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                                                            • ICH, FDA Bioanalytical Method Validation And Qualification Services Lab

                                                            20+ Years Expertise In ICH Or FDA Bioanalytical Method Validation Services GLP Or Fit-For-Purpose!

                                                            • FDA Audited Bioanalytical Method Validation For Your Pharmacokinetic (PK) Studies & Biomarker Assays
                                                            • Streamlined FDA Bioanalytical Method Validation For Your LC-MS Analysis, ELISA, Luminex, MSD, Or RT-qPCR Assay
                                                            • Full-Service Bioanalytical CRO Lab For Assay Troubleshooting, GLP Method Validation, & Stability Testing Services
                                                            • High-Value, Custom Bioanalytical Method Validation For Small-Medium Companies At Industry-Leading Turnaround

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                                                            Scientist For Bioanalytical Method Validation | NorthEast BioLab
                                                            Click below for answers to your Bioanalytical Method Validation questions -
                                                            • What is FDA or ICH Bioanalytical Method Validation?
                                                              What is FDA or ICH Bioanalytical Method Validation?
                                                            • Which Bioanalytical Method Validation services do we offer?
                                                              Which Bioanalytical Method Validation services do we offer?
                                                            • Why choose us for your FDA or ICH Bioanalytical Method Validation?
                                                              Why choose us for your FDA or ICH Bioanalytical Method Validation?
                                                            • How is Bioanalytical Method Validation performed?
                                                              How is Bioanalytical Method Validation performed?

                                                            Ask Us About Your Study

                                                            • Compliance with the latest FDA and ICH guidelines for chromatographic assays (CCs) and ligand binding assays (LBAs)
                                                            • Qualification ensures the method is fit for purpose before full validation
                                                            • Validation confirms method reliability through detailed experiments
                                                            • Includes testing Reference Standards, Calibration Curve, Quality Controls (QCs), Selectivity, Specificity, Sensitivity, Matrix Effects, Extraction Recovery, and Carryover
                                                            • Three or six independent validation runs over multiple days to measure Intraday and Interday Accuracy and Precision
                                                            • Stability testing includes Bench-Top, Freeze-Thaw Cycles, and Short-Term ULT Stability
                                                            • Provides a full report in hyperlinked PDF format and on-site/archived documentation for regulatory submissions
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                                                            What is FDA or ICH Bioanalytical Method Validation?

                                                            Bioanalytical Method Validation: Align with FDA to ICH guidelines

                                                            Method validation is a process that is used to confirm whether the analytical procedure used for drug analysis is suitable for its intended use. Method qualification vs validation is crucial to understanding the differences between initial assessments and full-scale validation. ICH Analytical method validation, following ICH method validation guidelines, is the key to judging the quality, consistency, and reliability of sample analysis data. For most healthcare regulators, including the FDA, method qualification vs validation plays a critical role in preclinical and clinical studies, with method validation is a mandatory step in preclinical and For most healthcare regulators, including the FDA, method validation is a mandatory step in preclinical and clinical studies for pharmacokinetic and toxicokinetic evaluation to fulfill specific performance criteria. Additionally, compliance with ICH guidelines for method validation ensures adherence to global regulatory standards. Our approach also aligns with the bioanalytical method validation guidance for industry, ensuring robust methods that meet both regulatory and industry expectations.

                                                            Bioanalytical Method validation takes place in the following cases:

                                                            • Once a method has been developed, but before it has been introduced into routine use.
                                                            • When the method that was developed gets changed to the extent that’s outside the original scope of the method.
                                                            • Whenever there is a change in conditions for which the method has already been validated.
                                                            • If samples are analyzed in more than one laboratory, cross-validation is needed to ensure consistency.

                                                            When it comes to test method validation, it’s important to follow standard guidelines like FDA bioanalytical method validation guidance for industry and ICH analytical method validation. If you have your own protocols, that’s great, if not, you need to develop a method validation plan. A good method validation process will test several ICH validation parameters such as calibration range, linearity, and accuracy and precision, robustness, specificity, and process stability of the analyte. Good Documentation Practice (GDP) should be in place to ensure that a full description of the method is captured in enough details to be followed by an independent analyst later.

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                                                            User Vector
                                                            VP, Bioanalytical Development

                                                            “NorthEast BioLab is the most responsive and thorough bioanalysis lab services CRO.”

                                                            User Vector
                                                            VP, Biomarker Development 

                                                            NorthEast BioLab is a responsive, collaborative, and reliable partner

                                                            User Vector
                                                            Executive Director, Pharmacokinetics

                                                            We trust NorthEast BioLab to design and execute streamlined, impactful bioanalytical projects

                                                            User Vector
                                                            President & CSO, Biotech

                                                            We found their integrity as refreshing as readiness to provide creative scientific input and high-quality data

                                                            User Vector
                                                            Sr. Associate Dir., Clinical Trials

                                                            We have worked with NorthEast BioLab for over ten years given their commitment to highest quality bioanalytical data.

                                                            User Vector
                                                            Co-Founder, Biotech & University PI

                                                            NorthEast BioLab tremendously supported us in reproducing our critical lab discoveries for drug metabolism

                                                            User Vector
                                                            VP, PK PD Analysis

                                                            NorthEast BioLab always exceeds expectations on bioanalytical assay development, validation, and sample analysis.

                                                            User Vector
                                                            Head, Bioanalytical Development

                                                            “NorthEast BioLab goes the extra mile. We look forward to more meaningful collaborations.”

                                                            User Vector
                                                            Sr. Dir., Bioanalytical Development & QC

                                                            NorthEast BioLab offers a science-based, hands-on approach to the latest bioanalytical platforms

                                                            User Vector
                                                            SVP Quality & Compliance, Biotech

                                                            We are thrilled to complete our bioanalytical studies with their top quality and incredibly responsive team.

                                                            User Vector
                                                            Director, PK

                                                            We worked closely to implement the most efficient and cost-effective bioanalytical assay for our PK Studies.

                                                            User Vector
                                                            VP, Head of Clinical Operations

                                                            Our projects with NorthEast BioLab include successful method development, validation, stability studies during Clinical Phase I – IV studies.

                                                            User Vector
                                                            Executive Director, Drug Research

                                                            NorthEast BioLab provides critical insight, and are compliant with regulatory standards and industry best practices. We highly recommend them and look forward to working together again.

                                                            User Vector
                                                            Dir., Bioequivalence Testing

                                                            Our latest successful study was a pivotal bioequivalence study, where samples from a cross-over study with about 100 volunteers needed swift analysis.

                                                            User Vector
                                                            Head, PK

                                                            This study, same as all other bioanalytical studies, was completed with top quality and reporting standard with incredible responsiveness.

                                                            User Vector
                                                            VP, Development Operations

                                                            NorthEast BioLab’s scientists deliver high-quality data on time and within budget

                                                            Tackle Your ICH, FDA Bioanalytical Method Validation And Qualification!

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                                                            Which Bioanalytical Method Validation services do we offer?

                                                            Bioanalytical Method Validation Services by NorthEast BioLab

                                                            We offer a comprehensive suite of bioanalytical method development and validation services to meet your research and regulatory needs.

                                                            Services:

                                                            Pharmacokinetics (PK) Study

                                                            We deliver precise pharmacokinetic analysis to assess drug absorption, distribution, metabolism, and excretion, vital for understanding pharmacological profiles.

                                                            ADA/Neutralizing Antibody Assay

                                                            Our assays are designed to accurately assess immunogenicity by detecting antidrug antibodies and neutralizing antibodies in clinical samples, essential for biopharmaceutical evaluations.

                                                            Cytokine/Biomarker Analysis

                                                            Utilizing highly sensitive and validated platforms, we quantify cytokines and biomarkers, offering insights into immune response, disease progression, and therapeutic outcomes.

                                                            Cell-Based Assays

                                                            Our cell-based assays ensure the reproducibility of drug screening, potency testing, and cellular response studies, providing crucial data for biologics development.

                                                            Bioanalytical Assay Validation

                                                            We ensure that all bioanalytical methods are fully validated per regulatory guidelines, offering reproducible and compliant results for both preclinical and clinical studies.

                                                            Expertise:

                                                            Mass Spectrometry (LC-MS/MS)

                                                            We specialize in LC-MS/MS for small molecule analysis, ensuring high sensitivity and specificity, making it ideal for pharmacokinetic and drug metabolism studies.

                                                            Meso Scale Discovery Assay

                                                            We develop multiplexed biomarker assays using Meso Scale Discovery technology, offering higher sensitivity, precision, and throughput than traditional methods.

                                                            ELISA Assay

                                                            ELISA development and validation services are customized to optimize sensitivity and specificity for protein and antibody detection.

                                                            qPCR/ddPCR Assay

                                                            Our qPCR and ddPCR assay expertise enables precise quantification of nucleic acids, supporting studies in gene expression and genetic variation.

                                                            Flow Cytometry

                                                            We provide advanced flow cytometry services, allowing for multi-parameter analysis of cell populations, contributing to in-depth immunological and cellular research.

                                                            Western Blot/In-Cell Western

                                                            With our expertise in traditional and in-cell Western blotting, we offer reliable quantification and detection of proteins, vital for understanding molecular biology and protein expression.

                                                            Our method development and validation services adhere to stringent regulatory guidelines, ensuring the highest level of precision, reproducibility, and compliance. This supports your drug development and research projects by delivering reliable and timely results​

                                                            Bioanalytical Method Validation Services by NorthEast BioLab

                                                            NorthEast BioLab test method validation services are extensive and adapt to the different phases of your drug development journey. Our method validation services include but are not limited to:

                                                            Full Validation of Newly Developed Methods

                                                            We are adept at validation of newly developed methods. This entails completion of full three-day validation as per regulatory guidance (FDA, ICH) on bioanalytical method validation. All experiments for the complete validation are performed, such as determination of method specificity, matrix effect and matrix suppression, extraction recovery, and carryover, etc. Analyte stability in the biological matrix is determined during short-term bench top, autosampler, and freeze-thaw stages. Additionally, we ensure compliance with ICH method validation requirements, ensuring that all processes align with global regulatory standards. Our validation process is meticulously designed to meet ICH analytical method validation criteria, reinforcing our commitment to excellence. Our approach also adheres to the bioanalytical method validation guidance for industry, ensuring comprehensive and industry-compliant validation practices.

                                                            Bioanalytical Method Validation Services | NorthEast BioLab

                                                            Registered And Inspected By Various Regulatory Agencies

                                                            • Good Laboratory Practice for Nonclinical Laboratory Studies | NorthEast BioLab
                                                            • Food and Drug Administration (FDA | NorthEast BioLab
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                                                            • United States Drug Enforcement Administration | NorthEast BioLab
                                                            • Department of Consumer Protection | NorthEast BioLab

                                                            Don’t Wait, Start Your ICH, FDA Bioanalytical Method Validation And Qualification Service Today!

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                                                            FDA or ICH Bioanalytical Method Validation | NorthEast BioLab

                                                            Why choose us for your FDA or ICH Bioanalytical Method Validation?

                                                            Achieve Bioanalytical Method Validation expectations by FDA and ICH on time and under budget

                                                            Given that drug development is an enormously resource-intensive process, finding the right Contract Research Organization can help you optimize costs and save time. At NorthEast BioLab, we have over 15 years of experience in analytical method development, method qualification vs validation, and transfer. We ensure that our processes align with ICH method validation guidelines, providing globally recognized compliance for your projects. We also rigorously adhere to ICH validation parameters, ensuring that every aspect of our validation meets the highest standards. We make sure that we accomplish our shared goals while pursuing an accelerated timeline and cost optimization.

                                                            For method validation, we offer a whole range of stringency levels so that the client can choose what they need. We generate an extremely comprehensive validation report that details the method being validated, as well as its outcomes. We also ensure that we report on the protocol used, calculations made, procedures followed, and equipment used, while distinguishing between method qualification vs validation to ensure clarity in the process. Additionally, our approach aligns with ICH analytical method validation standards to meet industry requirements and expectations.

                                                            We understand that collaboration lies at the heart of this process and ensure proper communication between our clients and our front-line lab analysts and managers. We also believe in integrity and transparency and keep our clients in the loop about all research developments. Compliance with ICH guidelines for method validation is integral to our approach, ensuring that our methods meet global standards. Additionally, we adhere to bioanalytical method validation guidance for industry, ensuring that all practices are aligned with both regulatory and industry expectations. We bring together our core strengths, operational excellence, regulatory expertise, and scientific experience to make sure that your drug development process- from drug discovery to clinical trials- flows seamlessly.

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                                                            Bioanalytical Method Validation | NorthEast BioLab

                                                            How is Bioanalytical Method Validation performed?

                                                            Bioanalytical Method Validation: Parameters and Acceptance Criteria

                                                            Specificity

                                                            The developed assay must be specific for the analyte(s) and internal standard in the blank matrix. At least six independent matrix blanks must be analyzed to show that no interferences are arising from different lots of plasma. Assay qualification ensures that the method is capable of consistently identifying and quantifying the analyte(s) in different sample matrices.

                                                            Matrix Suppression

                                                            The degree to which the signal is suppressed by the extracted components of the matrix is assessed by injecting solutions of the analyte prepared in reconstituted blank matrix extracts and comparing the signal to the analyte prepared in the mobile phase or reconstitution solution. Values are reported as percent suppression. In some instances, signal enhancement is observed.

                                                            Matrix Effect on Accuracy and Precision (6 independent lots)

                                                            The ability of the assay to accurately and reproducibly quantitate the analyte(s) in different lots of the matrix is assessed by spiking six independent lots to a concentration equivalent to the QC_Low concentration. Assay qualification is performed to ensure the method is fit for its intended purpose before full validation.

                                                            Calibration Curves: Requirements

                                                            • Calibration standards should be prepared in the matrix same as the study samples.
                                                            • Calibration curve should consist of a minimum of six concentration levels analyzed in singlet or duplicate.
                                                            • One matrix blank (Control) and one zero sample (i.e., matrix blank with IS, Control IS) should be included in each validation run.

                                                            Calibration Curves: Acceptance Criteria

                                                            • The back-calculated concentrations of the individual standards must be within accepted deviation from the nominal value.
                                                            • Deletion of calibrators should be done one at a time in a sequential manner beginning with the most deviant calibrator.
                                                            • At least 3/4th of the original calibration standards are mandatory to meet the accuracy requirements.
                                                            • The quantitation range of the study samples should not be affected by these changes. At least one standard calibrator at the LLOQ and ULQ must be within specification.
                                                            • If the quantitation range is modified, three quality control levels within the adjusted calibration range should fulfill the accuracy requirements.

                                                            Inter-day Accuracy and Precision

                                                            The inter-day accuracy and precision should be calculated using the data from three one-day validation runs. Precision is based on the percent coefficient of variation (%CV) observed by the mean of the QC samples at each QC concentration level.

                                                            Intra-day Accuracy and Precision

                                                            • Accuracy and precision should be calculated using the mean concentration results of the QC samples at each level. Precision should be based on the percent coefficient of variation (%CV) observed by the mean at each quality control concentration level.
                                                            • Dixon test for the outliers: Dixon test is applied to the percent accuracy determined for the QCs based on the theoretical and measured concentrations of the QCs from the standard curve.
                                                            • Outliers may be omitted from the precision and accuracy calculation after performing the Dixon test.

                                                            Carryover

                                                            • During method validation runs, a double-blank sample should be injected after the highest calibration standard to determine if the equipment is cross-contaminating the sample during loading.
                                                            • Peak response for the analyte(s) due to carryover must not be more than a specified % of the response of the lowest calibration standard (LLOQ). For internal standard again, the response must not be more than a determined % of the average internal standard response.

                                                            Quality Control Samples

                                                            • Quality control samples should be prepared at a minimum of four concentration levels (QC_LLOQ, QC_Low, QC_Mid, and QC_High).
                                                            • An additional QC level QC_Dil must be included in at least one of the runs to test for dilution integrity.
                                                            • Six replicates of each QC concentration levels should be analyzed in each validation run.
                                                            • Acceptance criteria for QC: The individual back-calculated concentration of each QC sample for the three in-range QC levels must be within accepted deviations from nominal.

                                                            Stability of Analyte(s)

                                                            Stability testing should include process stability, as well as short term and long-term stability of analytes in solution and in the matrix.

                                                            Ligand Binding Assays

                                                            Ligand Binding Assays (LBAs) are critical analytical techniques used to measure interactions between ligands, such as drugs or hormones, and their specific targets, including receptors or proteins. These assays are pivotal in drug development and therapeutic monitoring, allowing for the assessment of drug concentrations, biological activity, and the efficacy and safety of new therapeutics. The FDA document details various types of LBAs, including immunoassays, radioimmunoassays, enzyme-linked immunosorbent assays, and fluorescence-based assays. It also highlights the importance of validating these assays to ensure accuracy, precision, and regulatory compliance, emphasizing rigorous standards for assay design and performance to support credible results in regulatory submissions.

                                                            Batch Run Size

                                                            Batch run size depends on a variety of factors. Consideration during LC-MS analysis includes autosampler stability, run time, column stability, MS stability, etc. Here, the batch size is determined by repeat injection of blanks with QCs at regular intervals during a validation run.

                                                            Lipemic and Hemolytic Plasma Samples

                                                            High and low concentrations of QCs should be used to prepare 6 replicates with lipemic plasma (in mg/dL of lipids). Similarly, 6 replicate samples with hemolytic plasma (based on mg/dL of heme) should be analyzed.

                                                            Limit of Quantitation

                                                            The lower limit of quantitation (LLOQ) indicates the lowest concentration of study samples that can be quantitated with acceptable accuracy. The LLOQ is the lowest calibration standard used to generate a calibration curve.

                                                            Extraction Recovery of Analyte(s) and Internal Standards

                                                            • Recovery of the analyte(s) is calculated using the in-range quality control samples at three different concentration levels. The study compares the responses of the analyte(s) and IS from the validation QCs to the responses in non-extracted samples prepared in mobile phase/reconstitution solvent.
                                                            • The percent recovery of the analyte is calculated at each concentration level by dividing the mean response of the analyte (minimum of three determinations) in the matrix sample by the mean response of the analyte at that concentration in the non-extracted samples.
                                                            • The percent recovery of the internal standard is calculated by dividing the overall mean response of the internal standard in the matrix samples by the overall mean response of the internal standard in the non-extracted samples.
                                                            • Recovery studies for stable-labeled internal standards are not required, since, by definition, it is chemically like the analyte.

                                                            Maximum Solvent Concentration of Standards

                                                            • When preparing standards and QCs in a matrix such as plasma, urine, etc., the maximum amount solvent, from a stock standard(s) containing the analyte(s), should not exceed a certain percentage of the total volume.
                                                            • This can be calculated using the equation below:

                                                            % Stock Standard = spiking amount (ml) / [matrix amount (ml) + spiking amount (ml) *100

                                                            System Suitability Sample (SST)

                                                            • A system suitability sample (SST) must be developed during method validation. In general, the system suitability sample is a combination of all the expected analytes in the assay prepared in a suitable solvent system. This process underscores the concept of assay qualification vs validation, where initial qualification ensures the method’s suitability before moving on to full validation.
                                                            • Analyte(s) must be at a concentration that corresponds to the low end of the calibration curve but high enough to give a robust and reproducible signal.
                                                            • The strength and the composition of the SST solution must be documented along with a representative chromatogram generated using the SST.
                                                            • The representative chromatogram should be used as the baseline for checking if an analytical system is suitable for conducting the validated assay. The parameters to be used for system evaluation are retention time and response. Assay qualification is conducted prior to method validation to ensure the system’s suitability for consistent and accurate analyte quantification. Furthermore, assay qualification vs validation helps to ensure that the method’s performance is assessed thoroughly before full validation.

                                                            Matrix

                                                            Whenever possible, the method validation should be done in the matrices for which the assay is intended to be used. If unavailable, then evidence must be provided to demonstrate that a substitute is acceptable.

                                                            Reference Standard(s) and Internal Standard (IS) Purity

                                                            Reference standards used in the preparation of calibration and Quality Control Samples must have a Certificate of Analysis (CoA) indicating the purity and expiration date. A CoA is not required for the internal standard, but the material must be checked for impurities that may interfere with the analyte(s).

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                                                            Related FAQs

                                                            Answers to additional Method Validation questions popular among our potential clients.

                                                            What's the difference between assay qualification and validation?

                                                            Qualification: Ensures method suitability before validation.
                                                            Validation: Confirms method reliability through detailed experiments.

                                                            What experiments are included in validation?

                                                            Includes testing Reference Standards, Calibration Curve, QCs, and various method attributes.

                                                            How many validation runs are done and what do they measure?

                                                            Three or six runs over multiple days are needed to assess the accuracy and precision of CCs and LBAs.

                                                            What stability tests are performed?

                                                            Bench-Top, Freeze-Thaw Cycles, Short-Term ULT Stability.

                                                            What documentation is provided for FDA and ICH submissions?

                                                            A Full report in PDF format and on-site/archived documentation.

                                                            What is partial validation?

                                                            Partial validation evaluates previously validated methods with recommended modifications. It can range from a single intra-assay precision check to a full validation. Raw data from partial validation is retained and may be requested during inspections.

                                                            Can you use previously validated methods for new projects?

                                                            Yes, we offer methods for non-proprietary compounds that have already been validated. We ensure the approach is suitable for the current drug development stage, which helps speed up development and optimize resources.

                                                            When is re-validation of a method necessary?

                                                            Re-validation may be required when analyzing new compounds, changing the sample matrix, or updating the method according to new regulatory guidelines.

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                                                            • Western Blot, In Cell Western

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                                                            • Bioanalytical Assay Validation

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