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SCC Requirements and

Guidance for Method
Verification and Validation
in Testing Laboratories
(RG-MVVT)
2021-05-24
Standards Council of Canada
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Ottawa, ON K1P 6L5

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Aussi offert en français sous le titre Exigences et lignes directrices du CCN – Validation des
méthodes dans les laboratoires d’essais

SCC Requirements and Guidance for Method Verification

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Table of Contents
Introduction .................................................................................................................................4
1. Scope ..................................................................................................................................4
2. Normative References .........................................................................................................4
3. Informative References ........................................................................................................5
4. Definitions ............................................................................................................................5
5. Selection of Test Methods....................................................................................................7
6. Verification of Test Methods.................................................................................................7
7. Validation Process ...............................................................................................................8
7.1. Extent of Validation .......................................................................................................8
7.2. Performance Characteristics and Criteria of a Test Method ..........................................9
7.3. Approaches used in Validations ..................................................................................10
7.4. Uncertainty Evaluation ................................................................................................10
8. Documentation ...................................................................................................................11
Annex A: Performance Characteristics (parameters) to be considered by the laboratory when
conducting method development and validation: .......................................................................12
Annex B: Guideline for validation of test methods in Agriculture Inputs, Food, Animal Plant-
Protection (AFAP) - PSA ...........................................................................................................14

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Introduction
The Standards Council of Canada (SCC) recognises the significance of method validation as a
key requirement to deliver meaningful and reliable results. Method validation is a process that
requires several steps in selecting appropriate methods and procedures for all laboratory
activities, followed by verification or validation depending on the category of the method.

This document sets out the requirements for, and gives guidance to, applicant and accredited
laboratories about the interpretation of the validation requirements for all types of test methods
as described in clause 7.2 “Selection, verification and validation of methods” of ISO/IEC
17025:2017.

1. Scope
These general guidelines shall apply to all types of laboratory activities including sampling,
regardless of field for the interpretation of the validation and verification requirements for testing
methods and additional requirements applicable to most common types of testing. Additional
program or sector-specific requirements for validation as outlined in specific Program Specialty
Area (PSA) documents will also apply.

2. Normative References
• ISO/IEC 17025:2017 General requirements for the competence of testing and calibration
laboratories.
• ISO/IEC Guide 99:2007 International Vocabulary of metrology- Basic and general concepts
and associate terms (VIM)
• International vocabulary of metrology – Basic and general concepts and associated terms
(VIM), JCGM 200:2012, GUM 2008 with minor corrections
• SCC Requirements and Guidance for the Accreditation of Testing Laboratories.
• SCC Requirements and Guidance for Accreditation of Laboratories Engaged in Test Method
Development and Non-Routine Testing
• SCC Requirements and Guidance for the Accreditation for Forensic Testing Laboratories.
• SCC Guidelines for the Presentation of Laboratory Scopes of Accreditation.
• Eurachem/CITAC Guide, The Fitness for Purpose of Analytical Methods. A Laboratory
Guide to Method Validation and Related Topics. 2nd edition, 2014.
• Eurachem/CITAC Guide, Quality Assurance for Research and Development and Non-
routine Analysis, 1st edition, 1998.
• Eurachem/CITAC Guide CG4, Quantifying uncertainty in analytical measurement, 3rd
edition, 2012.

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• Evaluation of measurement data – guide to the expression of uncertainty in measurement,
Joint Committee for Guides in Metrology, JCGM 100:2008, GUM 1995 with minor
corrections.
• IUPAC - Harmonized Guidelines for Single Laboratory Validations of Methods of analysis.
Pure Appl. Chem. 74(5), 2002, p 835-855.
• Health Canada Compendium Methods for Chemical and Microbiological Analysis of Foods,
https://www.canada.ca/en/health-canada/services/food-nutrition/research-programs-
analytical-methods.html
• Official Journal of the European Communities (2002) Commission Decision of 12 August
2002 Implementing Council Directive 96/23/EC Concerning the Performance of Analytical
Methods and the Interpretation of Results. Official Journal of the European Union, C (2002),
3044

3. Informative References
• Supplement to Eurachem Guide on the Fitness for Purpose of Analytical Methods, Planning
and Reporting Method Validation Studies, Planning and Reporting Method Validation
Studies –, 1st edition,2019).
• Eurachem/CITAC Guide, Setting and Using Target Uncertainty in Chemical Measurement,
1st edition,2015).
• ILAC G19:08/2014 Modules in a Forensic Science Process.
• AOAC INTERNATIONAL Methods Committee Guidelines for Validation of Qualitative and
Quantitative Food Official Methods of Analysis. J AOAC Int’l 85(5) 2002, p.1187-1200.
• Protocol for the Design, Conduct and Interpretation of Collaborative Studies. Pure Appl.
Chem, 60(6), 1988, p 855-864.

4. Definitions
Method: similar to “measurement procedure” defined in Guide 99.
Measurement procedure: a set of operations, described specifically, used in the performance
of particular measurements according to a given method. It is usually recorded in a document
that sometimes itself called a “measurement procedure” (or a measurement method) and is
usually insufficient detail to enable an operator to carry out a measurement without additional
information. (Guide 99)
Measurement procedure (JCGM 200, item 2.6): detailed description of a measurement
according to one or more measurement principles and to a given measurement method, based
on a measurement model and including any calculation to obtain a measurement result
NOTE 1: A measurement procedure is usually documented in sufficient detail to enable an
operator to perform a measurement.
NOTE 2: A measurement procedure can include a statement concerning a target measurement
uncertainty.

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NOTE 3 A measurement procedure is sometimes called a standard operating procedure,
abbreviated SOP.

Verification (referred to as Method Verification): The process of ensuring that the laboratory
has the ability to perform a previously validated method consistent with the requirements of the
method and the needs of the laboratory.

Validation (referred to as Method Validation): The process of ensuring that a method has the
capabilities and performance characteristics consistent with specified requirements and that it’s
fit for the intended use and designed application.

Fitness for Purpose: (IUPAC Harmonized Guidelines for Single Laboratory Validations of
Methods of analysis.): It is the extent to which the performance of a method matches the
criteria, agreed between the analyst and the end-user of the data, that describe the end-user’s
needs. Fitness-for-purpose criteria will ultimately be expressed in terms of acceptable combined
uncertainty.

Standard Published Method: international, regional or national standards or other recognized

reputable technical organizations available in the latest valid version or in relevant scientific
texts or journals, or as specified by the manufacturer of the equipment unless it is not
appropriate or possible to do so (ISO/IEC 17025, clause 7.2.1.4)

Modified method: standard and non-standard methods used outside their intended scope or
otherwise modified.

In-house method: A method in-house developed by the laboratory for its own use.
(e.g. laboratory-developed method)

Performance criteria: requirements for a performance characteristic according to which it can

be judged that the analytical method is fit for the purpose and generates reliable results (EC
Directive, 2002).

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5. Selection of Test Methods
Often, the customer specifies the method to be used, which may or may not be a standard
published method. Standard published methods are preferred, but the laboratory may use ones
published by technical organizations, supplied by equipment manufacturers, published in
scientific literature, or developed by the laboratory, provided the customer is in agreement and
these non-standard methods have been validated before use. The degree of validation required
will be discussed in Section 7.

Validation does not apply to standard published methods in terms of the requirement of ISO/IEC
17025 clause 7.2.2. Verification does apply to standard published methods as described in
clause 7.2.1. of ISO/IEC 17025.

It is recognized that for laboratories to be responsive to customer’s needs and changing

technology, new methods will need to be implemented or existing methods modified on a
regular basis. Refer to the following documents designed to address some of these issues
within the following Program Specialty Areas:
• SCC Requirements and Guidance for Accreditation of Laboratories Engaged in Test
Method Development and Non-Routine Testing.
• SCC Requirements and Guidance for the Accreditation for Forensic Testing Laboratories

6. Verification of Test Methods

Modified methods may consist of deviation(s) from a standard reference method or a
prescriptive procedure for use on an on-going basis. If the laboratory can demonstrate the
deviation(s) is (are) not significant, then a verification according to clause 7.2.1 of ISO/IEC
17025 standard will be required.

The laboratory shall verify that it can properly perform methods before introducing them by
ensuring that it can achieve the documented performance characteristics according to clause
7.2.1.5 of ISO/IEC 17025.

When standard published methods are adopted by the laboratory without significant deviations,
verification is required under following examples but may not be limited to:

• Confirmation that the implementation of the standard published method is fit for the
intended purpose (e.g. precision, bias, linearity, interference, robustness, grounding,
linearity, electrical connections, physical stability are consistent with the ones published
in the reference method);
• Estimation of key performance parameters such as method detection limit (MDL),
reporting limit (RL) or signal-to-noise ratio for representative matrices, or types of
samples under test (Annex A for examples of performance parameters).
• Evaluation of measurement uncertainty;
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 • Confirmation that the method works reliably and accurately with the typical samples
processed (e.g. acceptable spiked sample recovery, or comparison against an
independent reference or other validated test method);
• Confirmation that any decision rule associated with the method is valid for the
laboratory's implementation.

If guidelines within a particular PSA specify verification requirements, these shall also be
followed.

7. Validation Process
7.1. Extent of Validation
Validation shall apply for the following categories of method according to clause 7.2.2.1 of
ISO/IEC 17025:
• non-standard methods (in-house);
• laboratory-designed/developed methods (in-house);
• standard methods used outside their intended scope (modified);
• significant modifications of standard methods that could impact the reliability of results
(modified).

The stated purpose of the validation is to confirm that the methods are fit for the intended use.
In addition, clause 7.2.2. states that:
“The validation shall be as extensive as is necessary to meet the needs of the given application
or field of application”.

The table below is meant to summarize requirements based on verification or validation of

categories of test methods commonly performed in testing laboratories.

Test method category Validation or verification requirements

Standard Published Method Verification of published performance
characteristics against the laboratory’s
method performance in accordance with the
requirement of ISO/IEC 17025 clause 7.2.1.5.
Standard Published Method that has been Validation is required and the extent will vary
modified by the laboratory or another entity based on the risk associated with the
conducted analysis.
(e.g. different matrices, concentration ranges,
analytes, standard published method used or
a similar purpose but different conditions)

In-house developed method Validation

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 Method published in the scientific literature Validation
with/without any performance data

Changes in implementation of a previously Verification will suffice. The extent will vary in
validated method (e.g. changes to order to demonstrate changes do not have a
equipment, reagents, lab environment or significant impact on performance
staff) characteristics.

Archived standard published or previously Verification of previous performance

validated method that is reinstated characteristics

Ad hoc or special analyses Extent of validation limited by circumstance

Commercial Test Kits - collaboratively tested, Verification of published performance

third party evaluation (e.g. AOAC) characteristics but validation may be required
if any changes are made.

Commercial Test Kits - no performance data Validation

available, incomplete or not applicable for the
matrix being tested
Instrument manufacturer’s method which is Verification if instrument manufacturer’s
not published in a scientific journal method criteria is available and complete.
Validation if instrument manufacturer’s
method criteria is not present or incomplete.

7.2. Performance Characteristics and Criteria of a Test

Method
Refer to Annex A of this document for a list of applicable parameters (characteristics). Validation
should also evaluate sampling, sub-sampling and transportation of samples to the laboratory,
where these can affect the method outcome or where there are sample acceptance criteria and
where the laboratory is responsible for these activities. Also, to be considered are
interpretations of population results, incorporating statistics as applicable. Where the laboratory
is responsible for sampling or sub-sampling, the method validation shall ensure that there are
no negative impacts on population results. Statistics may be used as applicable. The
terminology used to describe the performance characteristic may vary among disciplines and
should be defined by the laboratory as necessary for clarity (see Annex A for examples).

In addition to relevant parameters (characteristics), a validation summary should include the

following:
• Reference (e.g. identify technical records for more details)
• Measurand
• Type of sample(s), (e.g. description of the tested matrices)
• Type of measurement (e.g. qualitative, semi-quantitative, quantitative, determinative)
• Method status (routine or non-routine)

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• Description of the intended use (e.g., legal, regulation, as agreed with customer
[screening, confirmatory, exploratory, process control, others])

In some disciplines, the guidelines available to the laboratory testing community are extensive.
It is therefore the responsibility of the laboratory, with input from customers, to seek out the
relevant characteristics to be evaluated with respect to the laboratory’s specific situation and the
customer’s needs. The laboratory must have a documented validation plan, either to be used
generally or applied to a specific project or customer. Test method performance characteristics
to be evaluated will vary with the type of test and its intended use. Discipline-specific or
customer required performance criteria are to be applied to demonstrate fitness for purpose.

7.3. Approaches used in Validations

Validations must address the reliability (or repeatability) and reproducibility of the test method
and also the ability to produce correct results which are related to the accuracy or trueness of
results. To demonstrate accuracy, there must be a comparison against an independent known
reference resulting in consistent outcomes and maintaining metrological traceability.
Materials used to evaluate test method performance must be representative of those to be
analyzed when the test method is in routine use. Certified reference materials should be used
to assess trueness, when available. Previously analysed proficiency testing samples, such as
those available from proficiency testing exercises can be used to assess bias. However,
reference materials can underestimate the variation seen in test samples. The use of naturally
contaminated or naturally occurring samples if available should be considered. The method
under validation can be compared to an established standard method and the bias between the
two methods determined. Often reference materials or a standard method are not available.
Recovery studies are conducted by spiking field blanks with a known amount of analyte or
organism. Blanks must be representative of typical samples received for testing, so validations
may need to be conducted on several different blanks obtained from several sources. In many
biological systems, experiments are conducted to generate naturally occurring materials.

7.4. Uncertainty Evaluation

A robust estimation of measurement uncertainty must be performed as part of the validation.
Some standard methods have already published uncertainties which should be used as a
starting point in determining the laboratory’s own evaluation. Please refer to SCC Requirements
and Guidance for the Accreditation of Testing Laboratories, clause 7.6 for further details.

For detailed discussions of uncertainty evaluations in validation studies see the following:
• Eurachem / CITAC Guide, Quantifying Uncertainty in Analytical Measurement
• IUPAC’s Harmonized Guidelines for Single-Laboratory Validation of Methods of Analysis
(Appendices A14 and B)
• Evaluation of measurement data – guide to the expression of uncertainty in measurement,
JCGM 100:2008, GUM 1995 with minor corrections.

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It is important to recognize that some significant sources of uncertainty may not be covered in
multi-laboratory or single laboratory validations. Ruggedness testing conducted during the
validation study can provide information of the effect of some parameters. The Eurachem Guide
recommends that precision should be estimated over time and to include the natural variation of
all factors. This includes data generated by quality control samples, replicates, proficiency
testing material, etc.

For quantitative and semi-quantitative method, an estimate of uncertainty is required, while for
qualitative methods an identification of sources of uncertainty and under which conditions they
are controlled is necessary.

8. Documentation
The laboratory must have available for review indexed records, summarizing the detailed
method validation / verification data for all non-standard, in-house developed or modifications
and amplifications of standard published methods. These records shall include:

• The test method including information about equipment, reagents, calibration etc.
• Reference to the validation procedure or plan used to generate method performance
characteristics.
• Test method performance characteristics and how these were calculated or defined.
The raw data should be available for review.
• Test method performance criteria against which the characteristics were evaluated and
whether or not the method is fit for purpose.
• Review and authorization of the report by a competent authorized person.
• The intended use of the method including relevant matrices.
• Estimates of uncertainty.

If a method that is not a standard published method is used routinely, often over time there will
be modifications or improvements made. This information needs to be documented and
available for assessment. Ongoing proficiency testing data and quality control data should be
reviewed by the laboratory to confirm the fitness of the method. The validation/verification
information shall be kept according to the timeline established by the laboratory under the
requirements of clause 8.4.2 of ISO 17025.

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Annex A: Performance Characteristics
(parameters) to be considered by the laboratory
when conducting method development and
validation:
The list below serves as a guide for characteristics or parameters that a laboratory should
consider when developing and validating a test method. Performance characteristics
(parameters) and the acceptance criteria used to evaluate the performance characteristics shall
take into account:

 the intended use of the test method including customer needs: “the extent of validation, and
the consequences in time and cost, are one of the key issues to be agreed upon between
analyst and customer when commissioning method development.” (Eurachem/ CITAC
Guide - Quality Assurance for Research and Development and Non-routine Analysis,
section 6.8.5.4)
 the discipline: some characteristics, including the definitions, are discipline or test type
specific.
 the type of test (qualitative, quantitative) and purpose (screening, confirmatory).

Characteristics or criteria to be considered may include, but are not limited to:
• Accuracy
• Action levels (for regulatory analyses)
• Analytical specificity* (selectivity, exclusivity, inclusivity)
• Calibration (see linearity, range)
• Confirmation
• Diagnostic selectivity*, Diagnostic sensitivity*
• Efficacy
• False positive rate, False negative rate (paired studies)
• Ion Suppression for LC/MS or LC/MSMS assay
• Limit of detection (detection capability, decision limit, level of detection)
• Limit of determination (limit of quantitation)
• Linearity (calibration, range)
• Measurement bias
• Measurement uncertainty
• Precision
• Predictive value
• Probability of detection (unpaired studies)
• Range (see calibration, linearity)
• Recovery
• Relative Sensitivity, Relative Specificity
• Repeatability
• Reporting limit
• Reproducibility
• Ruggedness/robustness
• Selectivity*, Sensitivity*, Specificity*
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• Stability (of analyte, organism, sub-samples, extracts)
• Target organisms
• Test controls (including reference populations)
• Thresholds

* Definitions for some terms may vary among disciplines. For example, the term, “selectivity,” is
recommended for analytical chemistry instead of “specificity” (see IUPAC definition). Some
definitions such as analytical specificity, diagnostic selectivity and diagnostic sensitivity are used
in biological testing.

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Annex B: Guideline for validation of test methods
in Agriculture Inputs, Food, Animal Plant-
Protection (AFAP) - PSA
In some sectors, validation typically refers to interlaboratory studies such as those conducted by
a sector-specific technical organization. A test method is evaluated with different analysts in a
number of different laboratories usually using different equipment and materials. For example,
AOAC International organizes collaborative studies in food analysis. Interlaboratory validation
may be a requirement in some fields of regulatory analyses. The International Union of Pure
and Applied Chemistry (IUPAC) published Protocol for the design, conduct and interpretation of
collaborative studies, which was accepted by 27 participating organizations as the minimum
requirement for these studies. However, due to time constraints, availability of resources and
the need to address emerging issues, new hazards or new products methods cannot always be
subjected to full interlaboratory validations. In some specialized testing areas, it is difficult to find
a sufficient number of participants.

IUPAC’s Harmonized Guidelines for Single-Laboratory Validation of Methods of analysis

provides some general guidelines for the extent of single laboratory validation studies.
For laboratories under the AFAP – PSA that are performing food microbiology under legislation
enforced by Canadian Food Inspection Agency (CFIA), the Health Canada Compendium of
Analytical Methods are validated and considered standard reference methods. These methods
are current and updated through a joint Health Canada -CFIA committee, therefore the methods
are actively used for regulatory testing. The Compendium of Methods of Analytical Methods are
ready reference methods used by Health Products and Food Branch (HPFB) of Health Canada
in the areas of food chemical analysis. Official Methods used for chemical analysis of foods are
HPB methods which are laboratory procedures for surveillance used in support of Health
Canada’s regulatory compliance inspection programs and considered validated if used as
published All the described methods are validated only for a very specific set of matrices.
Therefore, proper validation must be completed prior to using these methods for matrices
outside the original scope of the method.

The AOAC food matrix triangle is a common tool used to assist laboratories in selecting
matrices to be included in their studies. The AOAC food triangle is constructed based on the
relative levels of fat, protein and carbohydrate divided into nine sectors. Consequently,
validation is required to be performed over a wide variety of foods since subsequent steps of
preparation, extraction and testing may be different for a sample containing 100% carbohydrate
compared to a sample that is high in lipids. While planning method validation studies, samples
that are reflective of the types of samples received by the laboratory should be considered
including samples that might be a challenge to analyze (e.g. high fat, high protein, high
moisture). Analysts’ professional judgement will be required when validating a certain segment
of the food triangle; other factors should be considered such as extraction technique, solids vs.
liquid ratio and matrix interferences.
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