What is method validation?

Method validation is the process of generating documented evidence that an analytical procedure is fit for its intended purpose. It assesses defined performance characteristics against predetermined acceptance criteria, and records the outcome in a formal report.

What is the difference between method development and method validation?

Method development creates and optimises the analytical procedure so that it works. Method validation then demonstrates and documents that it works, against defined acceptance criteria.

Which performance characteristics need to be validated?

It depends on the purpose of the method. We agree the applicable set with you at the protocol stage.

How long does a method validation study take?

Timescales depend on the number of performance characteristics required, the complexity of the matrix and the amount of experimental work involved. We give an indicative timescale once the protocol scope is agreed.

What do you need from us to start a validation study?

The written method, a description of the sample matrix and expected concentration range, the intended purpose of the method and any regulatory context, plus any acceptance criteria you have already defined. Representative samples, reference standards and safety data are needed before laboratory work begins.

What happens if the method fails validation?

We report the failure clearly, with the data showing which criterion was not met and why. In most cases the method can be refined and revalidated, with often a targeted change to sample preparation or instrument conditions. We will set out what we think is required rather than simply returning a negative result.

Do you provide the validation documentation we need for an audit?

Yes. Every study is issued with a formal validation report covering the protocol, raw data, statistical evaluation, any deviations and the conclusion against acceptance criteria.

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Method Validation Services

Independent method validation that proves your analytical procedure performs as intended

Exeter Analytical (UK) Ltd provides analytical method validation services for organisations that need documented evidence that a testing method is fit for its intended purpose. From our UKAS accredited laboratory, we design and execute validation studies for pharmaceutical, chemical, agrochemical, battery technology and industrial materials.

A method that works is not the same as a method you can prove works. Method validation generates the objective data that regulators, auditors and customers expect before a method is relied upon for batch release, product specification or regulatory submission.

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What Is Analytical Method Validation?

Analytical method validation is the process of generating documented evidence that an analytical procedure is suitable for its intended purpose. Through planned experimental work against a predefined acceptance criterion, it demonstrates that a method produces results of the required accuracy, precision and reliability for the analyte and matrix in question.

Method validation is distinct from method development. Development builds the procedure and optimises it to work. Validation proves it works and records the proof. Development asks, can we measure this reliably? Validation asks can we demonstrate it, to a standard someone else will accept?

A validation study typically requires:
• A written protocol defining the performance characteristics to be assessed
• Predefined acceptance criteria appropriate to the method’s purpose
• Planned experimental work generating sufficient data to evaluate each characteristic
• Statistical evaluation of the results against those criteria
• A formal report documenting the study, the data and the conclusion

The scope of method validation depends on what the method is for. An identification test, a quantitative assay, an impurity limit test and a trace-level determination each require a different combination of performance characteristics.

Validation Performance Characteristics We Assess

Specificity And Selectivity

Confirmation that the method measures the intended analyte without interference from matrix components, impurities, degradation products present in the sample.

Accuracy

The closeness of measured results to a true or accepted reference value, typically assessed through studies compared to a reference method or certified material.

Precision

Agreement between repeated measurements. The appropriate level at which this is measured is agreed at the protocol stage.

Linearity And Response

The relationship between analyte concentration and instrument response across the working range, evaluated statistically to confirm the calibration model is appropriate.

Our method validation studies evaluate the performance characteristics relevant to your method and its intended application.

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Range

The interval between the upper and lower concentrations over which the method has been demonstrated to deliver acceptable accuracy, precision and linearity.

Detection Limit (LOD)

The lowest analyte concentration that can be reliably detected, though not necessarily quantified. Critical for limit tests and contamination screening.

Quantitation Limit (LOQ)

The lowest concentration that can be quantified with acceptable accuracy and precision, which determines whether a method can support your specification limits.

Robustness

The method’s capacity to remain unaffected by small, deliberate variations in operating parameters — the characteristic that determines whether a method survives routine use rather than performing only under ideal conditions.

Solution And Sample Stability

Where relevant, confirmation that samples, standards and prepared solutions remain stable across the timeframe of a realistic analytical run.

Our Method Validation Process

1. Scoping and Protocol Design

We review the method, its intended application. Then agree which performance characteristics are required and what acceptance criteria apply. The protocol is written and agreed with you before any laboratory work begins. This is where most validation problems are avoided.

2. Pre-Validation Assessment

Where a method has not previously been assessed, we carry out preliminary checks to confirm it is stable enough to validate. Running a full validation on a method that is not ready is an expensive way to discover it needs more development work.

3. Execution of The Validation Study

The planned experimental work is carried out by experienced analysts on calibrated instrumentation, with full data traceability.

4. Data Evaluation and Statistical Analysis

Results are evaluated against the predefined acceptance criteria, with appropriate statistical treatment of precision, linearity and recovery data.

5. Validation Report

You receive a complete report: protocol, raw data, statistical evaluation, deviations and their assessment, with a clear conclusion on whether the method meets its acceptance criteria. The written report can be used by your quality team, an auditor, or as supporting documentation in a regulatory submission.

6. Outcome and Next Steps

Where a method meets its criteria, it is ready for routine use. When it doesn’t, we tell you why and what would need to be changed.

Techniques We Validate Methods For

Validation studies are carried out across the full range of instrumentation in our laboratory, including:

• ICP-OES — trace and major element determination
• CHN elemental analysis — carbon, hydrogen, nitrogen
• Ion chromatography — anion and cation determination
• Oxygen flask combustion — fluorine, chlorine, bromine and iodine determination
• Sulphated ash
• Classical wet chemistry — titrimetric and gravimetric procedures

See the full range of elemental analysis laboratory services, or the industries we support including pharmaceuticals, energy and battery technology, agrochemicals and polymers and plastics.

Why Choose Exeter Analytical For Method Validation?

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Independent And Impartial

We have no commercial bias in the outcome of a validation study. If a method does not meet its acceptance criteria, you will be told so, with the data to explain why.

Reports Written to Be Used

Our reports can be structured for quality systems, audits and regulatory submissions.

Direct Access to The Scientists

You speak directly to the analysts running your study, not an account manager relaying questions.

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Frequently Asked Questions

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Ready To Validate Your Analytical Method?

Ensure confidence in your testing process with method validation services from our professionals. Speak with our scientists to discuss your validation requirements and quality objectives.

024 7632 3223