CDER评审官指南《色谱分析方法的验证》CenterforDrugEvaluation.docx

CDER评审官指南《色谱分析方法的验证》CenterforDrugEvaluation.docx

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CDER评审官指南《色谱分析方法的验证》CenterforDrugEvaluation

CDER评审官指南《色谱分析方法的验证》Center-for-Drug-Evaluation

CenterforDrugEvaluation

andResearch（CDER）

ReviewerGuidance

Validationof

ChromatographicMethods

November1994

CMC3

率............................................……………………..16

G.Robustness耐久性..........................................…………………….16

H.SampleSolutionStability供试品溶液的稳定性.....................……………………...17

I.Specificity/selectivity专属性/选择性............................………………………17

J.SystemSuitabilitySpecificationsandTests系统适用性规定和试验....…….………………21

1.Capacityfactor容量因子...............................……………………………...22

2.Precision/Injectionrepeatability精密度/进样重复性...........…………………………….22

3.Relativeretention相对保留时间............................…………………………….22

4.Resolution分离度…….................................………………………………22

5.Tailingfactor拖尾因子...................................…………………………….23

6.Theoreticalplatenumber理论塔板数...................…..…………………………..26

K.GeneralPointstoConsider要点...............................…………………….28

V.COMMENTSANDCONCLUSIONS注解和结论.........................……………..29

VI.ACKNOWLEDGEMENTS致谢.................................…..…………….29

VII.REFERENCES参考文献..........................................…………….29

1ThisguidancehasbeenpreparedbytheAnalyticalMethodsTechnicalCommitteeoftheChemistryManufacturingControlsCoordinatingCommittee（CMCCC）oftheCenterforDrugEvaluationandResearchattheFoodandDrugAdministration.AlthoughthisguidancedoesnotcreateorconferanyrightsfororonanypersonanddoesnotoperatetobindFDAortheindustry,itdoesrepresenttheagency’scurrentthinkingonthevalidationofchromatographicmethods.Foradditionalcopiesofthisguidance,contacttheDivisionofCommunicationsManagement,HFD-210,CDER,FDA,5600FishersLane,Rockville,MD20857（Phone:

301-594-1012）.Sendoneself-addressedadhesivelabeltoassisttheofficesinprocessingyourrequest.AnelectronicversionofthisguidanceisalsoavailableviaInternettheWorldWideWeb（WWW）（connecttotheFDAHomePageatWWW.FDA.GOV/CDERandgotothe“RegulatoryGuidance”section）.

REVIEWERGUIDANCE1VALIDATIONOFCHROMATOGRAPHICMETHODS

I.INTRODUCTION

Thepurposeofthistechnicalreviewguideistopresenttheissuestoconsiderwhenevaluatingchromatographictestmethodsfromaregulatoryperspective.ThedocumentdiscussesthepointstonoteandweaknessesofchromatographysothatCDERreviewerscanensurethatthemethod'sperformanceclaimsareproperlyevaluated,andthatsufficientinformationisavailableforthefieldchemisttoassessthemethod.Analyticalterms,asdefinedbytheInternationalConferenceofHarmonization（ICH）,1993,havebeenincorporatedinthisguide.

本技术指南的目的是给审评人员审评验证色谱方法的,该文件讨论色谱方法的要点和不足,以便CDER的审评人员能够保证方法的良好性能，也使化学工作者了解为通过审评应给出的足够的信息。

国际协调会议（ICH）1993年定义的分析术语，已在这一指南中运用。

Chromatographicmethodsarecommonlyusedforthequantitativeandqualitativeanalysisofrawmaterials,drugsubstances,drugproductsandcompoundsinbiologicalfluids.Thecomponentsmonitoredincludechiralorachiraldrug,processimpurities,residualsolvents,excipientssuchaspreservatives,degradationproducts,extractablesandleachablesfromcontainerandclosureormanufacturingprocess,pesticideindrugproductfromplantorigin,andmetabolites.

色谱方法通常用于原料、药物、药物制剂和生物体液中化合物的定性和定量。

涉及的成分包括手性的或非手性的药物、过程杂质、残留溶媒、附加剂如防腐剂、分解产物、从容器和密闭包装或制造过程中带入的可提取和可过滤的杂质、植物药中的农药和代谢物等。

Theobjectiveofatestmethodistogeneratereliableandaccuratedataregardlessofwhetheritisforacceptance,release,stabilityorpharmacokineticsstudy.Dataaregeneratedforthequalitativeandquantitativetestingduringdevelopmentandpostapprovalofthedrugproducts.Thetestingincludestheacceptanceofrawmaterials,releaseofthedrugsubstancesandproducts,in-processtestingforqualityassurance,andestablishmentoftheexpirationdatingperiod.

试验方法的目的是得到可信赖的和准确的数据，无论是用于验收、出厂、稳定性或药物动力学研究。

得到的数据用于药品开发或批准后的定性和定量，试验包括原料的验收、药物和药物制剂的出厂、过程检验（In-processtesting）的质量保证和失效期的建立。

Validationofamethodistheprocessbywhichamethodistestedbythedeveloperoruserforreliability,accuracyandprecisenessofitsintendedpurpose.DatathusgeneratedbecomepartofthemethodsvalidationpackagesubmittedtoCDER.

方法的验证是由药品的开发者或使用者来检验其方法是否达到预期的可靠性、准确度和精密度的过程。

得到的数据成为方法的验证资料的一部分交给CDER.。

Methodsvalidationshouldnotbeaone-timesituationtofulfilAgencyfilingrequirements,buttheme