第十二章氣相色譜法

Section1Overview第一節(jié)概述氣相色譜法（gaschromatography,GC）是以氣體為流動相的色譜法。當(dāng)氣化的被測物質(zhì)隨載氣進(jìn)入色譜柱時，基于被測物質(zhì)在氣相和固定相之間吸附-解吸附（氣-固色譜）或分配（氣-液色譜）差異進(jìn)行分離。氣液色譜：利用待測物在載氣和固定在惰性固體表面的液體固定相之間的分配原理實(shí)現(xiàn)分離。Gaschromatography(GC)isagas-basedmobilephasechromatography.Whenthegasifiedtestsubstanceentersthecolumnwiththecarriergas,itisseparatedbasedonthedifferencebetweentheadsorptive-desorption(gas-solidchromatography)orthedistribution(gas-liquidchromatography)betweenthegasphaseandthestationaryphase.?Gas-solidchromatography:theuseofdifferentsubstancesinthesolidadsorbentonthephysicaladsorption-desorptioncapacityofdifferentmaterialseparation.氣固色譜：利用不同物質(zhì)在固體吸附劑上的物理吸附-解吸能力不同實(shí)現(xiàn)物質(zhì)的分離。LiquidChromatography:Separationwasachievedusingthedistributionprincipleoftheanalyteinthecarriergasandtheliquidstationaryphaseimmobilizedontheinertsolidsurface.

AdvantagesofGaschromatographic

氣相色譜優(yōu)點(diǎn)

Goodseparationability:theoreticalnumberof103~106Highsensitivity:10-11~10-13gHighselectivity:separableenantiomersandotherdifficulttoseparatesubstancesFast:AnanalysiscanbedoneinsecondstotensofminutesCanbeusedfornon-chromophorecompositionanalysis分離能力強(qiáng)：理論板數(shù)103～106靈敏度高：10-11～10-13g選擇性高：可分離對映體等難分離物質(zhì)快速：一次分析可在幾秒~幾十分鐘完成可用于無發(fā)色團(tuán)組分分析DisadvantagesofGaschromatographic

氣相色譜缺點(diǎn)

Onlyforheatstability,easytovaporizethematerialanalysisDerivativewhenanalyzingnonvolatilematter

Duetothesmallamountofinjection,quantitativeinjectionhassomedifficulties只適用于熱穩(wěn)定性好、易氣化的物質(zhì)分析分析非揮發(fā)性物質(zhì)時需衍生化由于進(jìn)樣量少，定量進(jìn)樣有一定困難GasChromatograph氣相色譜儀Schematicdiagramofagaschromatographic氣相色譜流程示意圖1.Gassupplysystem（載氣系統(tǒng)）Includinggascylindersorgasgenerators,pressureregulators,purifiers,flowcontrollers,andsoon.包括氣體鋼瓶或氣體發(fā)生器，壓力調(diào)節(jié)器，凈化管，流量控制器等。

Function:toprovideclean,constantflowofthecarriergas功能:提供清潔、流量恒定的載氣2.Sampleinjectionsystem

(進(jìn)樣系統(tǒng))Includingtheinjector(microinjectionorautosampler),septumandgasificationchamber.包括進(jìn)樣器(微量進(jìn)樣針或自動進(jìn)樣器)、隔墊和氣化室。Function:IntroducethesampleintotheGCsystemandevaporateintothegas.功能:將試樣引入GC系統(tǒng)并蒸發(fā)成氣體。3.Columnsystem（色譜柱系統(tǒng)）

◆Column,columnoven(色譜柱，柱溫箱)◆Columntype(色譜柱類型):Filledcolumn,columndiameter2~5mm(填充柱,柱內(nèi)徑2～5mm)Capillarycolumn,columndiameter0.1~0.53mm(毛細(xì)管柱,柱內(nèi)徑0.1～0.53mm)◆Columntemperaturecanbechangedaccordingtoprogram(programtemperature)柱溫可按程序改變（程序升溫）4.Detectionanddatasystem(檢測和數(shù)據(jù)處理系統(tǒng))◆Detector,dataacquisitionandprocessingdevice(檢測器，數(shù)據(jù)獲取和處理裝置)5.Controlsystem（控制系統(tǒng)）Temperaturecontrol,carriergasflowcontrol,(automaticinjectioncontrol),signalcontrol溫度控制，載氣流量控制，（自動進(jìn)樣控制），信號控制

(1)steampressure<10Paattheusetemperature(2)goodthermalstability,chemicalinertia(3)goodselectivity(4)themeasuredobjecthasacertaindegreeofsolubility第二節(jié)固定相stationaryphase一、Gas-liquidstationaryphase（氣-液色譜固定相）氣-液色譜固定相由固定液和載體組成.（一）stationaryliquid(固定液)Thestationaryliquidisgenerallyahighboilingsubstance.固定液一般為高沸點(diǎn)物質(zhì)在使用溫度下蒸汽壓<10Pa熱穩(wěn)定性好，化學(xué)惰性選擇性好對被測物有一定溶解度要求Itisconsistsofastationaryliquidandasupport.Stationaryliquidclassification(固定液分類)：●Classificationbychemicalstructure:alkanes,polysiloxanes,polydiols,estersandpolyesters

按化學(xué)結(jié)構(gòu)分類:烷烴,

聚硅氧烷,聚二醇,酯和聚酯Alkanes:squalane,Apiezon,烷烴類:異三十烷,阿皮松Polysiloxanes(聚硅氧烷類):R=-CH3,methylsilicone,OV-1,OV-101,SE-30,non-polarR=94%methyl,5%phenyl,1%vinyl,SE-54,weaklypolarR=50%methyl,50%phenyl,OV-17,middlepolarR=50%methyl,25%cyanopropyl,25%phenyl,OV-225,polarPolyethyleneglycol(聚二醇類):polyethyleneglycol，PEG（聚乙二醇）PEG-6000PEG-20MEsters(酯類):R=octyl,DOP(dioctylphthalate)R=nonyl,DNP(dinonylphthalate)Polyester(聚酯類):Diethyleneglycolsuccinatepolyester，DEGS

(丁二酸二甘醇聚酯)Thepolarityofthefixativeisafunctionoftheinteractionbetweenthefixativeandtheanalyte,whichisoppositetothepolaritydefinedbythechemicalstructure.固定液的極性是指固定液與被測物之間相互作用力的函數(shù)，與純粹的從化學(xué)結(jié)構(gòu)定義的極性不同，它是相對的。●Sortbypolarity(按極性分類)Relativepolarity:相對極性:P0-10，+1；21-40,+2;……..;81-100,+5。P值越大，極性越強(qiáng)。Somecommonlyusedfixative一些常用的固定液Fixedliquidchoice(固定液的選擇)Non-polarcomponents:Selectnon-polarfixative非極性組分：選擇非極性固定液Dispersionmainlyinaccordancewiththeboilingpointfromlowtohighintheorderofthepeak

色散力為主，按照沸點(diǎn)從低到高的順序出峰Polarcomponents:Selectpolarfixative

極性組分：選擇極性固定液

Dipoleforcemainlyinaccordancewiththepolarityfromsmalltolargeintheorderofthepeak

偶極作用力為主，按照極性從小到大的順序出峰無嚴(yán)格規(guī)則，一般可按“相似性原則”Nostrictrules,generallyaccordingtothe"similarityprinciple"Fixedliquidchoice(固定液的選擇)Polarandnonpolarmixedcomponents:Selectpolarfixative

極性與非極性混合組分：選擇極性固定液

Thenonpolarcomponentfirstpeaksandthepolarcomponentpeaksintheorderofpolarity

非極性組分先出峰，極性組分按極性順序出峰Hydrogen-bondedcomponents:Selectpolyglycol-basedfixative氫鍵型組分：選擇聚二醇類固定液

Accordingtotheformationofhydrogenbondcapacityintheorderofthepeak按照形成氫鍵能力大小順序出峰

Whenselectingafixative,focusonwhatisthemajordifferencebetweentheseparatedcomponentsandchoosetheappropriatefixative.

選擇固定液時，要重點(diǎn)關(guān)注被分離組分間的主要差異是什么，據(jù)此選擇合適的固定液。Example:Theeffectofdifferentfixativeonseparation例：不同固定液對分離的影響(二)Carrier載體Largesurfacearea(比表面積大;)Chemicallyinert(化學(xué)惰性;)Goodthermalstability;(熱穩(wěn)定性好;)Haveacertainmechanicalstrength(有一定機(jī)械強(qiáng)度)basicrequirements基本要求Types類型diatomite(硅藻土)Non-diatomaceousearth(非硅藻土類)(Glassmicrospheres,Teflon(玻璃微球，特氟龍)ChromosorbW（白色載體，101等）ChromosorbP（紅色載體，6201等）Passivationmethod鈍化方法Pickling酸洗（AW）Alkaliwash堿洗(BW)Silylation硅烷化(DMCS,HMDS)Weakenthecarriersurfaceadsorptionactivity減弱載體表面吸附活性二、Gas-solidchromatographystationaryphase

氣-固色譜固定相Adsorbents:Graphitizedcarbonblack,silicagel,aluminafortheanalysisoflowmolecularweightalcohols,alkanesandaldehydes吸附劑:石墨化炭黑，硅膠，氧化鋁，用于分析低分子量醇、烷烴和醛酮Molecularsieve:fortheanalysisofH2,O2,CO,N2,CO2,CH4andsoon分子篩:用于分析H2,O2,CO,N2,CO2,CH4等PolymerPorousMicrospheres(GDX):Analysisofcommonlyusedaminoacidsinethanolandorganiccompounds.高分子多孔微球（GDX）:藥物分析中常用語分析乙醇、有機(jī)化合物中微量水分。例：廢氣成分檢測固定相：5A分子篩;TCD檢測器三、Carriergas（載氣）N2:themostcommonlyusedgaschromatographiccarriergas;lowthermalconductivity,lowsensitivityforthermalconductivitytestingN2:最常用的氣相色譜載氣；熱導(dǎo)率低，用于熱導(dǎo)檢測時的靈敏度

低H2:highthermalconductivity,theuseofthermalconductivitydetectorcommonlyusedinthecarriergas.Flammable,payattentiontosafetyH2:熱導(dǎo)率高，使用熱導(dǎo)檢測器時常用該載氣。

易燃，需注意安全He:highthermalconductivity,commonlyusedinGC-MSHe:熱導(dǎo)率高，常用于GC-MSThethirdcolumntype

第三節(jié)柱類型◆Packedcolumn:填充柱:●Glassorstainlesssteel玻璃或不銹鋼材質(zhì)●Diameter2~4mm,length0.5~4m內(nèi)徑2～4mm,長0.5～4m●Fixedphaseparticles:60/80meshor80/100mesh

固定相顆粒：60/80目或80/100目●Commonlyusedcarriergasflowrate:20~60mL/min常用載氣流速：20～60mL/min●Columnefficiency:800~1000/m柱效：800～1000/m●Conventionaldruganalysisiscommonlyused

常規(guī)藥物分析時常用◆Capillarycolumn毛細(xì)管柱

●Quartzmaterial,coatedwithpolyimideprotectivelayer.

石英材質(zhì),外涂聚酰亞胺保護(hù)層.

●Diameter0.10~0.53mm,commonlyusedspecifications0.10,0.25,0.32,0.53mm.

內(nèi)徑0.10～0.53mm，常用規(guī)格0.10、0.25、0.32、0.53mm.

●Commontypes:常用類型：Coatedwithcapillary涂壁毛細(xì)管(WCOT)Carriercoatedcapillary載體涂層毛細(xì)管(SCOT)Cross-linkedcapillary交聯(lián)毛細(xì)管（用于GC-MS）

●Carriergasflowrate:1~2mL/min

載氣流速：1～2mL/min

●Applicationofsplit/splitlessinjection

應(yīng)用分流/不分流進(jìn)樣Section4Detector

第四節(jié)檢測器Concentrationtypedetector(濃度型檢測器):TCD,ECDQualitydetector(質(zhì)量型檢測器):FID,FPD,NPDPerformance性能指標(biāo):Sensitivity(S):1mlofcarriergascarrying1mgofthemeasuredcomponentsintothedetectorwhenthevoltage(fortheconcentrationofthedetector),orcarry1mgpersecondofthemeasuredcomponentsintothedetectorwhenthevoltageValue(qualitytypedetector).2.Noise(N)anddrift

噪聲(N)和漂移3.Detectionlimit(D):D=2N/S

檢測限（D）:D=2N/S靈敏度(S):每1mL載氣中攜帶1mg被測組分進(jìn)入檢測器時產(chǎn)生的電壓值(對濃度型檢測器),或者每秒鐘攜帶1mg被測組分進(jìn)入檢測器時產(chǎn)生的電壓值（質(zhì)量型檢測器）。一、Thermalconductivitydetector,TCD

熱導(dǎo)檢測器R1/R2=R3/R4,i=0R1/R2≠R3/R4,i≠0被測組分通過熱導(dǎo)池時，由于其熱導(dǎo)率與載氣不同，帶走的熱量不同，導(dǎo)致電橋不平衡，檢流計(jì)中有電流通過。將微電流通過電阻轉(zhuǎn)換成電壓，即為色譜信號。Wheatstone電橋Whenthemeasuredcomponentpassesthroughthethermalconductivitycell,becauseofitsthermalconductivityandthecarriergasisdifferent,takeawaytheheatisdifferent,resultinginbridgeimbalance,galvanometerflowthrough.Themicrocurrentthroughtheresistanceintovoltage,thatis,thechromatographicsignal.Thermalconductivitydetectorcharacteristics熱導(dǎo)檢測器的特點(diǎn)：Belongtotheuniversaldetector,aslongasthethermalconductivityandcarriergascanbedetected.屬于通用性檢測器，只要熱導(dǎo)率與載氣不同即可檢測.Comparedwithotherdetectors,thesensitivityislow.與其他檢測器相比，靈敏度較低.ResponseWidedynamicrange(105)響應(yīng)動態(tài)范圍寬(105)Nodamagetothecomponentundertest對被測組分無破壞性Factorsthataffectthesensitivityofthermalconductivitydetectors影響熱導(dǎo)檢測器靈敏度的因素1.Bridgecurrent(電橋電流)Theresponsevalueisproportionaltothecubicpowerofthebridgecurrent,sotheincreaseofthebridgecurrentcansignificantlyincreasetheresponsesignal,butthebridgecurrentcannotbearbitrarilyincreased,thecarriergasN2:100-150mA,H2docarriergas:150-200mA.響應(yīng)值與橋電流的三次方成正比，故增加橋電流可顯著增加響應(yīng)信號，但橋電流不可任意增大，

載氣N2時:100-150mA,H2做載氣時:150-200mA。Note:addthebridgebeforethefirstneedtopassthegas,soastoavoidhotwireblown加橋電流前需先通載氣，以免熱絲燒斷2.Detectortemperature

(檢測器溫度)Notlowerthanthecolumntemperature,oftenhigherthanthecolumntemperature20~50℃.不得低于柱溫，常比柱溫高20~50℃.3.Carriergas

(載氣)Sensitivityisproportionaltothethermalconductivityofthecarriergasandthecomponentundertest,H2>He>N2靈敏度正比于載氣與被測組分的熱導(dǎo)率差，H2>He>N24.Hotwireresistancevalue(熱絲電阻值)載氣熱導(dǎo)率

載氣熱導(dǎo)率

H2224.3CH445.8He175.6propane26.4N231.5ethanol22.3Air31.5acetone17.6

二、Flameionizationdetector，F(xiàn)ID(氫焰離子化檢測器)Structure(結(jié)構(gòu))Carbon-containingorganicmatterisburnedintheH2-Airflametoproducedebrisions,andanioncurrentisformedundertheactionofanelectricfield.Theseparatedcomponentsofthecolumnaredetectedbasedontheintensityoftheelectricalsignalgeneratedbytheioncurrent含碳有機(jī)物在H2-Air火焰中燃燒產(chǎn)生碎片離子，在電場作用下形成離子流，根據(jù)離子流產(chǎn)生的電信號強(qiáng)度，檢測被色譜柱分離的組分。Ionizationmechanism(離子化機(jī)理)

Themechanismisnotveryclearthatchemicalionizationisapossibleionizationmechanism.機(jī)理不十分清楚，化學(xué)離子化是可能的離子化機(jī)理.Takebenzeneasanexample:以苯為例:FactorsthataffectFIDsensitivity:影響FID靈敏度的因素：1.Gasflowrateratio(氣體流速比例):

N2:H2=1:1~1:1.5；H2:Air=1:102.Detectortemperature(檢測器溫度):>100℃（常用200-250℃）FIDFeatures(FID特點(diǎn))?Qualitydetector質(zhì)量型檢測器?Simplestructure,durable結(jié)構(gòu)簡單、耐用?Highsensitivity(10-13g/s)靈敏度高(10-13g/s)?ResponseWidedynamicrange(107)響應(yīng)動態(tài)范圍寬(107)?Theresponsevalueisrelatedtothenumberofcarbonatomsintheorganicmatter響應(yīng)值與有機(jī)物中含碳原子的數(shù)目有關(guān)?Noresponsetobustiblecompounds(H2O,CO2,SO2,CS2,NOx)對不可燃化合物（H2O,CO2,SO2,CS2,NOx）無響應(yīng)三、Electroncapturedetector，ECD（電子捕獲檢測器）63Nior3HStructure:結(jié)構(gòu):Detectionprinciple(檢測原理:)?Theβ-electronsemittedbytheradioactivesourceionizethecarriergasmoleculesandformastablebasestreamundertheactionofanelectricfield.放射源發(fā)出的β-電子使載氣分子離子化，在電場作用下形成穩(wěn)定的基流；?Organicmoleculeswithstrongelectronegativeelementscaptureβ-electrons,reducingthebaseflowandformingapeak.具有強(qiáng)電負(fù)性元素的有機(jī)分子捕獲β-電子，使基流降低，形成倒峰。Characteristicsofelectroniccapturedetectors

電子捕獲檢測器的特點(diǎn)?(10-15g/s)withelectronegativegroups(halogen,nitro,peroxide)

對含電負(fù)性基團(tuán)（鹵素、硝基、過氧化物）具有選擇性響應(yīng)(10-15g/s)?Alkali,alcohol,hydrocarbonsarebasicallyinsensitive

對胺、醇、碳?xì)浠衔锘静幻舾?Responsetonarrowdynamicrange(102)

響應(yīng)動態(tài)范圍較窄(102)?Non-linearresponse:非線性響應(yīng):?RequireshighpurityN2(>99.999%)ascarriergas

需用高純N2(>99.999%)作為載氣?Non-destructivetesting非破壞性檢測Otherimportantdetectors

其他重要檢測器?Flamephotometricdetector，F(xiàn)PD(火焰光度檢測器)

HasaselectiveresponsetothecompoundscontainingSandP對含S和P化合物具有選擇性響應(yīng)?thermionicdetector，TID;orNitrogenphosphorusdetector,NPD

熱離子檢測器;也稱氮磷檢測器HasaselectiveresponsetoNandPcontainingcompounds

對含N和P化合物具有選擇性響應(yīng)?Massspectrometerdetector,MSD(質(zhì)譜檢測器)?Fouriertransforminfrareddetector

傅里葉變換紅外檢測器（FTIR）Section5Selectionofchromatographicconditions

第五節(jié)色譜條件選擇一、thebasisforselectionofchromatographicconditions色譜條件選擇的依據(jù)Whereαisseparationfactor,k2isretentionfactor(capacityfactor)ofcompound2whichisretainedstrongerthancompound1.1.Fixedphaseselection(固定相選擇)

SeesectionII.(見第二節(jié)).2.Columntemperature(柱溫)Aftercolumnselection,columntemperatureisthemostimportantfactoraffectingseparation.Columntemperaturedecreased,theseparationincreased,butthepeakwidthincreased,theanalysistimeislonger.色譜柱選定后，柱溫是影響分離的最重要條件。柱溫降低，分離度提高，但峰寬增加，分析時間加長。Selectionprinciple:inthedifficulttoseparatesubstancestogetagoodseparation,analysisofappropriatetime,peakshapesymmetryunderthepremise,asfaraspossiblewithlowcolumntemperature.選擇原則：在使難分離物質(zhì)對得到良好分離，分析時間適宜，峰形對稱的前提下，盡量用低柱溫。

?Isothermal:thecolumntemperatureremainsconstantduringtheanalysis.等溫:在分析過程中柱溫保持不變.

?temperatureprogramming:Duringaperiodofanalysis,thecolumntemperaturechangesaccordingtoacertainproceduretofacilitateproperseparationofcomponentswithlargedifferencesinproperties.Themethodisapplicabletotheanalysisofcomplexcomponents(suchaswideboilingrangesampleswithlargepolarities)程序升溫(temperatureprogramming):在一個分析周期中，柱溫按照一定程序改變，以利于性質(zhì)差異大的組分達(dá)到合適的分離度。該法適用于復(fù)雜組分（如寬沸程樣品、極性差異大的樣品）分析。二、Selectionofexperimentalconditions(實(shí)驗(yàn)條件的選擇)例：等溫和程序升溫對分離效果的影響Example:Theeffectofwarmerprogramtemperatureontheseparationeffect3.

Carriergas(載氣)

Lowwirespeed,withN2(低線速時，用N2)Highspeed,withH2orHe(高線速時，用H2或He)WithTCD,useH2orHetoincreasesensitivity(用TCD時，使用H2或He可提高靈敏度)4.

Otherconditions(其他條件)(1)Inlettemperature:shouldensurethatthesampleinstantaneousgasification進(jìn)樣口溫度：應(yīng)保證樣品瞬間氣化(2)Detectortemperature:higherthancolumntemperature20-50°C檢測器溫度:高于柱溫20-50℃1.positionmethod(分解法)?Pyrolysis:Suitableforpolymerandothermacromoleculeanalysis熱裂解法:適用于高聚物等大分子分析?Hydrolysis:themacromoleculeshydrolyzeintosmallmolecules,theproteinhydrolyzedintoaminoacids水解法:將大分子水解成小分子,蛋白質(zhì)水解成氨基酸2.Derivatizationmethod衍生化法?esterification(酯化):-COOH-----COOR?silanization(硅烷化):-OH------O-Si(CH3)3-COOH------COOSi(CH3)3-NHR------NRSi(CH3)3?acylation(酰化):-OH------OCOR-NN2-------NHCOR三、

Samplepretreatment

(樣品預(yù)處理)Section6QualitativeAnalysisandQuantitativeAnalysis

第六節(jié)定性分析和定量分析

一、Systemsuitabilitytest(系統(tǒng)適用性試驗(yàn))

Testwithaprescribedreferencesolutionorsystemsuitabilitytestsolutiontodetermineifthechromatographicsystemusedisspecified.

用規(guī)定的對照品溶液或系統(tǒng)適用性試驗(yàn)溶液進(jìn)行試驗(yàn)，以判定所用色譜系統(tǒng)是否規(guī)定的要求。1．Numberoftheoreticalplatesofthecolumn(n)Thisparameterisusedtoevaluatetheseparationefficiencyofthecolumn.

色譜柱的理論板數(shù)（n）此參數(shù)用于評價(jià)色譜柱的分離效能。2．Separation(R):Requires>1.5(分離度（R）:要求>1.5)3．Repeatability:Usedtoevaluatetherepeatabilityofthechromatographicsystemresponsevaluesincontinuousinjections.

重復(fù)性:用于評價(jià)連續(xù)進(jìn)樣中色譜系統(tǒng)響應(yīng)值的重復(fù)性。4．TheThetailingfactor(T)isusedtoevaluatethesymmetryofthechromatographicpeaks.

拖尾因子（T）用于評價(jià)色譜峰的對稱性。

Unlessotherwisespecified,Tshouldbebetween0.95and1.05.

除另有規(guī)定外，T應(yīng)在0.95~1.05之間。

Section6QualitativeandQuantitativeAnalysis

第六節(jié)定性分析和定量分析

二、Qualitativeanalysis(定性分析)

Knownreferencesubstancecontrolmethod(已知對照品對照法)Usingtherelativeretentionvalue(采用相對保留值定性)UseKovatstoretainexponentialqualitative(用Kovats保留指數(shù)定性)GC-MS,GC-FTIRcombinedwithqualitative

以GC-MS、GC-FTIR聯(lián)用法定性三、Quantitativeanalysis(定量分析)(一)Correctionfactor(校正因子)(二)Quantitativemethod(定量方法)1.Normalizationmethod(歸一化法)

?Allcomponentsshouldbeseparatedanddetected

所有組分均應(yīng)被分離并被檢測到?Theamountofinjectionisnotcritical對進(jìn)樣量要求不嚴(yán)格2.Externalstandardization（外標(biāo)法）（2）Onepointexternalstandardmethod（外標(biāo)一點(diǎn)法）Suchasthecalibrationcurvethroughtheorigin,availableexternalstandardmethod如校正曲線通過原點(diǎn)，可用外標(biāo)一點(diǎn)法（1）Standardcurvemethod,orCalibrationcurvemethod

（標(biāo)準(zhǔn)曲線法或校正曲線法）Note:Theinjectionvolumemustbestrictlyaccurate進(jìn)樣量必須嚴(yán)格準(zhǔn)確3.Internalstandardmethod

(內(nèi)標(biāo)法)Requirementsforinternalstandards:對內(nèi)標(biāo)物的要求：Asubstancethatdoesnotexistinthesample

樣品中不存在的物質(zhì)Andthemeasuredcomponentsarecompletelyseparated,buttheretentiontimeisclose;whenthevariouscomponentsarequantitativelyquantified,theinternalstandardpeakispreferablybetweenseveralmeasuredcomponentpeaks.與被測組分完全分離，但保留時間接近；多種組分同時定量時，內(nèi)標(biāo)峰最高Highpurity純度高3.Internalstandardmethod

(內(nèi)標(biāo)法)（1）Internalstandardcorrectionfactormethod

內(nèi)標(biāo)校正因子法（2）Internalstandardcal