质量分析方法验证中检出限和定量限测定方法探讨

DrugStandardsofChina2012Vol.13No.1201213133。[e-mail]··1231.1000502.1320003.100061、IUPACICH。R921.2A1009－36562012－1－33－3DiscussionontheDetectingMethodsforLimitofDetectionandLimitofQuantificationinValidationofAnalyticalMethodLuJing1FuLingyan2WangXu31.NationalInstitutesforFoodandDrugControlBeijing1000502.JilinCityInstituteforDrugControlofJilinProvinceJilin1320013.PharmacopoeiaCommissionofthePeople’sRepublicofChinaBeijing100061AbstractTheconceptsanddetectingmethodsforLimitofDetectionandLimitofQuantificationwerediscussedbasedontheanalysisandcomparisonwithIUPACICHandtheotherrelatedfieldsdomestic.Severaldifferentdetectionmethodswerecomparedbythetestexperiments.Thesuggestionswereputforwardfortheprovisionofthedetectingmethods.Keywordslimitofdetectionlimitofquantification《》2005“”“”、。2010《》。、、。1“”1“”。“”“”。“”“”“”。。2-3。1.1“”4-6。1975IUPAC。IUPAC“”。1998IUPAC《》IUPACCompendiumofAnalysisNomencla-ture7xLCLqL20。CL=ksb/mCL－m－sb－k－23。ICH1996201213134DrugStandardsofChina2012Vol.13No.18DL=3.3σSσ－S－。σ。1.2ICH83371.2.1。。1mL0.04mg。1mL10mL1～9μL0.0040.0120.0200.0280.036μg1μL3μL0.040.12μg、0.012μg1。11～70.004μg～0.12μg891.2.23∶12∶1。。1.2.3。、。12～20CL=kisic珔XCL－ki－23si－c－珚X－。ICH。1.2.49-10σsosi。IUPAC。0IUPAC2。2VBxXi。Xi±VBx0aVBYaYcX0Xc=VBxX=0YNXNYN=a+2VBYXN=YN－abDrugStandardsofChina2012Vol.13No.1201213135a－b－abSYXcXNXB。MDLEstimator。4AgilentTC-C18-20mmol·L－10～15min5%→15%15～25min15%→45%。、、、1mL0.1mg0.5g75%10mL15min2mL0.250.50.751.01.25mL70%5mL。5μL5。MDLEstimatorMDL、ICH、。3μg·mL－11。13DL=3.3σSCL=kisic珚XMDLEstimator0.01930.01840.02550.00740.00730.01270.00740.00870.01840.00150.00150.0035ICH。2。ICH。2“”“”、。“。。。10∶1”。ICH、。《》。1016。RSD%＜3%/＜2%。QL=10σSσ－S－。。“＜”。。3“”“”。。“”。。。、。1S．2010．．2010．130-131．2．J．200716372-73．3．J．20084272155-157．4GB/T13966-1992S．5GB/T4470-1998、S．6GB/T5009．1-2003S．7IUPACCompendiumofAnalyticalNomenclature1998．8ICH．ValidationofAnalyticalProceduresMethodologyQ2B．9．—IUPACJ．199321101232-1236.10．J．199615676-80．