进样,CNAST0546能力驗證气相色谱法测定药品中乙醇含量顶空进样,总结,方法偏离和确认方法验证精密度准确度专属性线性仪器比对人员比对方法比对实验室间比对,小知识：Alcohol,Aldehyde-free无醛乙醇的制备,USP-Dissolve2.5gofleadacetatein5mLofwater,addthesolutionto1000mLofalcoholcontainedinaglass-stopperedbottle,andmix.Dissolve5gofpotassiumhydroxidein25mLofwarmalcohol,coolthesolution,andadditslowly,withoutstirring,tothealcoholsolutionofleadacetate.After1hourshakethemixturevigorously,allowittostandovernight,decanttheclearliquid,andrecoverthealcoholbydistillation.溶解2.5g醋酸铅于5ml水中，将溶液加到装有1000ml乙醇