Microsoft PowerPoint - FINAL-AOAC StandardsDevDebpres8-2018
Understanding AOAC Standards Standard Method Performance Requirements, and AOAC Official Methods
AOAC Annual Meeting Toronto, Canada
Goals
• 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
Objectives
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: http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html. 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 https://www.ecfr.gov/cgi‐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
and
of
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.
PepsiCo
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.
Hygiena
BioMérieux, Inc.
Kellogg Company
SC Labs
Bio‐Rad Laboratories Biotecon Diagnostics Bruker Daltonik GmbH CEM Corporation Charm Sciences Coca‐Cola Company Cargill, Inc.
Labcorp
SCIEX
Mead Johnson Nutrition
Shimadzu Scientific Instruments, Inc.
Medallion Labs / General Mills, Inc.
Starbucks Coffee Company Thermo Fisher Scientific
Megazyme
Merck KGaA ‐ EMD Millipore Mérieux NutriSciences ‐ Silliker Microbac Laboratories, Inc.
Tyson Foods, Inc. Waters Corporation
Danone
Microbiologics, Inc. Neogen Corporation
Deerland Enzymes Elanco / Eli Lilly & Co.
AOAC Leverages the Power of Many
AOAC Leverages Networks to Assemble Stakeholders & Experts
AOAC INTERNATIONAL Headquarters
• 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
Journal of AOAC INTERNATIONAL, OMA, ALACC Guide
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
Defensibility
Acceptability
Consensus
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
Terminology
Term
Definition
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.
Dominance
Stakeholder
Stakeholder Panel
Working Group
Terminology (con’t)
Term
Definition
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
Consensus
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
Transparency
– 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.
Openness
– 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.
Consensus
• 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
Australia
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
Government
Academia/Research
Voting Panel
NGO
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
Sponsors
• 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
SMPRs
An analytical voluntary consensus standard
Logically documents a community’s analytical method needs
Very detailed description of the analytical requirements.
SMPR
Includes method
Published as a standard.
performance requirements.
Used as acceptance criteria for
method approval
Questions?
SMPRs
• Introduction • Background • Format • Process • Performance parameters • Guideline for Development of SMPRs
Standard Methods Performance Requirements
• Commonly referred to as: – SMPRs – “Smipper”s
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 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.
Background
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.
Background
• Last 20 years, acceptance criteria have been included in common study protocols: – antibiotic residues in milk – mycotoxins in grain – peanut allergens
Background
• 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.
Background
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
Background
• 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
Fitness‐for‐Purpose
SMPR
• 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
Time‐to‐result
Bias
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
Unit
100
1
100%
98-102 98-102 97-103 95-105 90-107 80-110 80-110 80-110 60-115 40-120
10
10 -1 10 -2 10 -3 10 -4 10 -5 10 -6 10 -7 10 -8 10 -9
10%
1
1%
0.01
0.1%
0.001
100 ppm
0.0001
10 ppm
0.00001
1 ppm
0.000001
100 ppb
0.0000001
10 ppb
0.00000001
1 ppb
Precision
• The closeness of agreement between independent test results obtained under stipulated conditions. • Same lab, same samples, same analysts, same instrument.
Precision
• 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
Unit
RSD%
100
1
100%
1.3 1.9 2.7 3.7 5.3 7.3
10%
10
10 -1 10 -2 10 -3 10 -4 10 -5 10 -6 10 -7 10 -8 10 -9
1%
1
0.1%
0.01
100 ppm (mg/kg) 10 ppm (mg/kg) 1 ppm (mg/kg) 100 ppb (μg/kg) 10 ppb (μg/kg) 1 ppb (μg/kg)
0.001
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.
Reproducibility
• 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 %
1.0
2
1 %
0.01
4
0.01%
0.0001
8
1 ppm
0.000001
16
10 ppb
0.00000001
32
1 ppb
0.000000001
45
Table excerpted from: Definitions And Calculations Of Horrat Values From Intralaboratory Data, AOAC INTERNTIONAL, Horrat for SLV.doc, 2004-01-18.
Microbiology
• 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
Questions?
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.
4.10.03
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
113
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
138
13
> 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 dmckenzie@aoac.org 301-924-7077 ext 157
Questions?
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