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Bioanalytical Method,Validation,Guidance for Industry. Additional copies are available from, Office of Communications Division of Drug Information. Center for Drug Evaluation and Research,Food and Drug Administration. 10001 New Hampshire Ave Hillandale Bldg 4 th Floor. Silver Spring MD 20993 0002, Phone 855 543 3784 or 301 796 3400 Fax 301 431 6353. Email druginfo fda hhs gov, http www fda gov Drugs GuidanceComplianceRegulatoryInformation Guidances default htm.
Policy and Regulations Staff HFV 6,Center for Veterinary Medicine. Food and Drug Administration,7500 Standish Place Rockville MD 20855. http www fda gov AnimalVeterinary GuidanceComplianceEnforcement GuidanceforIndustry default htm. U S Department of Health and Human Services,Food and Drug Administration. Center for Drug Evaluation and Research CDER,Center for Veterinary Medicine CVM. Biopharmaceutics,Bioanalytical Method Validation,Contains Nonbinding Recommendations.
TABLE OF CONTENTS,I INTRODUCTION 1,II BACKGROUND 2. III BIOANALYTICAL METHOD DEVELOPMENT AND VALIDATION 4. A Guiding Principles 4,B Bioanalytical Parameters of CCs and LBAs 5. 1 Reference Standards and Critical Reagents 5,2 Calibration Curve 6. 3 Quality Control Samples 7,4 Selectivity and Specificity 7. 5 Sensitivity 8,6 Accuracy Precision and Recovery 8.
7 Stability 9,8 Dilution Effects 10,9 Partial and Cross Validations 11. C Validated Methods Expectations of In Study Analysis and Reporting 12. IV INCURRED SAMPLE REANALYSIS 14,V ADDITIONAL ISSUES 15. A Endogenous Compounds 15,B Biomarkers 15,C Diagnostic Kits 16. D Bridging Data From Multiple Bioanalytical Technologies 17. E Dried Blood Spots 18,VI DOCUMENTATION 18,A Summary Information 18. B Documentation for Method Validation and Bioanalytical Reports 19. VII APPENDIX 20, Table 1 Requirements and Acceptance Criteria for Bioanalytical Method Validation and In.
Study Conduct 20,Table 2 Documentation and Reporting 28. Table 3 Example of an Overall Summary Table for a Method Validation Report or a Clinical. Study Report 33, Table 4 Example of Summary Analytical Runs for a Bioanalytical Study Report 36. VIII GLOSSARY 37,Bioanalytical Method Validation,Contains Nonbinding Recommendations. Bioanalytical Method Validation,Guidance for Industry 1. This guidance represents the current thinking of the Food and Drug Administration FDA or Agency on. this topic It does not establish any rights for any person and is not binding on FDA or the public You. can use an alternative approach if it satisfies the requirements of the applicable statutes and regulations. To discuss an alternative approach contact the FDA office responsible for this guidance as listed on the. title page,I INTRODUCTION, This guidance helps sponsors of investigational new drug applications INDs or applicants of.
new drug applications NDAs abbreviated new drug applications ANDAs biologic license. applications BLAs and supplements validate bioanalytical methods used in human clinical. pharmacology bioavailability BA and bioequivalence BE studies that require. pharmacokinetic toxicokinetic or biomarker concentration evaluation 2 This guidance can also. inform the development of bioanalytical methods used for nonclinical studies that require. toxicokinetic or biomarker concentration data For studies related to the veterinary drug. approval process such as investigational new animal drug applications INADs new animal. drug applications NADAs and abbreviated new animal drug applications ANADAs this. guidance may apply to blood and urine BA BE and pharmacokinetic studies. The information in this guidance applies to bioanalytical procedures such as chromatographic. assays CCs and ligand binding assays LBAs that quantitatively determine the levels of drugs. their metabolites therapeutic proteins and biomarkers in biological matrices such as blood. serum plasma urine and tissue such as skin, This final guidance incorporates public comments to the revised draft published in 2013 and. provides recommendations for the development validation and in study use of bioanalytical. methods The recommendations can be modified with justification depending on the specific. type of bioanalytical method This guidance reflects advances in science and technology related. to validating bioanalytical methods, In general FDA s guidance documents do not establish legally enforceable responsibilities. Instead guidances describe the Agency s current thinking on a topic and should be viewed only. This guidance has been prepared by the Office of Clinical Pharmacology in the Center for Drug Evaluation and. Research and the Center for Veterinary Medicine at the Food and Drug Administration. This guidance applies to both sponsors and applicants The use of the word sponsor applies to both sponsors and. applicants and hence INDs NDAs BLAs and ANDAs,Bioanalytical Method Validation 1. Contains Nonbinding Recommendations, as recommendations unless specific regulatory or statutory requirements are cited The use of. the word should in Agency guidances means that something is suggested or recommended but. not required,II BACKGROUND, The 2001 guidance for industry on Bioanalytical Method Validation was originally based on the.
deliberations of two workshops described in publications entitled. Analytical Methods Validation Bioavailability Bioequivalence and Pharmacokinetic. Bioanalytical Methods Validation A Revisit With a Decade of Progress 4. Additional workshops summarized in the following publications have informed subsequent. revisions e g the 2013 draft guidance for industry entitled Bioanalytical Method Validation 5. Quantitative Bioanalytical Methods Validation and Implementation Best Practices for. Chromatographic and Ligand Binding Assays6, The AAPS FDA Workshop on Incurred Sample Reanalysis7. The AAPS Workshop on Crystal City V Quantitative Bioanalytical Method Validation. and Implementation 2013 Revised FDA Guidance8, Shah VP KK Midha S Dighe IJ McGilveray JP Skelly A Yacobi T Layloff CT Viswanathan CE Cook RD. McDowell KA Pittman S Spector 1992 Analytical Methods Validation Bioavailability Bioequivalence and. Pharmacokinetic Studies Pharm Res 9 588 592, Shah VP KK Midha JW Findlay HM Hill JD Hulse IJ McGilveray G McKay KJ Miller RN Patnaik ML. Powell A Tonelli CT Viswanathan A Yacobi 2000 Bioanalytical Methods Validation A Revisit With a Decade. of Progress Pharm Res 17 1551 1557, When final this guidance will represent the FDA s current thinking on this topic For the most recent version of a. guidance check the FDA Drugs guidance Web page at, http www fda gov Drugs GuidanceComplianceRegulatoryInformation Guidances default htm.
Viswanathan CT B Surendra B Booth AJ DeStefano MJ Rose J Sailstad VP Shah JP Skelly PG Swann R. Weiner 2007 Quantitative Bioanalytical Methods Validation and Implementation Best Practices for. Chromatographic and Ligand Binding Assays Pharm Res 24 1962 1973. Fast DM M Kelley CT Viswanathan J O Shaughnessy SP King A Chaudhary R Weiner AJ DeStefano D. Tang 2009 Workshop Report and Follow Up AAPS Workshop on Current Topics in GLP Bioanalysis Assay. Reproducibility for Incurred Samples Implications of Crystal City Recommendations AAPS J 11 238 241. Booth B ME Arnold B DeSilva L Amaravadi S Dudal E Fluhler B Gorovits SH Haidar J Kadavil S Lowes. R Nicholson M Rock M Skelly L Stevenson S Subramaniam R Weiner E Woolf 2015 Workshop Report. Bioanalytical Method Validation 2,Contains Nonbinding Recommendations. Validated analytical methods for the quantitative evaluation of analytes i e drugs including. biologic products and their metabolites and biomarkers in a given biological matrix e g blood. plasma serum or urine are critical for the successful conduct of nonclinical biopharmaceutics. and clinical pharmacology studies These validated methods provide critical data to support the. safety and effectiveness of drugs and biologic products Validating the analytical method. ensures that the data are reliable by addressing certain key questions including. Does the method measure the intended analyte For example does anything interfere. with the measurement and is the method specific or selective for the analyte. What is the variability associated with these measurements For example what are the. accuracy and precision of the method, What is the range in measurements that provide reliable data For example what is the. sensitivity of the method e g what is the lower limit of quantitation LLOQ of the. method and what is the upper limit of quantitation the method ULOQ. How do sample collection handling and storage affect the reliability of the data from the. bioanalytical method For example what steps need to be followed while collecting. samples Do the samples need to be frozen during shipping What temperatures are. required to store the samples and how long can the samples be stored. When changes are made to a validated method the sponsor should conduct additional validation. i e partial or cross validation, The fit for purpose FFP concept states that the level of validation should be appropriate for the. intended purpose of the study The key questions listed above should be evaluated relative to the. stage of drug development Pivotal studies submitted in an NDA BLA or ANDA that require. regulatory decision making for approval safety or labeling such as BE or pharmacokinetic. studies should include bioanalytical methods that are fully validated Exploratory methods that. would not be used to support regulatory decision making e g candidate selection may not. require such stringent validation This FFP concept applies to drugs their metabolites and. biomarkers, The analytical laboratory conducting toxicology studies for regulatory submissions should. adhere to 21 CFR 58 Good Laboratory Practices GLPs 9 The bioanalytical method for human. BA BE and pharmacokinetic studies must meet the criteria specified in 21 CFR 320. Bioequivalence and Bioavailability Requirements i e 21 CFR 320 29. Crystal City V Quantitative Bioanalytical Method Validation and Implementation The 2013 Revised FDA. Guidance AAPS J 17 277 288, For the Center for Veterinary Medicine all BE studies are subject to Good Laboratory Practices.
Bioanalytical Method Validation 3,Contains Nonbinding Recommendations. The following sections discuss the development validation and in study use of bioanalytical. methods and how best to document validation methods and results Refer to the Glossary for the. definitions of assay parameters and analytical terms used in this guidance. III BIOANALYTICAL METHOD DEVELOPMENT AND VALIDATION. A Guiding Principles, The purpose of bioanalytical method development is to define the design operating conditions. limitations and suitability of the method for its intended purpose and to ensure that the method is. optimized for validation, Before the development of a bioanalytical method the sponsor should understand the analyte of. interest e g determine the physicochemical properties of the drug in vitro and in vivo. metabolism and protein binding and consider aspects of any prior analytical methods that may. be applicable, The elements and acceptance criteria of method development and validation are summarized in. Table 1 Table 2 describes how the sponsor should document the development and validation of. the bioanalytical assay and where it should be stored or submitted. Method development involves optimizing the procedures and conditions involved with extracting. and detecting the analyte Method development includes the optimization of the following. bioanalytical parameters which are discussed in greater detail in section III B to ensure that the. method is suitable for validation,Reference standards.
Critical reagents,Calibration curve,Quality control samples QCs. Selectivity and specificity,Sensitivity,Stability of the analyte in the matrix. Bioanalytical method development does not require extensive record keeping or notation. However the sponsor should record the changes to procedures as well as any issues and their. resolutions during development of the bioanalytical method to provide a rationale for any. changes during the development of the method, Bioanalytical method validation proves that the optimized method is suited to the analysis of the. study samples The sponsor should,Bioanalytical Method Validation 4. Contains Nonbinding Recommendations, Conduct a full validation of any new bioanalytical method for the analysis of a new drug.
entity its metabolite s or biomarkers, Conduct a full validation for any revisions to an existing validated method that adds a. metabolite or an additional analyte, Establish a detailed written description e g protocol study plan and or standard. operating procedure SOP for the bioanalytical method before initiating validation The. description should identify procedures that control critical parameters in the method e g. environmental matrix procedural variables from the time of collection of the samples to. the time of analysis to minimize their effects on the measurement of the analyte in the. Document and report in the method validation report all experiments used to make. claims or draw conclusions about the validity of the method. Validate the measurement of each analyte in the biological matrix The specific. requirements and acceptance criteria for each bioanalytical parameter are listed in Table. Bioanalytical method development does not require extensive record keepingor notation However the sponsor should record the changes to procedures as well as any issues and their resolutions during development of the bioanalytical methodto provide a rationale for any changes during the development of the method

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