The Third AAPS/FDA Bioanalytical Workshop, entitled "Quantitative Bioanalytical Methods Validation and Implementation: Best Practices for Chromatographic and Ligand Binding Assays" was held on May 1-3, 2006 in Arlington, VA. The format of this workshop consisted of presentations on bioanalytical topics, followed by discussion sessions where these topics could be debated, with the goal of reaching consensus, or identifying subjects where addition input or clarification was required. The discussion also addressed bioanalytical validation requirements of regulatory agencies, with the purpose of clarifying expectations for regulatory submissions. The proceedings from each day were reviewed and summarized in the evening sessions among the speakers and moderators of the day. The consensus summary was presented back to the workshop on the last day and was further debated. This communication represents the distillate of the workshop proceedings and provides the summary of consensus reached and also contains the validation topics where no consensus was reached.

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Method validation is a process that demonstrates that a method will successfully meet or exceed the minimum standards recommended in the Food and Drug Administration (FDA) guidance for accuracy, precision, selectivity, sensitivity, reproducibility, and stability. This article discusses the validation of bioanalytical methods for small molecules with emphasis on chromatographic techniques. We present current thinking on validation requirements as described in the current FDA Guidance and subsequent 2006 Bioanalytical Methods Validation Workshop white paper.K EYWORDS: bioanalytical , validation , precision , accuracy , sensitivity , selectivity , reproducibility INTRODUCTIONBioanalytical methods are used for the quantitation of drugs and their metabolites in biological matrices. In today ' s drug development environment, highly sensitive and selective methods are required to quantify drugs in matrices such as blood, plasma, serum, or urine. Chromatographic methods (high-performance liquid chromatography [HPLC] or gas chromatography [GC]) have been widely used for the bioanalysis of small molecules, with liquid chromatography coupled to triple quadrupole mass spectrometry (LC/MS/ MS) being the single most commonly used technology. After developing a method with desired attributes, the method is validated to establish that it will continue to provide accurate, precise, and reproducible data during study-sample analysis. Method validation is a process that demonstrates that the method will successfully meet or exceed the minimum standards recommended in the Food and Drug Administration (FDA) Guidance 1 for accuracy, precision, selectivity, sensitivity, reproducibility, and stability. The validation is performed using a control matrix spiked with the compounds to be quantifi ed. This article discusses the validation of bioanalytical methods for small molecules with emphasis on chromatographic techniques. We present current thinking on validation requirements as described in the current FDA Guidance 1 and subsequent 2006 Bioanalytical Methods Validation Workshop white paper. 2 VALIDATION PARAMETERSBioanalytical methods can be developed in the laboratory conducting the validation or obtained from another laboratory or literature. The results from a method validation can be no better than the quality of the method that was developed. Thus, before beginning the method validation, it is important that the method is set up and tested in the laboratory. For methods obtained externally, modifi cations may be necessary to achieve the desired performance of the method relative to how it was developed originally. This process will help ensure that when validation begins, chances for its successful completion (and more important, successful sample analysis) are high. During method validation, values for validation parameters are obtained. The essential parameters required according to the FDA Guidance 1 are selectivity, sensitivity, accuracy, precision, reproducibility, and stability. While obtaining these parameters, other param...

Over 400 professionals representing pharmaceutical companies, CROs, and multiple regulatory agencies participated in the 6th Workshop on Recent Issues in Bioanalysis (WRIB). Like the previous sessions, this event was in the format of a practical, focused, highly interactive and informative workshop aiming for high-quality, improved regulatory compliance and scientific excellence. Numerous 'hot' topics in bioanalysis of both small and large molecules were shared and discussed, leading to consensus and recommendations among panelists and attendees representing the bioanalytical community. The major outcome of this year's workshop was the noticeable alignment of multiple bioanalytical guidance/guidelines from different regulatory agencies. This represents a concrete step forward in the global harmonization of bioanalytical activities. The present 2012 White Paper acts as a practical and useful reference document that provides key information and solutions on several topics and issues in the constantly evolving world of bioanalysis.

The 2013 7th Workshop on Recent Issues in Bioanalysis was held in Long Beach, California, USA, where close to 500 professionals from pharmaceutical and biopharmaceutical companies, CROs and regulatory agencies convened to discuss current topics of interest in bioanalysis. These 'hot' topics, which covered both small and large molecules, were the starting point for fruitful exchanges of knowledge, and sharing of ideas among speakers, panelists and attendees. The discussions led to specific recommendations pertinent to bioanalytical science. Such as the previous editions, this 2013 White Paper addresses important bioanalytical issues and provides practical answers to the topics presented, discussed and agreed upon by the global bioanalytical community attending the 7th Workshop on Recent Issues in Bioanalysis.

The 5th Workshop on Recent Issues in Bioanalysis (WRIB) was organized by the Calibration and Validation Group as a 2-day full immersion workshop for pharmaceutical companies, CROs and regulatory agencies to discuss, review, share perspectives, provide potential solutions and agree upon a consistent approach to recent issues in the bioanalysis of both small and large molecules. High quality, better compliance to regulations and scientific excellence are the foundation of this workshop. As in the previous editions of this significant event, recommendations were made and a consensus was reached among panelists and attendees, including industry leaders and regulatory experts representing the global bioanalytical community, on many 'hot' topics in bioanalysis. This 2011 White Paper is based on the conclusions from this workshop, and aims to provide a practical reference guide on those topics.

The 4th Calibration and Validation Group Workshop on Recent Issues in Regulated Bioanalysis, a 2-day full immersion workshop, was organized by the Calibration and Validation Group. Contract research organizations, pharmaceutical companies and regulatory agencies came together to discuss several 'hot' topics concerning bioanalytical issues and regulatory challenges and to reach a consensus among panelists and attendees on many points regarding method validation of small and large molecules.

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