Microsoft PowerPoint - FINAL-AOAC StandardsDevDebpres8-2018

Understanding AOAC Standards Standard Method Performance Requirements, and AOAC Official Methods

AOAC Annual Meeting Toronto, Canada


• Attendees will learn:

– Types of AOAC standards – Process for developing an AOAC standard  – Process from AOAC standard to AOAC Official  Methods . – What is and the Purpose of an AOAC SMPR – AOAC Official Methods approval process – About AOAC Official Methods and the components of an Official Method


Attendees will: – be able to understand AOAC processes to develop standards. – be able to understand how the process can lead to Official First Action status. – be able to identify the various types of AOAC standards – learn about the evolution of SMPRs. – be able to distinguish between a fitness-for-purpose statement and a SMPR. – be able to recognize uses for AOAC SMPRs and AOAC standards. – be able to understand expectations for drafting an candidate method for Official Methods

Attendees will be thankful that this session is over  .

AOAC began in Washington, DC as the Association  of Official Agricultural Chemists (1884)

• Federal and state departments of  agriculture through the USDA  Bureau of Chemistry.   Initially to standardize  methodology to be used for  composition of fertilizers by state  laboratories  Directed by Harvey Washington  Wiley who wrote the 1906 law  that began the US Food and Drug  Administration (FDA) 

• By the 1980s AOAC’s membership  included microbiologist, food  science professionals • In 1991, Association of Official  Agricultural Chemists  legally  changed its name to AOAC  INTERNATIONAL  • Often referred to as Association of  Analytical Communities ‐ used to  encompass all of the scientific  disciplines involved in AOAC’s work.

Title 21: Food and Drugs PART 2—GENERAL ADMINISTRATIVE RULINGS AND DECISIONS Subpart A—General Provisions

§2.19 Methods of analysis. Where the method of analysis is not prescribed in a regulation, it is the policy of the Food and Drug Administration in its enforcement programs to utilize the methods of analysis of the AOAC INTERNATIONAL (AOAC) as published in the latest edition (13th Ed., 1980) of their publication “Official Methods of Analysis of the Association of Official Analytical Chemists,” and the supplements thereto (“Changes in Methods” as published in the March issues of the “Journal of the Association of Official Analytical Chemists”), which are incorporated by reference, when available and applicable. Copies are available from the AOAC INTERNATIONAL, 481 North Frederick Ave., suite 500, Gaithersburg, MD 20877, or at the National Archives and Records Administration (NARA). For information on the availability of this material at NARA, call 202‐741‐6030, or go to: NOTES: • [42 FR 15559, Mar. 22, 1977, as amended at 47 FR 946, Jan. 8, 1982; 54 FR 9034, Mar. 3, 1989; 70 FR 40880, July 15, 2005; 70 FR 67651, Nov. 8, 2005] • Title 21 → Chapter I → Subchapter A → Part 2 → Subpart A → §2.19 • Accessed on 7‐27‐2018‐bin/text‐idx?SID=7a20040ac19ed218138aed8bacc33e2f&mc=true&node=se21.1.2_119&rgn=div8

e-CFR data is current as of July 24, 2018

International Harmonization Impact

• Current agreement with ISO to participate  in each other’s standards development  activities – for milk and milk products.   • IDF is engaged through this agreement • Methods are jointly submitted to  CODEX process by AOAC, ISO, and IDF  for dispute resolution status • 12 Final Actions methods submitted  into CODEX process.   • Active participation in revision of ISO  standards for the validation of alternative  microbiology method validation

The Vision

AOAC’s Mission

As a 


AOAC INTERNATIONAL advances  and  , by members, organizations, and experts dedicated to 

developing and validating 



AOAC Organizational Affiliate Members As of August 2018

• • • •

• • • • • • • • • • • • • • • • •

• • • • • • • • • • • • • • •

3M Food Safety Abbott Nutrition

Eurofins Scientific, Inc.

Nestle Research Center

Fonterra Co‐operative Group  Ltd.

NSF International

Agilent Technologies, Inc. Archer Daniels Midland  Company

Ocean Spray Cranberries, Inc.

Grain Millers, Inc GW Research Ltd.


Perkin Elmer

Association Of American Feed  Control Officials, Inc (AAFCO)

Health Canada

Q Laboratories, Inc. R‐Biopharm, Inc.

Herbalife International Of  America, Inc

• • • • • • • • • • • • •

BioControl Systems, Inc.

ROMER Labs Division Holding  GmbH

Biolan Microbiosensores, S.L.


BioMérieux, Inc.

Kellogg Company

SC Labs

Bio‐Rad Laboratories Biotecon Diagnostics Bruker Daltonik GmbH CEM Corporation Charm Sciences Coca‐Cola Company Cargill, Inc.



Mead Johnson Nutrition

Shimadzu Scientific  Instruments, Inc.

Medallion Labs / General Mills,  Inc.

Starbucks Coffee Company Thermo Fisher Scientific


Merck KGaA ‐ EMD Millipore Mérieux NutriSciences ‐ Silliker Microbac Laboratories, Inc.

Tyson Foods, Inc. Waters Corporation


Microbiologics, Inc. Neogen Corporation

Deerland Enzymes Elanco / Eli Lilly & Co.

AOAC Leverages the Power of Many

AOAC Leverages Networks to Assemble Stakeholders & Experts


• Develop international voluntary consensus standards method performance requirements

• Discuss & adopt methods that are published in the Official Methods of Analysis of AOAC INTERNATIONAL using judgment of the world’s leading experts. Providing fit for purpose methods through standards development

General Locations of AOAC stakeholder panel participants General Locations of the 16 AOAC INTERNATIONAL current Sections

AOAC ® INTERNATIONAL (AOAC) is an independent third‐party international standards  developing organization and AOAC has no vested interest in the development of standards or in  the evaluation of methods of analysis.

Analytical Excellence addresses emerging issues and influence standards development as a global leader in analytical excellence

Standards Development 

Official Methods of  Analysis (OMA) &  Performance  Tested Methods  (PTM)

Laboratory  Proficiency  Testing & Quality  Management

Analytical Excellence


OVERVIEW: Project Initiation to Adopted Method

• Urgent or Emerging Analytically‐based Issues  • AOAC forms an Advisory Panel of key stakeholders

Initiation of  Projects

• AOAC forms stakeholder panel and engages working groups to  draft standards • Stakeholder panel develops/approves voluntary consensus  standards – most common are standard method performance  requirements.

Standards  Development

• AOAC forms Expert Review Panel (ERP) to review & approve  methods using approved standard • Adopted methods are published in the Official Methods of  Analysis of AOAC INTERNATIONAL &  Journal of AOAC  INTERNATIONAL

Conformity  Assessment

Main Features

6 months for  standards  development 6 month for methods  review/adoption Stakeholder panels &  ERPs meetings

> 80 Official Methods  adopted by ERPs using  standards (> 50  methods adopted for  infant formula and  adult nutritionals)

Domestic and  International  Principles for  Standards  Development

Global & domestic  volunteer driven,  participation, and  cooperation

108 analytical  standard method  performance  requirements

AOAC Stakeholder Panels

Strategic Food  Analytical  Methods SPSFAM

Agent  Detection 

Alternative  Methods ISPAM

AOAC   Standards  Developing  Communities

Assays SPADA

Infant Formula  and Adult  Nutritionals SPIFAN

Dietary  Supplements SPDS

AOAC Standards Development Processes

Transparency, Openness,  Balance, Due Process,  Consensus, Appeals US National Technology  Transfer and  Advancement Act ( PL 104‐ 113) Standards Process




Examples of AOAC Consensus Standards

• Standard Method Performance Requirements • Method Validation Guidelines

• Sampling Standards • Methods of Analysis

What Are Standards

• Common and repeated use of rules, conditions, guidelines or  characteristics for products or related processes .  • The definition of terms; classification of components; delineation of  procedures; processes, products, systems, services, or practices;  test  methods and sampling procedures. • A Performance standard is a standard that states requirements in  terms of required results with criteria for verifying compliance but  without stating the methods for achieving required results. • Voluntary Consensus standards are standards developed or adopted  by voluntary consensus standards bodies , both domestic and  international.

Standards Development and Stakeholders

• AOAC conforms to NTTAA* and therefore includes all  stakeholder perspectives.

National Technology Transfer Advancement Act (Public Law 104‐113) – coordination of federal standards and conformity assessment activities  with private sector standards and conformity assessment activities.

• AOAC and an Advisory Panel will recommend a finite  number of potential voters in the stakeholder panel  representing the various perspectives.

OMB A-119 and NTTAA

• National Technology Transfer and Advancement Act of  1995 – Directs federal agencies with respect to their use of private  sector standards and conformity assessment practices. – Directs federal agencies to adopt private sector standards,  wherever possible, in lieu of creating proprietary non‐ consensus standards. – Codified existing policies in A‐119, established reporting  requirements, and authorized the National Institute of  Standards and Technology (NIST) to coordinate conformity  assessment activities of federal agencies.

OMB A-119 and NTTAA

• US OMB Circular A‐119 – Standards developed by voluntary consensus standards bodies are  often appropriate for use in achieving federal policy objectives and in  conducting federal activities, including procurement and regulation. – Encourages federal agencies to benefit from the expertise of the  private sector – Promotes federal agency participation in such bodies to ensure  creation of usable standards – Reduces reliance on government‐unique standards




Balance of Interests

No one interest or perspective should dominate or be the majority.  It can be  affected not only by the number of participants in particular categories but also by  the funding source.  The provider of the funding in standards development work can  sometimes dominate the process.  If funding is to be provided by a government  agency or other entity, care must be taken to avoid undue influence on the outcome  of the process by the sponsor. A position or exercise of dominant authority, leadership or influence by reason of  superior leverage, strength or representation to the exclusion of fair and equitable  consideration of other viewpoints.  The process shall have a lack of dominance of any  one interest, organization or perspective A person with a direct or material interest, impact, risk or investment in an issue or  concern and/or outcomes. Identified segment of community members from various perspectives and interests  who are assembled to share in and address issues and concerns of the group.  Their  product is but not limited to standard method performance requirements.  Specific group of stakeholders commissioned by the stakeholder panel and approved  by the stakeholder panel chair to apply expertise develop draft standard(s) for  recommendation to the stakeholder panel.



Stakeholder Panel

Working Group

Terminology (con’t)



Advisory Panel

Planning or ad hoc committee of key stakeholders to identify additional  stakeholders and experts, identify priorities and help to plan the first stakeholder  meeting.

Key Stakeholder

A stakeholder who may have a great material interest 


General agreement, but not necessarily unanimity, and includes a process for  attempting to resolve objections by interested parties, as long as all comments have  been fairly considered, each objector is advised of the disposition of his or her  objection(s) and the reasons why, and the consensus body members are given an  opportunity to change their votes after reviewing the comments

Fitness for Purpose

Description of what the method needs to do

Standard Method  Performance Requirements

Voluntary consensus standard that details the fitness for purpose; including relevant  analyte(s), non‐relevant analytes, matrices, potential interferents, and performance  characteristics including analytical range, levels of confidence; recoveries, etc….   A vetted balanced representative subset of the stakeholder panel who vote on  motions presented to the stakeholder panel on behalf of the stakeholder panel  demonstrating consensus of the stakeholders

Voting Members

Basic Principles of Standards Development

As an international standard developing organization, AOAC standard  setting activities include:

Transparency Openness Balance of Interests Due Process Consensus Appeals


– Announces the proposed standard development  activity

– Invites all stakeholders to participate and  contribute their perspectives

– Invites comments prior to final approval and  adoption of standards.


– Make the standards development process available for  participation for all who are materially interested.  

– Leverage networks of key stakeholders, membership and  volunteers to ensure that all materially affected parties and  interests are invited to participate and provide input.  

– Ensures that meetings are open to the public and are  advertised.

Balance of Interests • AOAC establishes a voting member panel that is representative  of the scope of perspectives of the entire stakeholder panel.  – Vetted by the AOAC Official Methods Board – Balance and dominance • The stakeholder chair moderates the meeting and will maintain  seek to maintain a lack of dominance by any one stakeholder;  and • Primary voters and alternate voters may be specified – to ensure that identified perspectives are represented.

Due Process

• AOAC stakeholder panel meetings are open and all  stakeholders are highly encouraged to participate in any of the  discussions and share their perspectives.  

• Meetings are conducted in accordance to parliamentary  procedure.  

• Draft AOAC standards method performance requirements are  open for comment.  Every effort will be made to ensure that all  perspectives have the opportunity to participate.


• AOAC considers two‐thirds majority of the representative  voting members of the stakeholders or of the assembly. 

• Evidence of consensus is the documented vote.  Voting takes  place during in person meetings or by email or facsimile  ballot.  

• Voting and changes in votes are conducted in accordance  with standard parliamentary procedures.

Appeals Process

• All formal complaints, appeals or comments  are sent to the AOAC Staff.

• All written concerns will be considered and  given a response.

Recap of the Overall Process for Methods Submitted in response to SMPRs or Call for Methods

1. Allows AOAC to focus on projects addressing an urgent need  of a critical mass of stakeholders.

2. Drives AOAC processes forward faster.

3. Assembles stakeholders (industry, government and  academia) to neutral place to articulate and reach consensus  on requirements and resolve conflicts. 4. Those requirements are codified and are published as  “Standard Method Performance Requirements” (SMPRs).

5. Methods are solicited that purport to meet those  requirements.  

6. Expert review panels (ERPs) judge the methods against the  SMPRs.  Method(s) that best meet the SMPRs are adopted  and designated “First Action” Official Method of Analysis .  7. Process for First Action status to Final Action status follows  as the same process for all AOAC First Action Official  Methods .

Initiating Standards Development to Final Action Status of Methods

Advisory  Panel

ERP Review of First  Action Methods &  any  recommendations  for Final Action  Status/Repeal/etc..

OMB review &  rendered decisions  on Final Action  status/Repeal

Call for Methods Call  for Experts (if  needed)

ERP Review of  Methods and First  Action status 

Established  SMPRs

Stakeholder Panel

Working  Groups

Advisory Panel

• Identifies key stakeholders and subject matter experts • Frames the issues and set priorities for the stakeholder  panel • Provides financial support • Stakeholder Panel Chair moderates discussion

After 2 years, ERP  recommends to  AOAC Official  Methods Board  regarding status  of method

Publication of  Standard Method  Performance  Requirements

First Action,  Official Methods  status

Expert Review  Panel

Expert Review  Panel

Advisory Panel

Stakeholder Panel

Working  Groups

Stakeholder Panel Composition

• Product Manufacturers • Analyte/Method Subject Matter Experts • Technology Providers • Method Developers • Government and Regulatory Agencies • Contract Research Organizations • Reference Materials Developers

• Ingredient Manufacturers • Method End Users • Academia • Non‐Governmental Organizations  (ISO,  IDF, etc…) • Other…. as identified

Anyone with a material interest can participate Balanced group of voting stakeholders Chair and voting members vetted

After 2 years, ERP  recommends to  AOAC Official  Methods Board  regarding status  of method

Publication of  Standard Method  Performance  Requirements

First Action,  Official Methods  status

Stakeholder  Panel

Expert Review  Panel

Advisory Panel

Working  Groups

Stakeholder Panels: Voting Members • All stakeholders are entitled to due  process.   – All stakeholders can share their  perspectives – Anyone with a material interest may  participate – Standards are established by a group  that lacks dominance by any one  interest ‐ BALANCE Perspective 1 Perspective 2 Stakeholder Panel Composition

Perspective 3

• Voting Panel members represent  stakeholders of same/similar  perspectives.

Perspective 6

Perspective 4

Perspective 5

• Voting panel demonstrates consensus  on behalf of the stakeholder panel. 

SPSFAM Participants  ‐ Broad Perspectives

academia 4%

ngo 2%

government 14%

industry 80%

SPSFAM Participants ‐ Specific Perspectives

vet drugs 2%

cro 14%

tech providers 14%

dietary supp 5%

state regulators 7%

research 5%

food/beverage 14%

regulators 12%

food/formula 9%

ref materials 5%

iso 2%

food/ingred 5%

indep 2%

food/cro 2%

formula 2%

SPSFAM Participants ‐ Regional Perspectives


Argentina 3%

3% Canada

Netherlands 2%

5% Italy 2%

New Zealand

2% Singapore 2% Sweden 2%

Switzerland 2% UK 2%

USA 75%

SPSFAM Participants ‐ Regional and Specific Perspectives

CANADA regulator 2%

ARGENTINA  research 2% AUSTRALIA cro 2%

CANADA cro 2%

NETHERLANDS  food/formula

USA vet drugs 2%

CHINA regulator 2% ITALY  research 2%

2% NEW ZEALAND iso 2%

USA tech provider 11%

SINGAPORE  food/formula

USA state regulator 7%

2% SWEDEN  regulator 2% SWITZERLAND  food/formula 2%

USA regulator 4%

USA  reference  materials 4%

UK tech  provider 2%

USA cro 11%

USA  independen t 2%

USA food/formula 7%

USA food/beverage 13%

USA food/ingred 4%

USA dietary supplements 4%

USA food/cro 2%

Representative SPSFAM Voting Panel

Industry ‐ Food



Voting Panel


Industry ‐ CRO

Industry – Technology Provider

Industry – Dietary  Supplement

Representative Voting Panel is vetted,  modified (if necessary) and approved by the  AOAC Official Methods Board.

Stakeholder Panel Working Groups

• Subsets of stakeholder  panel • Develop draft standards • Reconcile public comments  received on draft standards • Recommend draft standard  to the stakeholder panel for  deliberation and consensus

• Members approved by the  stakeholder panel chair • Can meet prior to  stakeholder meeting • Develops draft standard(s) • May review methods  resulting from a Call for  Methods

Stakeholder Panel Role and Output

• Defines specific analytical issue(s)

1 st

• Forms working groups to draft standard(s)  that address the issue(s)

2 nd

• Comments on draft standard(s)

3 rd

• Adopts voluntary consensus standard(s)

4 th

AOAC Voluntary Consensus Standards  • Standard Method Performance Requirements (SMPRs)  – Published in Official Methods of Analysis of AOAC INTERNATIONAL – Manuscript published in  Journal of AOAC INTERNATIONAL

Advisory Panel, Stakeholder Panel & Working Groups

Advisory  Panel

• Funding


• Community of experts and key stakeholders • Routine 100+ stakeholders • Balanced representative subset of vetted voting stakeholders

Stakeholder Panel

• Consists of technical experts from Industry, Government, CRO’s, and Academia to develop method performance criteria required for needed methods • Present background and history on analytical method needs for stakeholder panel

Working  Groups

Establish SMPR ® Standard Method Performance Requirements

Establish  SMPRs

• Documents a community’s analytical method needs • Very detailed description of the analytical requirements • Includes method acceptance requirements • Used to qualify methods for AOAC approval in the Official Methods SM program • Published as a standard

Standard Methods Performance  Requirements (SMPRs)

• Documents a community’s analytical  method needs. • Very detailed description of the  analytical requirements. • Includes method acceptance  requirements. • Used to adopt AOAC Official Methods  by Expert Review Panels. • Published as a standard in the OMA  and in the  Journal of AOAC  International.

Publication of  Standard  Method  Performance  Requirements

After 2 years, ERP  recommends to  AOAC Official  Methods Board  regarding status of  method

Expert Review  Panel

First Action, Official  Methods  status

Advisory Panel

Stakeholder Panel

Working Groups

Example SMPR: Selected Food Allergens

Performance parameters and targets that method must meet

Specified intended method use

How the method is to be applied

Definitions used for this SMPR as it relates to the method

Example SMPR: Selected Food Allergens (con’t)

Commodities from which the method should

be able to determine allergenic targets


An analytical  voluntary  consensus  standard

Logically  documents a  community’s  analytical  method needs

Very detailed  description of  the analytical  requirements.


Includes  method 

Published as a  standard.

performance  requirements.

Used as  acceptance  criteria for 

method  approval



• Introduction • Background • Format • Process • Performance parameters • Guideline for Development of SMPRs

Standard Methods Performance Requirements

• Commonly referred to  as: – SMPRs – “Smipper”s


• documents a community’s analytical method  needs. • very detailed description of the analytical  requirements. • includes method acceptance requirements. • used to qualify methods for AOAC approval under  the Alternative Pathway model. • published as a standard.

Uses of SMPRs

Basis for method acceptance and approval.

• Guidance to method developers for the development of  new methods. • Advance the state‐of‐the‐art in a particular direction. • Address specific analytical needs. • Allow AOAC to reach a broader community of method  developers and users. • Development time = 3 to 6 months.


Most OMA methods have been validated without  formal acceptance criteria. Compared to a reference method. Certain reference documents existed (but hard to  find) for describing PRSD (R) , expected recovery, &  HorRat value.


• Last 20 years, acceptance criteria have  been included in common study protocols: – antibiotic residues in milk – mycotoxins in grain – peanut allergens


• In 2004, AOAC was awarded a US Dept of Homeland  Security (DHS) project to evaluate hand held assays. • AOAC developed a common study protocol, and for  the first time, developed and published a separate  acceptance criteria statement. • AOAC began developing what are now called standard  method performance requirements in 2007.


In 2009: AOAC replaced the term “acceptance criteria” with  “Standard Method Performance Requirements” (SMPR).

An SMPR was completed for antibiotic residues in  seafood.

Background In 2010 AOAC completed development of  standard method performance  requirements were also developed for: – Ricin hand held assays – Bacillus anthracis hand held assays – Bacillus anthracis PCR assays  – Francisella tularensis PCR assays  – Yersinia pestis PCR assays


• By 2010, a variety of method performance  requirements and acceptance requirements from  different AOAC projects had been developed ‐ each  with its own format and style. • AOAC recognized that it needed a standard process  and format.  • A standard format was developed in 2010.

SMPR Format

Each SMPR is identified by a unique SMPR‐ number consisting of the year followed by a  sequential identification number  (YYYY.XXX).

SMPR Format

• Intended use • Applicability • Analytical technique • Definitions

SMPR Format

• System suitability • Reference materials • Validation guidance • Maximum time‐to‐determination • Method performance requirements table

Performance requirements parameters for  quantitative methods:

• Analytical range • Limit of detection • Limit of  Quantitation  • Repeatability • Recovery • Reproducibility

SMPRs can be developed for all types of methods:

Quantitative methods – Trace components – Main components Qualitative methods – Trace components – Main components Identification methods

SMPRs are published in the OMA. SMPR ID numbers use the year and 3 numerals. OMA ID numbers use the year and 2 numerals.

AOAC has adopted 113 SMPRs since 2010

SMPR Process

Fitness‐for‐Purpose Statement

• AOAC uses this term in a different way than other organizations. • a general statement of what a method needs to be able to do. • an approximation that can be reviewed by the Stakeholder Panel. • allows AOAC staff to collect methods that might be useful.

AOAC INTERNATIONAL Fitness for Purpose Statement Guideline A description of the minimum performance characteristics required by an analytical method to detect or measure an analytes or analytes. A Fitness for Purpose statement must clearly

1) analyte or class of analytes 2) analytical range 3) matrix or matrixes 4) types of test samples (powder, liquid, raw food, sprays, etc.) 5) regulatory requirements (if any) 6) time-to-signal (sample preparation to analytical results) 7) type of analysts (trained chemists or microbiologist, first responder, field hand)

identify the:

A Fitness for Purpose statement may also provide additional information about the analytical requirements that materially affects the types of methods that can be used. . For example, will the method be used in a laboratory under controlled conditions or will the method by used in the field. A Fitness for Purpose statement should describe whether qualified methods will be screening or confirmatory techniques, and/or intended to be used as reference methods for dispute resolution

A Fitness for Purpose statement should be no longer than one paragraph.

Version 2 6/21/10



• Very early in process • General statement of method performance • No or few acceptance criteria • 1 or 2 paragraphs • No formal format • Not a standard

• A deliverable • Very detailed specification of method performance requirements • Acceptance criteria • 2 to 3 pages • Standard format • Formal AOAC standard • Published in the OMA

Quantitative Performance Parameters

• • • • •

Limit of Quantitation  (LOQ) Limit of Detection  (LOD)

Precision Recovery

Reference materials System Suitability

• •

Applicable Range



Performance parameters will be discussed again later.

SMPR Process

Public Review – AOAC staff will post draft SMPRs to the AOAC website. – Send out to interested parties. – Collect and compile comments. – Work with WG chair to address comments.

SMPR Process

Stakeholders Panel Review – WG Chair presents draft SMPR with comments and responses. – Explain and answer questions. – Stakeholder’s Panel votes. – Staff assigns the SMPR number.

SMPR Process

Publication • Staff works with chair to prepare SMPR for publication. • CSO works with WG chair to prepare a companion article for the SMPR.

SMPR Process: Working Group

Development time:  3 – 6 months. You can expect confusion arising from  different understandings of terms,  definitions, and concepts. That’s why we developed the SMPR guidance,  and included an introduction session on  both the subject matter and validation.

Table 5: Expected Recovery as a Function of Analyte Concentration

Mean Recovery (%)

Analyte %

Analyte Ratio





98-102 98-102 97-103 95-105 90-107 80-110 80-110 80-110 60-115 40-120


10 -1 10 -2 10 -3 10 -4 10 -5 10 -6 10 -7 10 -8 10 -9







100 ppm


10 ppm


1 ppm


100 ppb


10 ppb


1 ppb


• The closeness of agreement between independent test results obtained under stipulated conditions. • Same lab, same samples, same analysts, same instrument.


• Expressed as:

– RSD(r) or RSD r

or as “RSD little r”

– RSDr estimated as 2/3 of RSDR

Table 4: Expected Precision (repeatability) as a Function of Analyte Concentration

Analyte % Analyte Ratio






1.3 1.9 2.7 3.7 5.3 7.3



10 -1 10 -2 10 -3 10 -4 10 -5 10 -6 10 -7 10 -8 10 -9





100 ppm (mg/kg) 10 ppm (mg/kg) 1 ppm (mg/kg) 100 ppb (μg/kg) 10 ppb (μg/kg) 1 ppb (μg/kg)


0.0001 0.00001 0.000001 0.0000001 0.00000001

11 15 21 30

Performance parameters

• All of the following information (plus a ton more) is in: Appendix F: Guidelines for Standard Method Performance Requirements in the 19 th edition of the Official Methods of Analysis

Performance parameters

• Reproducibility • – Precision under reproducibility conditions. – Conditions where independent test results are obtained with the same method on identical test items in different laboratories with different operators using different equipment.


• Also known as inter-laboratory variation or precision.

• Measured as: – Relative Standard Deviation Reproducibility – RSDR or RSD R or “RSD big R”

Predicted RSDR or PRSD(R)

• PRSD(R) = 2C -0.15 • where C is expressed as a mass fraction.

Table 6: Predicted Relative Standard Deviation of Reproducibility (PRSD R )

Concentration, C

Mass fraction, C

PRSD(R) (%)

100 %



1 %






1 ppm



10 ppb



1 ppb



Table excerpted from: Definitions And Calculations Of Horrat Values From Intralaboratory Data, AOAC INTERNTIONAL, Horrat for SLV.doc, 2004-01-18.


• You might notice that not too much applicable to microbiology. • The SMPRs are adaptable to food microbiology, but not currently used. • Prefer to use a comparison to reference methods.

Appendix F:  Guideline to SMPRs

• Complete guidance designed to contain all of AOAC’s validation requirements. • Everything you need to develop an SMPR • Published in OMA

SMPR Guideline

Contents covers • Chemistry & microbiology • Quantitative & qualitative • Definitions • Evaluation recommendations • Expected results • Informative sections

SMPR Guideline

Introduction SMPRs Annex A: SMPR Format

Table A1: Performance Requirements Table A2: Recommended Definitions

Table A3: Recommendations for Evaluation Table A4: Annex 5: Expected Precision Table A5: Expected Recovery Table A6: Predicted Relative Standard Deviation of Reproducibility Table A7: POD and Number of Test Portions

SMPR Guideline

Annex B:  Classification of Methods Annex C:  Understanding the POD Model Annex D:  Definitions and Calculations of HorRat Values from  Intralaboratory Data Annex E:  AOAC Method Accuracy Review  Annex F:   Development and Use of In‐House Reference  Materials


After SMPR Development

How does one get from SMPR to OMA?

Call for Methods

• Based on the fitness‐for‐purpose  statement. • Try to collect as many methods that  might be useful. • To provide information on the analytical  possibilities and claimed performance.

Call for Methods

• AOAC issues a Call for Methods based on a  generally accepted fitness for purpose or  standard method performance  requirements

• Candidate methods are selected that may  meet the SMPR

Expert Review Panel (ERP)

• Group of stakeholders who are also subject matter experts  on methodology • Vetted by the AOAC Official Methods Board • Reviewed methods as candidates for further validation  work

After 2 years, ERP  recommends to  AOAC Official  Methods Board  regarding status  of method

Publication of  Standard Method  Performance  Requirements

First Action,  Official Methods  status

Expert Review  Panel

Advisory Panel

Stakeholder Panel

Working  Groups

How it Works: The Details Expert Review Panels

• Must be supported by relevant stakeholder body

• Membership is carefully managed and properly vetted by  the AOAC Official Methods Board

• Holds transparent public meetings

• Remains in force to monitor methods as long as method is   in First Action Status.

ERPs and AOAC Official Methods

• ERPs review methods for First Action Official Methods status • ERPs adopt methods as First Action Official Methods status • ERPs track First Action methods for 2 years after adoption – ERP reviews any additional information (collaborative study,  proficiency testing, other feedback), makes recommendation to the  Official Methods Board regarding Final Action status.

How it Works: The Details Official First Action Status Decision

• Method adopted by ERP must perform adequately against  the SMPR set forth by the stakeholders 

• Method becomes Official First Action on date when ERP  decision is made.

How it Works: The Details Official First Action Status Decision

• Methods to be drafted into AOAC format by a  knowledgeable AOAC staff member or designee in  collaboration with the ERP and method author.  • Report of decision complete with ERP report regarding  decision including scientific background (references etc) to  be published concurrently with method in traditional AOAC  publication venues

Tracking First Action Official Methods 

• When ERP has sufficient information it can: – Make a recommendation for Final Action Official Method status – Make a recommendation to repeal the Official Method

• Official Methods Board – Reviews ERP recommendations and renders decisions on Final  Action status or repeal

After 2 years,  ERP  recommends to  AOAC Official  Methods Board  regarding status  of method

Publication of  Standard  Method  Performance  Requirements

First Action,  Official  Methods  status

Stakeholder  Panel

Expert Review  Panel

Advisory Panel

Working  Groups

How it Works: The Details Transition to Final Action Status

• ERP will monitor performance and data submitted for two  years

• Further data indicative of adequate method reproducibility  performance to be collected. Data may be collected via a  collaborative study or by proficiency or other testing data of  similar magnitude

How it Works: The Details Transition to Final Action Status

• Removed from Official First Action and OMA if no evidence  of method use or no data indicative of adequate method  reproducibility is forthcoming 

• ERP makes recommendations to the Official Methods Board  (OMB)

• OMB renders decision on transition to Final Action Status

The Path Using Standards

1. This pathway was designed  to focus on those projects  that address an urgent need  of a significant number of  stakeholders.

2. It drives AOAC processes  forward faster.

3. Stakeholders across all areas  – industry, government and  academia found neutral  ground to come together  where their common and  conflicting requirements  could be resolved and  articulated.

Use of Standards for Method Approval 4. Those requirements were  then codified and have been 

published as “Standard  Method Performance  Requirements.” 

5. Methods were solicited to  meet those requirements.  

6. Expert review panels were  convened to pick the best of  those submitted.  That  method or methods were  designated “First Action” by  the ERP.

Adoption of Official Methods of Analysis

7. The method(s) that best  meet the SMPRs receive  “First Action” status by the  ERP.  8. “Final Action” status up to 2  years after adoption, if  sufficient evidence merits  that step.  9. Only the OMB promotes a  method to “Final Action”  status or repeal the  method.

10. Methods that did not meet  the bar would be repealed.

Criterion for OMA : Fulfills the Standard Methods Performance Requirements

How it Works – At a Glance

Funded Stakeholder Panel

Working Groups  to establish Standard  Method Performance Requirements  (SMPRs)

Expert Review Panels to adopt  methods as Official First Action based  upon performance against SMPRs

Guide to Method Format

• Title • Applicability (SMPR can guide) • Principle • Apparatus (SMPR can guide) • Reagents • Sample 

Preparation/Analysis/Determination/Preparation  of Standard Solutions (may have subsections)

• Calculation • Reference

About OMA Methods

• Must be extremely detailed • Should be written such that it can be used as written • Must include safety precautions and  warnings for any step or component used or  that results from using the method • Can be modified • Supporting Data Required

More About OMA Methods

• Not written as research method, but must be  prescriptive and as detailed as possible  – Like a recipe • Always easy to read, format will be updated – Some reference other methods – Need to review method and manuscript to determine some performance parameters • Must demonstrate precision parameters of  repeatability and eventually reproducibility – Repeated method use

Methods Evolve

• Methods can be modified – Editorial changes

– Minor modifications  • Changes that reflect no significant difference in the method results – Major modifications • Changes that reflect a significant difference in method  results • Significant changes in method steps

Two Year Tracking Period

• Between First Action and Final Action • Time during which method can be  optimized • Time during which method is used and  feedback is obtain on method performance • Time during which reproducibility is  assessed if not completed already • For Final Action consideration – Method may be tweaked based on the  information gathered during tracking period

TIPS for Writing OMA Methods

• Think of it as a recipe. – Trained analysts should run most methods

– Nothing should be assumed in trying to follow a method. – Have another analyst review and try follow the method. • Collect that data and analyze it with your own to assess how  easily, precisely, and accurately it can be followed • Evaluate the results – Do not under estimate the power/impact of sample preparation, homogeneity, standards, laboratory  environment, analyst training on results – You can be a “datasaurus” and have the most “perfect”  data sets

Expected results must be repeatable and reproducible!

Guide to Method Format (Method shown is incomplete to allow space for description.)

Chemical names of pesticides and drugs are given at end of pertinent chapter. permanent number and is included only for convenient accessibility. Locator number identifies method by chapter, subchapter, and sequence within the subchapter for easy cross referencing and access. 4 = chapter 4; .10 = subchapter 10; .03 = the third method found in Chapter 4, subchapter 10. The locator number is not the

Permanent number identifies method by year of adoption or first appearance in Official Methods of Analysis of AOAC INTERNATIONAL . 996 = First Action 1996; .13 = sequence of adoption in 1996. Title may include analyte and matrix, type of method, and official status. Applicability statement addresses utility and limitations on use of method or other information.


AOAC Official Method 996.13 Ethoxyquin in Feeds Liquid Chromatographic Method

First Action 1996 Final Action 1997 (Applicable for determination of 0.5–300 m g/g ethoxyquin in dry extruded pet food or meat meal.) See Table 996.13 for the results of the interlaboratory study supporting acceptance of the method. A. Principle Ethoxyquin is extracted with acetonitrile. Extract is analyzed by isocratic liquid chromatography with fluorescence detection. B. Apparatus ( a ) Liquid chromatograph (LC). —Generating 1500 ± 200 psi; with peak area integrator (manual or computer), isocratic LC pump, and column heater. Operating conditions: injection volume, 20 m L; flow rate, 1.3 mL/min; temperature, 35°C; fluorescence detector output, analog to digital conversion; detector settings: excitation, 360 nm; emission, 432 nm. ( b ) LC column. —250 ´ 4.6 mm id, C 18 octadecylsilane, 5 m m spherical, 100 Å pore size. C. Reagents ( a ) Water. —LC grade. ( b ) Acetonitrile. —LC grade. D. Preparation of Standard Solutions ( a ) Ethoxyquin standard stock solution. —400 m g/mL. Weigh the equivalent of 0.1000 g liquid ethoxyquin into 250 mL amber volumetric flask and dilute to volume with acetonitrile. ( Note: Amount of ethoxyquin needed for preparation of stock solution is based on purity of liquid, e.g., for purity of 93.5%, amount of liquid ethoxyquin = 0.100/0.935 = 0.1070 g.) H. Calculations Calculate concentration of ethoxyquin, m g/g or ppm, in test sample from calibration curve (using linear regression with line forced through zero intercept) as follows: Ethoxyquin, m g/g or ppm = C F W ´ ´ 15. where C = ethoxyquin concentration from LC calibration curve, m g/mL; 1.5 = volume of acetonitrile added to test solution, mL; F = dilution factor; W = weight of test portion, g. Reference: J. AOAC Int. 80, 725(1997).

Specifications for necessary laboratory apparatus and reagent preparations. See also Definition of Terms and Explanatory Notes .

Method may be divided into several descriptive sections.

Calculation symbols are identified and show correct units.

References direct the user to the published collaborative study and any subsequent revisions in the method. Other informative references may be included.

Chemical Abstracts Service Registry Number. A unique identifier that may be used to search a number of data-retrieval systems.

CAS-91-53-2 (ethoxyquin) 6-ethoxy-1,2-dihydro-2,2,4-trimethylquinoline

Revised: March 1998

Status of Official Methods of Analysis

Documentation and Communication

• AOAC carefully documents the actions of Stakeholder Panel,   Working Groups, and ERP

• AOAC will prepare summaries of the meetings  – Communicate summaries to the stakeholders – Publish summaries in the Referee section of AOAC’s  Inside  Laboratory Management • AOAC publishes its voluntary consensus standards and Official  Methods – Official Methods of Analysis of AOAC INTERNATIONAL – Journal of AOAC INTERNATIONAL • AOAC publishes the status of standards and methods in the Referee  section of AOAC’s  Inside Laboratory Management

Accomplishments since 2011


Voluntary Consensus Standards – Standard Method Performance  Requirements (SMPRs®) Total First Action Official Methods of Analysis SM adopted since 2011 Final Action Official Methods of Analysis SM submitted to Codex



> 290

Performance Tested SM certifications (Research Institute)

Harmonization in Standards Development • Agreement with ISO to participate in each other’s standards development  activities – originally for milk and milk products, but working on an expanded  scope • AOAC, ISO, and IDF jointly submitted 13 AOAC Final Action Official  Methods SM to Codex and 12 methods adopted by Codex.

Estimated Working Group Timelines

• Emergency Timeline – 3 weeks to develop SMPR (posting of SMPR for public comment is  after) – Parallel period of time to ERP Review (Call for Methods and Experts  more targeted and based on proposed work statement

• Expedited Timeline

Will need to negotiate

– 6 months to develop SMPR – Parallel 6 – 9 months to ERP Review (Call for Methods and Experts  based on draft SMPR and/or Fitness for Purpose statement)

• Typical Timeline 

– 6 months to develop SMPR – Subsequent 6 months to ERP Review  (based on meeting times)

If you have a method, we can help. • AOAC  Consulting Services – Expanded from the Research Institute service – Provides approved validation testing protocols – Other services to come: • Drafting validation testing manuscripts • Special analytical projects

For more information on SMPRs and AOAC standards  development, please contact …

Deborah McKenzie Senior Director, Standards AOAC INTERNATIONAL 301-924-7077 ext 157


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