AOAC CASP Meeting - MYM 2020
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Ca nabis Ana ytical Science Program
AOAC INTERNATIONAL
CANNABIS ANALYTICAL SCIENCE PROGRAM (CASP) MEETING
WEDNESDAY, MARCH 11, 2020 8:00AM - 2:00PM
at the
Gaithersburg Marriott Washingtonian Center 9751 Washingtonian Blvd. Gaithersburg, Maryland, 20878 SALON C/D/E
Pioneer Members
PerkinElmer R-Biopharm AG SōRSE Technology TEQ Analytical Titan Analytical
Association of Food and Drug Officials (AFDO) Applied Food Sciences BioRad MilliporeSigma
Partner Members
CV Sciences
Eurofins Scientific
Affiliate Members
Alkemist Labs BIOTECON Diagnostics Canopy Growth Corporation CEM Corporation
Charm Sciences Crystal Diagnostics Hygiena Institute of Food
Technologists (IFT)
WiFi: Marriott Conference Password: aoac2020 Sign-In Here: http://bit.ly/casp-mym
AOAC INTERNATIONAL Cannabis Analytical Science Program (CASP)
Wednesday, March 11, 2020 | 8:00AM – 2:00PM ET Gaithersburg Marriott Washingtonian Center – Salon C/D/E
MEETING AGENDA
I. WELCOME, INTRODUCTIONS AND ANNOUNCEMENTS (8:00AM – 8:15AM) David Schmidt, AOAC INTERNATIONAL
II. PROGRAM REVIEW (8:15AM – 8:30AM) Scott Coates, AOAC INTERNATIONAL
III. CONSENSUS BUILDING AT AOAC INTERNATIONAL (8:30AM – 8:45AM) Deborah McKenzie, AOAC INTERNATIONAL
IV. UPDATE ON THE USDA DOMESTIC HEMP PROGRAM (8:45AM – 9:30AM) Kerry Smith , Director, Laboratory Approval and Testing Division, Agricultural Marketing Service, USDA
V. REPORT FROM THE MICROBIAL CONTAMINANTS WORKING GROUP (9:45AM – 10:30AM) Julia Bramante, Colorado Department of Public Health & Environment
VI. REPORT FROM THE CHEMICAL CONTAMINANTS WORKING GROUP (10:30AM – 11:15AM) Susan Audino, Audino and Associates and Julie Kowalski, Consultant
VII. REPORT FROM THE CANNABOIDS IN CONSUMABLES WORKING GROUP (11:15AM – 12:00PM) Holly Johnson, American Herbal Products Association
- Lunch 12:00pm – 1:00pm -
VIII. INTRODUCTION TO TRAINING & EDUCATION WORKING GROUP (1:00PM – 1:30PM) Susan Audino, Audino and Associates and Toby Astill, PerkinElmer
IX. DISCUSSION ON NEXT STEPS FOR CASP (1:30PM – 1:45PM) Scott Coates, AOAC INTERNATIONAL
X. SUMMARY/WRAP UP (1:45PM – 2:00PM) Scott Coates & Palmer Orlandi, AOAC INTERNATIONAL
02-10-2020 Version 3 – Subject to Change Without Notice
Morning Break at 9:30AM
March 11, 2020 AOAC CASP Meeting – Presenter Bios
AOAC INTERNATIONAL CASP MEETING – SPEAKER BIOS
Susan Audino, Ph.D
Audino & Associates
Dr. Susan Audino is a chemist/chemometrician and independent consultant to chemical and biological laboratories. On behalf of Accreditation Bodies, she assesses laboratories to and is an instructor for multiple ISO/IEC standards such as ISO 17025. She is recognized as a leader in the cannabis industry, focusing on consumer safety and sound science in the development of official and consensus analytical test methods. Susan serves as a scientific advisor to several scientific organizations, regulatory bodies, and sits on expert review panels. Dr. Audino has chaired the AOAC cannabis advisory panel and currently chairs the chemical contaminants working group, and is a board member for the Center for Research on Environmental Medicine. She has provided seminars, workshops, webinars, and facilitated symposia domestically and internationally.
March 11, 2020 AOAC CASP Meeting – Presenter Bios
Julia Bramante, Ph.D.
Colorado Department of Public Health and Environment Lead Scientist
Julia began her career in the cannabis industry in 2014 at Gobi Labs, one of the first cannabis testing facilities to open in Colorado. She then transitioned to the Colorado Department of Public Health and Environment’s Marijuana Reference Laboratory where she currently serves as Lead Scientist. Julia is also the Chair of the Cannabis Chemistry Subdivision of the American Chemical Society and the Co-Chair of the AOAC CASP Microbial Contaminants Working Group.
March 11, 2020 AOAC CASP Meeting – Presenter Bios
Scott Coates, M.S.
AOAC INTERNATIONAL Senior Director of the AOAC Research Institute
Scott was appointed as the Senior Director of the AOAC Research Institute on July 1, 2018. He is responsible for daily management of and business development for the AOAC Research Institute. Scott also serves as the Program Lead for the Cannabis Analytical Science Program. Scott served as the Chief Science Office from 2009 until June 2018. In this capacity, he served as the technical lead for many AOAC projects. Scott led the writing and development of Appendix F in the Official Methods of Analysis of AOAC INTERNATIONAL that describes validation requirements and the development of Standard Method Performance Requirements . Before joining AOAC, he worked for 10 years as the Operations Manager for an in-vitro diagnostic manufacturer making medical test kits such as Strep tests and specialized bacterial culture media. Scott holds a B.S. in Microbiology (1978) and a M.S. in Biotechnology Management (1994) from the University of Maryland. Contact Scott at: scoates@aoac.org, (301) 924-7077 x137
March 11, 2020 AOAC CASP Meeting – Presenter Bios
Holly Johnson, Ph.D.
American Herbal Products Association
Chief Science Officer
Holly E. Johnson Ph.D., is the Chief Science Officer for the American Herbal Products Association (AHPA). She previously served for three years as Laboratory Director for Alkemist Labs, an ISO 17025 accredited natural products testing lab specializing in botanical dietary supplements. Dr. Johnson took her Ph.D. in Pharmacognosy at the College of Pharmacy, University of Illinois – Chicago (UIC), under renowned Pharmacognosist and researcher Dr. Norman Farnsworth. Holly was awarded a National Institutes for Health (NIH) Fellowship and trained at the UIC/NIH Center for Botanical Dietary Supplements. She was a Postdoctoral Research Fellow at the Institute for EthnoMedicine studying the etiology of neurodegenerative disease, and also worked for Waters Corporation conducting technical training and regulatory consulting for pharmaceutical and supplements companies. She is currently a Research Associate with the National Tropical Botanical Garden and serves on AOAC working groups, stakeholders’ panels, and expert review panels for Foods and Dietary Supplements. She is a member of the United States Pharmacopeia’s (USP) Medical Cannabis Expert Panel, the Editorial Board of the Journal of AOAC International, and she serves on the Advisory Boards of the American Botanical Council and the American Herbal Pharmacopeia. Holly has over 20 years’ experience working with natural products & botanicals and spent many happy years conducting research on medicinal plants and giving courses at the University of Hawaii.
March 11, 2020 AOAC CASP Meeting – Presenter Bios
Julie Kowalski, Ph.D.
jkSS llc Consultant
Julie Kowalski is a technical consultant primarily serving the cannabis and hemp testing market. She earned her graduate degree in Analytical Chemistry from Pennsylvania State University. Her professional experience includes troubleshooting, method development and validation for GC, GC-MS, LC, and LC-MS/MS in addition to pesticide residue analysis and chromatography method development. She has previously served as the President of the North American Chemical Residue Workshop, served on AOAC Expert Review Panels, the Cannabis Scientific Task Force for Washington State and is currently chairing the AOAC CASP Chemical Contaminants Working Group.
March 11, 2020 AOAC CASP Meeting – Presenter Bios
Kerry Smith, Ph.D.
United States Department of Agriculture (USDA) Director, Laboratory Approval and Testing Division
Kerry Smith, Ph.D., is the Director of the Laboratory Approval and Testing Division (LATD). LATD provides laboratory testing and approval services to facilitate domestic and international marketing of food and agricultural commodities. Kerry was critical in the reorganization and standardization of the Agricultural Marketing Services’ (Agency) laboratory services. She has led significant process and service enhancements, making LATD a leader in residue, mycotoxin, and adulteration testing. In addition, LATD serves as the scientific arm of the Agency, providing subject matter expertise in many areas, including bioengineered foods and hemp production. Kerry has worked for the United States Department of Agriculture (USDA) for 15 years.
Scott Coates Senior Director
AOAC Research Institute AOAC INTERNATIONAL
March 11, 2020
Pioneer
Association of Food and Drug Officials
Titan Analytical
Applied Food Sciences
PerkinElmer BioRad
TEQ Analytical
R- Biopharm AG
SōRSE Technology
MilliporeSigma
Partner
Eurofins Scientific
CV Sciences
Affiliate
Alkemist Labs Alkemist Labs
BIOTECON Diagnostics
CEM Corporation
Charm Sciences
Hygenia
Institute of Food Technologists (IFT)
Canopy Growth Corporation
Crystal Diagnostics
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Current CASP Working Groups and Projects
Microbiology in Cannabis Initial focus on Aspergillus . SMPR completed. Call for methods issued. Chemical Contaminants in Cannabis Residual Solvents in Cannabis. SMPR completed. Call for methods issued. • Heavy metals. SMPR completed. Pending review and adoption. Cannabinoids in Consumables Initial focus on cannabinoids in hemp plant materials. SMPR completed. Call for methods issued. Recommendation on reporting total THC (THC + THCA). Completed, in SMPR. • Recommendation on dry weight. SMPR completed. Pending review and adoption.
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Priorities March 2020 Chemical Contaminants Working Group
Pesticides Residual Solvents Heavy metals Mycotoxins
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Priorities March 2020 Cannabis in Consumables Working Group
Hemp plant materials Dry weight Extracts Foods/ beverages Personal care products Veterinary products
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Priorities March 2020 Microbiology in Cannabis Working Group
Aspergillus Listeria Salmonella E.coli ( STEC)
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New Working Groups
Training and Education Training Working Group • Dr. Toby Astill [Perkin Elmer] recruited to be Chair.
Proficiency Testing Working Group • To be organized in April.
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CASP Team Scott Coates, MSBTM CASP Program Lead Senior Director AOAC Research Institute scoates@aoac.org 301-924-7077 x137 Jonathan Goodwin, , SHRM-SCP, SPHR Deputy Executive Director & Chief HR Officer AOAC INTERNATIONAL jgoodwin@aoac.org 301-924- 7077 x104 Palmer A. Orlandi, Jr., Ph.D. Deputy Executive Director and Chief Science Officer AOAC INTERNATIONAL
Christopher Dent Manager, Standards Development & Official Methods of Analysis® AOAC INTERNATIONAL cdent@aoac.org 301-924- 7077 x119. Alicia Meiklejohn Governance and Business Development
AOAC INTERNATIONAL ameiklejohn@aoac.org 301-924-7077 x101
porlandi@aoac.org 301-924- 7077 x163.
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AOAC Standards Development
Approval of AOAC Standards & Consensus Documents for CASP draft SMPRs
Deborah McKenzie Sr. Director, Standards & Official Methods SM AOAC INTERNATIONAL
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ANALYTICAL AOAC Products, Services, and Analytical Excellence
Standards & Methods Development
A Complete & Harmonized Quality System Through
Official Methods of Analysis SM (OMA) & Performance Tested Methods SM (PTM)
Laboratory Proficiency Testing & Quality Systems
Analytical Excellence
Publications, Training, Educational Outreach & Horizon ‐ scanning
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Examples: AOAC Consensus Products
Basic Principles
• Transparency • Openness • Balance of Interests • Due Process • Consensus • Appeals
• Performance Requirements • Guidelines
• Sampling Standards • Methods of Analysis • Best Practices • Operational Documents
AOAC Consensus & Products
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To Date – Opportunities to Participate Balance of Perspectives & Due Process
TARGETED COMMUNICATION
INVITATIONS TO SMES
EMAIL BLASTS & WEBSITE NOTIFICATIONS
PARTICIPATION IN MEETINGS – AOAC AND EXTERNAL MEETING
ASSOCIATION NEWS ARTICLES
ONLINE & WRITTEN ‐ PUBLIC COMMENT FORMATS
BRIEFINGS & PUBLIC HEARINGS
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Global Perspectives Included
Contract Research Laboratories Independent Contractors US Rule Makers Academia Commodity Producers Product Manufacturers Instrument & Technology Providers State Regulators and Laboratories Reference Material Organizations Proficiency Testing Programs Trade Organizations Scientific Associations Rapid Method Developers Accreditation Organizations
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CASP Standards Development Activity
3 working groups launched new standards work: September ‐ October 2019
February 2020
Community Consensus via electronic consensus and approval March – April 2020
Comments on draft standard method performance requirements Comment period for all 3 documents began on February 2020 through March 2020. Online Open Comment Session held on February 17, 2020
‐ Heavy Metals ‐ Dry moisture ‐ Salmonella
Deliberate and reach consensus on a final versions of the documents WG chairs will present summaries of WG draft standards for deliberation and input March 11, 2020
Working groups developed draft documents: Working groups met to begin their work and continued drafting documents via web conference October 2019 – January 2020
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Approving the Draft Standards
Program Lead and Standards Manager will oversee the approval process
STEP 2 : Program Lead will conclude deliberation and Standards Manager will record and verify with WG chair(s) any revisions, if needed
STEP 1: WG chair(s) introduced to present the draft standard along with how comments were reconciled followed by discussion on the draft standard
STEP 3 : After final revisions are complete, the WG chair will make a motion for stakeholder acceptance of the standard and recommend approval. A second to the motion may be entertained, but is not necessary STEP 6: Standards Manager will walk attendees through the general consensus process. All attendees will be able to participate in the demonstration of consensus
STEP 4: Program lead will acknowledge the motion (and second, if offered) and offer time for discussion/questions on the motion.
STEP 5: After any due discussion, Program Lead will call for a vote on the motion.
NOTE: 2/3 vote in favor of a motion will pass a motion. 2/3 of those voting will demonstrate consensus in passing a motion Negative votes need to be recorded
If the motion is approved, a consensus standard is formed.
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Documentation and Communication
AOAC carefully documents the actions of CASP and the Working groups
AOAC will prepare summaries of the meetings Communicate summaries to the stakeholders Publish status and summaries in the Referee section of AOAC’s Inside Laboratory Management Publish documents in Journal of AOAC INTERNATIONAL, Official Methods of Analysis of AOAC INTERNATIONAL
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Questions?
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Julia Bramante Chair, CASP Microbial Contaminants Working Group SMPR Presentation
March 11, 2020 Gaithersburg Marriott Washingtonian Center 9751 Washingtonian Blvd., Gaithersburg, MD, 20878
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CASP Microbial Contaminants: Working Group Members (as of January 2020)
Organization
Organization
Organization
Organization Think20Labs LabsMart Inc,
Name
Name
Name
Name
Melissa Aldwin
Ambler Anterola
BreezeTrees, LLC
Stephen Bridgett
Goldman Graham Griffin Hansen Haskell Helbert Hildreth Hoffman Hordyk Hudalla Hughes Jayanthi Johnson Hayakawa Hom
PhytaTech
Raymundo
Lerma
Phytatech
Edward
Sawicki
Southern IllinoisUniversityCarbondale
OrganaKannalytics
Cynthia
LeVesque Lorenzen
CaligreenLaboratory
Devin
Sears
Toby Susan Brian
Astill
Perkinelmer
Todd Scott
G2Analytical
Kyle
YoungLivingEssentialOils
CARLOS Rachel Sheryl Casey Sidney SungOui Neil
SEPULVEDA
AGROLABMEXICO SoRSETechnology
Audino
S.A.Audino&Associates
BotanacorLaboratories DesignGroupCollaborative
Eva
Lynch
RockRiverLaboratory
Shegog
Beck
Microbiologics
Bradford
Lena
Madden Maqsood McKernan
Limerick InstituteofTechnology
Shepherd Silverman Simmons
NATA
Cornelius
Berka
BIOTECONDiagnostics
Darin
HawaiiDOHState LaboratoriesDivision
Madeeha
ProVerde Laboratories MedicinalGenomics
PacificStarLabs LLC
Pat
Bird
PMBBiotek SORA Labs
Yvonne
MedicinalGenomics
Kevin
Hygiena
Tammy Rafael
Blakemore Bombonato Bramante Brauninger Brodnick Campbell Boyar
Jana
SelfEmployed
Ronald Megan
Miller Murn Nelson
TherapeuticHealthChoices
Sudberg
AlkemistLabs
Curaleaf
Shannon Sherman
SteepHill
Microbiologics
Suh
ATCC
Kyle Julia
MedicinalGenomics
NJDeptofHealth,PublicHealth&Environmental LaboratMaria
AOAC
Christy
Swoboda Thomas
RomerLabs, Inc.
CDPHE
Nathan
Industrial Laboratories ProVerde Laboratories
Dustin
Newman Niehaus
Instituteof FoodSafety&Defense
Katherine
NJDepartmentofHealth VivariantLaboratories SartoriusCorporation
Roger Robert
A2LA (accreditationbody)
Chris
Gary
CrystalDiagnostics
Anand Tricia Gordon
Thota
TitanAnalytical
Daniel Srinivas
MCRLaboratories
Melissa Shawn
Nutter O'Leary
TitanAnalytical
Vail
Shari Mike
KaychaLabs
BiotechPharmacal Inc.
NJDOH
Vrdoljak
StateofCADeptofPublicHealth
Clark
BioRadLaboratories
Ron
BioMerieux
Shaun
Opie
E4Bioscience Think20Labs
Christopher
Waggener
VirginiaDCLS
Bob
Clifford
Shimadzu
James
Jursich
CenteraBioscience
Ben Jess
Orsburn Paoletti Parish Parisi Pfaller Phillips
Matthew
Ward
ColoradoDeptofPublicHealthandEnvironment
Pearl
D'Cruz
PEARLConsultingLLC
Ben
Katchman
PathogenDx
TEQAnalytical Labs
Jane
Weitzel
IndependentConsultant
Danielle
Deschene
SCLaboratories
Jason Kati Julie
Kircos
Neogen
Zachary
LevelOne Labs
Daniel Jeffrey
Wene
New JerseyDepartmentofHealthPHEL
Lori
Dodson
MarylandMedicalCannabisCommission
Kiss
ATCC
Salvatore
AlBalqaAppliedUniversity
Wigton
WesternAlternative
Wilfredo
Dominguez
3M
Kowalski
TraceAnalytics
Mike
Universityof Iowa
AnnaWilliams Williams
A2LA NIST
Janie Mike Ross
Dubois
ContractAnalytical Services
Kelsey Nikhil Robert
Kropp Kumar
CDPHE
Melissa
NIST
Walter
Wilson Wong
Esposito Franklin
MCRLabs
Canalysis Laboratories
Juan
Rodriguez Rodriguez Salfinger
GreenHillsAnalytics Lab
Seth
TEQAnalytical Laboratories/Industrial Laboratories
MCRLabs. LLC
LaBudde
Alena
Rm3Labs
Victoria Joshua Wendi
Wu
ABCTesting&MateriaMedicaLabs
Ted
Gatesy
MichiganDept.ofAgriculture
Jasen
Lavoie
U.S.CannabisPharma NeogenCorporation
Yvonne
AFDO
Wurzer Young
SCLaboratories MileHighLabs HardyDiagnostics
Quynh ‐ Nhi
Le
Nandakumara Sarma
USPharmacopeialConvention
Jessa
Youngblood
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Microbial Contaminants Working Group: Work Since Last CASP Meeting
• Six teleconferences (October 2019 – February 2020) • One SMPR drafted ( Salmonella ), one other started (STEC) • Public comment period (February – March, 2020) • SMPR made ready for review and approval
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SMPR Development
Standard Method Performance Requirements ® (SMPRs) for Detection of Salmonella in Cannabis and Cannabis Products
Applicability: Candidate methods used to detect Salmonella species and their serovars in cannabis (plants/flowers) and/or cannabis products (concentrates, infused edibles, and infused non ‐ edibles). Candidate methods may be validated for specific matrices, categories, or broader claims.
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Salmonella species • Straight rods, 0.7 – 1.5 x 2-5 μ m. • Facultative anaerobic, gram negative bacteria. • D-glucose and other carbohydrates are catabolized with the production of acid and usually gas. • Occur in humans, warm and cold blooded animals, food, and the environment. • Pathogenic for humans and many animal species. • Shown to survive well under dessication. • Causative agent of typhoid fever, enteric fevers, gastroenteritis, and septicemia.
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Definitions • POD, Probability of Detection.— The portion of positive analytical outcomes for a qualitative method for a given matrix at a given analyte level or concentration • dPOD CP – This difference in POD values between presumptive and confirmed results • LPOD – The POD value obtained from combining all valid collaborator data sets for a given matrix at a given analyte level or concentration • LCL, Lower confidence limit.— Calculated to determine 95% confidence interval of various POD values • UCL, Upper confidence limit.— Calculated to determine 95% confidence interval of various POD values • CFU, Colony forming unit.— Number of viable microorganisms, presented per a specific quantity. (ex. CFU/mL) • MPN, Most probable number.— Method used to estimate contamination levels
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Method Performance Requirements
Table 1. Validation Acceptance Criteria (Plants/Flowers, Concentrates, Infused Edibles, Infused Non ‐ Edibles)
Target Test Concentration a
Parameter
Parameter Requirements
Minimum Acceptable Results
Single Laboratory Validation with artificial contamination
Fractional positive results, 25 ‐ 75% (5 ‐ 15 positive test replicates) dPOD CP 95% CI: LCL < 0 < UCL b
Replicates per matrix: 20 Inoculation procedure: AOAC Appendix J
Low level to produce fractional positive results Ex. 0.2 ‐ 2 CFU/Test Portion
Fractional Concentration (low level)
Replicates: 5 Inoculation procedure: AOAC Appendix J
High level to produce consistently positive results Ex. 2 ‐ 10 CFU/Test Portion
High Concentration
POD of 1.00 c
Non ‐ Inoculated (Zero) concentration
Replicates: 5
0 CFU/Test Portion
POD of 0.00 c
Single Laboratory Validation with natural contamination
Fractional positive results, 25 ‐ 75% (5 ‐ 15 positive test replicates) for minimum 1 lot dPOD CP 95% CI: LCL < 0 < UCL b
Acceptable minimum detection level (low level)
2 separate lots of 20 replicates
N/A
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Method Performance Requirements
Table 1. Validation Acceptance Criteria (Plants/Flowers, Concentrates, Infused Edibles, Infused Non ‐ Edibles)
Target Test Concentration a
Parameter
Parameter Requirements
Minimum Acceptable Results
Multi Laboratory Validation
0.15 ≥ LPOD ≥ 0.85 dPOD CP 95% CI: LCL < 0 < UCL b
Replicates: 12
1 ‐ 10 CFU/Test Portion
LPOD
Replicates: 12
10 ‐ 50 CFU/ Test Portion
LPOD ≥ 0.95
Replicates: 12
0 CFU/Test Portion
LPOD ≤ 0.05
LPOD (0)
a Determined through MPN Procedures (see Table 4)
b The range between the lower and upper confidence interval should encompass 0, if not, the results must be investigated, and an explanation provided.
c If acceptance criteria is not observed, results must be investigated, and an explanation provided.
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Method Performance Requirements Table 7. Inclusivity/Exclusivity Performance Requirements
Final Test Concentration (CFU/mL)
Minimum Acceptable Results
Parameter
Parameter Requirements
Inclusivity Single ‐ laboratory validation (SLV) study: A minimum of 100 strains is required to be
10 ‐ 100 x limit of detection of the candidate method
100% positive results a
cultured by the candidate method enrichment procedure (including those detailed in Table 8).
Exclusivity SLV study: At least 30 non ‐ target organisms, cultured under optimal conditions for growth b
Overnight growth undiluted
100% negative results a
a. 100% correct analyses are expected. All unexpected results are to be retested following internationally recognized guidelines (ISO 16140, AOAC OMA Appendix J, The Compendium of Analytical Methods of Health Canada). Some unexpected results may be acceptable if the unexpected results are investigated, and acceptable explanations can be determined and communicated to method users b. In instances where an exclusivity culture produces a positive result by the candidate method, the culture may be reanalyzed after culture following the candidate method enrichment procedure. Both results (optimal growth conditions and candidate method enrichment) must be reported.
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Method Performance Requirements • Use of live (viable) cultures (liquid stressed/non-stressed, lyophilized) is required. • To screen samples for the presence or
• Final confirmation can be achieved via matrix assisted laser desorption/ionization time of flight (MALDI-TOF) mass spectroscopy, sequencing, or other suitable confirmatory procedures (e.g., biochemical analysis). • One matrix must contain microflora at 10x the level of the target microorganism. • A minimum three level MPN analysis to determine concentration of target microorganism. Use of matrix study replicates is encouraged.
absence of the target analyte, two methods that employ different technologies (e.g., agar plate, PCR, ELISA) must be used.
• To ensure the viability of the inoculating organism (both confirming presumptive
results or determining false negative results) a secondary enrichment followed by plating of the sample to a minimum of two types of agar plates, one of which is recommended to be chromogenic agar, is required (Table 6). Bulk inoculation of test material is required.
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Method Performance Requirements
Table 3. Acceptable Matrix Claims
Table 2. Category Test Portion Requirements
Minimum Test Portion Size a
Criteria
Category
Matrix Claim
Plants & Flowers
10 g
Number of Matrices Minimum Number of Categories
15 (minimum 3 matrices/category) ≥ 10 (minimum 2 matrices/category)
Concentrates
5 g
Broad Range
4 categories
Infused Edibles
25 g
Variety
4 categories 2 categories 1 category
Infused Non ‐ Edibles 10 g a Minimum test portion size required for validation. Alternatively, larger test portions may be validated.
Select
≥ 5 ≥ 5 ≥ 1
Specific Category Specific Matrix (s)
1 category RE: AOAC Technical Bulletin: TB02MAY2016: Acceptable Validation Claims for Proprietary/Commercial Microbiology Methods for Foods and Environmental Surfaces.
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Method Performance Requirements
Table 5. Condition of Inoculating Culture and Stabilization of Matrix Table 6: Recommended Secondary Selective Broths and Agar
Stabilization Conditions 4°C, 48 ‐ 72 h 4°C, 48 ‐ 72 h
Matrix
Inoculating Cells
Media Name
Media Type
Perishable product Heat processed perishable product
Liquid non ‐ stressed culture
Liquid heat stressed
Rappaport ‐ Vassiliadis (RV) (alternately Rappaport ‐ Vassiliadis R10)
Broth
Liquid non ‐ stressed culture (If frozen food is processed, cells must be heat stressed)
‐ 20°C, 2 weeks
Broth Broth
Tetrathionate (TT)
Frozen Product
Selenite cysteine (SC)
Ambient Temperature (20 ‐ 25 o C), 2 weeks Ambient Temperature (20 ‐ 25 o C), 2 weeks
Agar Agar Agar Agar Agar
Xylose lysine desoxycholate (XLD)
Dried culture
Hektoen enteric (HE) Bismuth sulfite (BS) Chromogenic Salmonella
Shelf stable dry product
Liquid non ‐ stressed culture (If shelf stable product is processed, cells must be heat stressed)
Shelf stable liquid product (heat processed)
MacConkey
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Comments Submitted
Comment Received
Response to Comment
Section 6 : Reference Materials Update 1st sentence to remove fungal spores
Fungal spores reference maintained in SMPR to account for potential use of fungal spores in exclusivity and/or artificial contamination.
Table 1, MLV Section, Column 2: Add Replicates in front of 12
MLV table updated to include “Replicates:” in front of 12 to provide clarity.
Table 6: Update title to read “Recommended Secondary Selective Broths and Agar Table 7, Inclusivity: Update strain requirements, Delete at least 10 strains per required Salmonella spp. Table 8: Update column 3 title to strains (not serovars) and add footnote indicating that it’s a requirement only if method claims
Table 6 title updated per comment recommendation.
Table 7, Inclusivity updated to read: A minimum of 100 strains is required to be cultured by the candidate method enrichment procedure (including those detailed in Table 8). Table 8 title updated to read: Minimum Number of Strains Included* Table 8 footnote updated to read: *Required number of strains per subspecies, per method claims
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Motion: Move to accept the Standard Method Performance Requirements ® (SMPR ® ) for Detection of Salmonella in Cannabis and Cannabis Products as presented.
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Discussion?
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Susan Audino, Ph.D. Science Advisor, CASP Program and Past Chair, CASP Chemical Contaminants Working Group SMPR Presentation March 11, 2020 Gaithersburg Marriott Washingtonian Center 9751 Washingtonian Blvd., Gaithersburg, MD, 20878
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CASP Chemical Contaminants: Working Group Members (as of January 2020) Organization Organization Organization Samantha Adams AgilentTechnologies Chris Hardwick Industrial Laboratories Jordan Polaskey MichiganDepartmentofAgricultureandRuralDevelopme Imad Aghila Libyanpetroleum institute Samuel Heckle CEMCorporation Cezary Poplawski R ‐ BiopharmRhone Ltd. Peter Alden WatersCorporation Laura Heiker Phytatech Garrett Reese RM3Labs Lori Allen Universityof Wisconsin ‐ Parkside Jana Hildreth SelfEmployed Juan Rodriguez GreenHillsAnalytics Lab Melissa Ambler BreezeTrees, LLC Shannon Hoffman SteepHill Alterra Sanchez UniversityofMaryland Aldwin Anterola Southern IllinoisUniversityCarbondale Chris Hudalla ProVerde Laboratories Jennifer Sanderson AgilentTechnologies, Inc. Susan Audino SAAudino&Assoiciates Daniel Hughes MCRLaboratories Nandakumara Sarma USPharmacopeialConvention Grace Bandong Eurofins Diana Hulboiiy EurofinsAbraxis Dustin Sawyer RockRiverLaboratory Frank Barretta PSILabs Brian Hultgren MettlerToledo Devin Sears LabsMart Inc, Harry Behzadi AccuScience laboratories Patrick Hutchins ClutchHempHoldings, LLC CARLOS SEPULVEDA AGROLABMEXICO SNEH BHANDARI MerieuxNutriSciences Srinivas Jayanthi BiotechPharmacal Inc. Maged Sharaf CamagScientific, Inc. Patrick Bird AOACConsultant Conor Jenkins Think20Labs Rachel Shegog SoRSETechnology Tammy Blakemore SORA Labs James Jursich CenteraBioscience Neil Shepherd NATA Timothy Bolduc AgilentTechnologies John Kaba FloridaDepartmentofHealthOfficeofMedicalMarijuanaLiberty Sibanda Randox Laboratories Rafael Bombonato Curaleaf David Kennedy Phenomenex BenjaminSouthwSouthwell Lake SuperiorStateUniversity Kyle Boyar MedicinalGenomics Mohamed Koroma Pharmavite LLC Alicia Stell CEMCorporation Gino Braiotta ColoradoDepartmentofPublicHealthandEnvironment Julie Kowalski JAKowalski Science Support Katherine Stenerson MilliporeSigma Julia Bramante ColoradoDepartmentofPublicHealthandEnvironment Eve Kroukamp PerkinElmer Inc. Benjamin Strong NeogenCorporation Hillel Brandes MilliporeSigma Kevin Kubachka FDA Alan Sutton GWPharmaceuticals Robert Brodnick TitanAnalytical Robert LaBudde LeastCostFormulationc Hiroko Suzuki Japan food research laboratory Julie Brunkhorst TrilogyAnalytical Laboratory Mary Lee CertifiedLaboratories Christy Swoboda RomerLabs, Inc. Antoinette Burton NestleQualityAssuranceCenter Kyle Lorenzen YoungLivingEssential Oils Yijin Tang AppliedFoodScience Candice Cashman CEM Lena Madden Limerick InstituteofTechnology Oliver Tasevski ColoradoDepartmentofPublicHealthandEnvironment Melissa Chandler UCT Katerina Mastovska Eurofins Katherine Thomas NJDepartmentofHealth Joanne Compton TEQAnalytical Laboratories Deborah McKenzie AOAC Robert Thomas ScientificSolutions Steve Crupi StateofAKEHL Naren Meruva WatersCorp Gregg Tomy UniversityofManitoba avinash dalmia PerkinElmer Joish Messerly Eurofins CONSTANZA TRILLEROS GESCYAM Pearl D'Cruz PEARLConsultingLLC Ronald Miller TherapeuticHealthChoices MarianTwohig Twohig WATERSCORPORATION Danielle Deschene SCLaboratories Jenny Nelson Agilent Gordon Vrdoljak StateofCADeptofPublicHealth Lori Dodson MarylandMedicalCannabisCommission Dustin Newman InstituteofFoodSafety&Defense Ping Wan Officeof IndianaStateChemist Paul Dorenbach SCLabs Matthew Noestheden SupraResearchandDevelopment Jian Wang CanadianFood InspectionAgency Janie Dubois ContractAnalytical Services Melissa Nutter TitanAnalytical Valerie Weiler EurofinsFood Integrity& Innovation Douglas Duncan ChemHistory LLC Dane Oberhill Phytatech Marielle Weintraub Zilis Mike Esposito MCRLabs Rob O'Brien SupraResearchandDevelopment Jane Weitzel IndependentConsultant Matthew Fiala FluentCannabisCare Shawn O'Leary New JerseyDepartmentofHealth Daniel Wene New JerseyDepartmentofHealthPHEL Ross Franklin MCRLabs. LLC Vlad Orlovsky HelixChromatography Jessica Westland AGILENTTECHNOLOGIES, INC. Stephen Goldman PhytaTech Ben Orsburn Think20Labs Jeffrey Wigton WesternAlternative Bridgett Graham OrganaKannalytics Matthew Otten JackHempicine, LLCdbaOregonCBD Walter Wilson NIST Todd Griffin G2Analytical Zachary Parish LevelOne Labs Paul Winkler SCIEX Michael Halvorson AGSScientific Eric Petty ColoradoDepartmentofAgriculture Seth Wong TEQAnalytical Laboratories/Industrial Laboratories Edward Hanbidge HempTech Ireland Andrew Pham AlkemistLabs Victoria Wu ABCTesting&MateriaMedicaLabs Scott Hansen BotanacorLaboratories Melissa Phillips NIST Michele Yacopucci State HygienicLabat theUniversityof Iowa Wendi Young MileHighLabs Xuejun Zang OrochemTechnologies Inc Name Name Name
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Special Appreciation
Mike Halvorson, AGS Scientific Monica San Miguel, Millipore Sigma
AOAC Staff Scott Coates Christopher Dent Deborah McKenzie
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Chemical Contaminants Working Group: Work Since Last CASP Meeting
• Five teleconferences (October 2019 – February 2020) • One SMPR drafted (Heavy Metals), one other started (Mycotoxin) • Public comment period (February – March, 2020) • SMPR made ready for review and approval
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SMPR Title
Determination of Heavy Metals in a Variety of Cannabis and Cannabis Derived Products
Applicability: Determination of total cadmium (CAS No. 7440 ‐ 43 ‐ 9), total arsenic (CAS No. 7440 ‐ 38 ‐ 2), total lead (CAS No. 7439 ‐ 92 ‐ 1), and total mercury (CAS No. 7439 ‐ 97 ‐ 6). Any other heavy metals may be included (e.g. barium, total chromium, selenium, and silver.)
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Background on Analyte
Heavy Metals is not new subject matter
“USDA Organic” produce, superfoods, herbal products, dietary supplements, drinking water, etc.
Problems
Disease Carcinogenic Adverse Internal/Biologic Effects
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Regulatory Schemes for Heavy Metals
1 State • Top 4
~ 23 States Hg Cd Pb As
• 33
• Oral • Inhalable • Other
Operating Systems
• Cr • Ba • Ag • Se
Regulations
Delivery
1 State • Top 4
4 States • Top 4 • Cr
Dosing
Matrix
• Cr • Ba • Sb • Cu • Ni • Zn
• Daily based on BW
• Flower • Extract
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Current state ‐ by ‐ state regulatory levelsofelemental contaminants in cannabisproducts CA CA MO MO MA MA RI RI
CO CO CO AR MI MI MT NV NM NY ND OH WA ppm ppm ppm ppm ppm ppm ppm ppm ppm ppm ppm ppm ppm ppm µg/kg Bw/day ppm ppm ppm µg/kg Bw/day ppm ppm ppm ppm ppm ppm ppm ppm µg/day ppm µg/kg Bw/day ppm ppm ppm µg/day As 0.2 1.5 0.2 1.5 0.2 1.5 0.2 1.5 0.2 3 1.5 0.2 1.5 1.5 0.14 0.4 0.4 0.4 0.14 10 0.2 1.5 1 1.5 0.2 0.14 0.98 10 2 0.14 0.2 0.4 0.14 10 Cd 0.2 0.5 0.2 0.5 0.2 0.5 0.2 0.5 0.2 3 0.5 0.2 0.3 0.3 0.09 0.4 0.44 0.3 0.09 4.1 0.2 0.5 5 0.5 0.2 0.09 0.63 4.1 0.82 0.09 0.2 0.3 0.09 4.1 Pb 0.5 0.5 0.5 0.5 0.5 1/10 0.5 10 0.5 10 1 0.5 1 1 0.29 1 1 1 0.29 10 0.5 0.5/10 10 0.5 0.5 0.29 2.03 6 1.2 0.29 0.2 1 0.29 6 Hg 0.1 3 0.1 3 0.1 1.5 0.1 1.5 0.1 1 1.5 0.1 0.5 0.5 0.29 0.2 0.2 0.2 0.29 2 0.1 3/1.5 1 3 0.1 0.29 2.03 2 0.4 0.29 0.2 0.2 0.29 2 Cr 0.6 2 0.6 2 0.6 2 Ba 60 ‐ Ag 1.4 ‐ Se 26 ‐ Sb ‐ 2 Cu ‐ 2 Ni ‐ 2 Zn ‐ 20 IA MN MD MD OK PA CT LA ME ME ME MI MI
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Method Performance Requirements
Required Analytes: • Arsenic • Cadmium • Mercury • Lead
Table 1: (optional) • Antimony • Barium • Chromium • Copper
• Nickel • Silver • Zinc
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Method Performance Requirements
Limit of Quantitation (LOQ)
≤ 10 ppb ( μ g/kg)
Reproducibility (RSD R )
Repeatability (RSD r )
Range
Recovery
>100 ppb to 1 ppm ≥ 10 ppb to 100 ppb > 1 ppm to 10 ppm
15% 11% 7.3%
32% 16%
60% - 115% 80% - 115% 80% - 115%
8%
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Nature of Comment
Comment
Change/Recommendation
67 ‐ delete ",and infant formula“ 82 through 89, add CAS numbers I propose to add a paragraph prior to line 56, highlighting the Need for sample homogenization. this process step could be defined in more Detail (e.g., equipment to be used or particle size to be achieved).
Editorial
I suggest removing infant formula from the list of reference materials since it is a finished product and finished products are mentioned. In addition, I suggest adding the CAS numbers to the list of elements in Table 1 since the numbers are provided for the main elements on page 1. In my opinion, information about sample preparation is missing. A crucial step in heavy metal analysis of cannabis (no matter whether hemp or marijuana) is a thorough sample homogenization. This is, as Cannabis is know to accumulate heavy metals and this is also the reason for it's use in remediation of soil. This accumulation takes place in all plant parts (e.g., buds, stems ansd seeds), but to a different extent. As a consequence, the analysis of an inhomogeneous sample will lead to unprecise/unreproducible/unrepeatable results
Technical
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Nature of Comment
Comment
Change/Recom mendation
Applicability • You have to include more elements, because cannabis and hemp are hyper ‐ accumulators. • The following elements have been reported in the public domain: Pb, As, Cd, Hg, Ni, Si, V, B, Co, Cu, Se, Ba, Ag, Sb, Cr, Mo, Mn, Zn, Fe from a variety of sources including the growing medium, soil, fertilizers, nutrients, water, growth enhancers, environmental pollutants, and the cannabinoid extraction process. • Cr, Ni, Fe from the metallic/Stainless steel grinding/processing equipment • Pb, Cu, Zn, Ni, Cr, Fe from metallic components inside vaping devices heating coils, solder joints, tanks etc Analytical Technique • ICP ‐ OES will not quantitate at 10 ppb with good statistical reproducibility. D/Ls of Pb /Cd, as, Hg are only 1 ppb. Definitions • LOQ: What does "that can be reported at a quantitative result" mean...you have to give this statistical boundaries to have any real meaning. Check out EPA or USP definitions for guidance. • Repeatability:This very confusing. Do you man short term RSD of 2 or 3 replicate measurements. If you do you have to define a measurement or integration time. Check out instrument vendors definition of short term precision for guidance. • Reproducibility: What is meant by "RSD calculated from among laboratory data." Do you mean reproducibility over extended periods/intervals of time, or with different instruments and/or different operators. You have to be more clear. Check out USP Chapter 233 for guidance.
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Nature of Comment
Comment
Change/Recomm endation
Definitions, cont’d • Recovery: You have to be more specific when defining spike recoveries. Your definition is totally inadequate,. Check out USP Chapter 233 for guidance. Method Performance Requirements: What if the repeatability is outside these specs. The achievable precision for any element is going to be impacted by the instrument sensitivity for that element. Pb is very a very sensitive element, while As is mono ‐ isotopic and is not well ionized in the plasma. In addition, if HCl is used in the sample prep, it will produce an ArCl polyatomic interference at mass 75 which will totally overlap the As 75. For that reason, I would not include a repeatability/reproducibility spec....I would just have a % recovery spec.. But again what do you do if the results fall outside these windows? Check out ACS Reagent Chemicals methodology for heavy metals for guidance. System Suitability: • Is this section referring to the calibration...it's unclear. If so you need to suggest a calibration range, based on the LOQ and the end of the linear dynamic range for that element. So my suggestion is to use a matrix blank as zero, a 20 ‐ 50x the LOQ as the low standard (made up with the matrix blank) and a high standard which is above your expected highest sample. A mid range standard is then typically used a QC sample. You should check out USP Chapter 233 validation protocols as guidance.
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Nature of Comment
Comment
Change/Recommen dation
Reference Materials: There will not be cannabis reference material for heavy metals for some time. You just cannot use other materials like tobacco, spinach leaves or hops (not sure where infant formula came from), because the elemental suite and range is not well suited for typical levels of Pb, Cd, As and Hg in cannabis flower or cannabis products. This is why a comprehensive, validated spike recovery procedure is the only way you can ensure that high quality and reproducible data. This is the way the FDA regulates pharma labs, because there are no pharmaceutical certified reference materials to assess the validity of the analytical procedure and the accuracy of the generated data.
Validation Guidance and References: I have no idea what this is referring to. Maximum Time ‐ To ‐ Result: I'm not sure I understand what this means. Summary:
As the leader of the heavy metals task on the ACS Analytical Reagents Committee, I have been involved with writing standard methods and procedures for elemental impurities/contaminants regent chemicals for the past 20 years. We worked very closely with the USP when they updated their 100 year old sulfide precipitation heavy metals test for drug materials, at the same we were changing our ACS test. Even though the list of metals were different, the plasma spectrochemistry procedure was very similar. For that reason, I would strongly recommend you take a look at either or both methodologies to help you develop your AOAC heavy metals' method for cannabis and hemp. USP took 20 years to change its method, we took 5 years to update our ACS test. Take advantage of the knowledge and experience that has gone into developing these methods.
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Motion: Move to accept the Standard Method Performance Requirements ® (SMPR ® ) for Determination of Heavy Metals in a Variety of Cannabis and Cannabis Derived Products as presented.
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Discussion?
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DRAFT AOAC SMPR 2019.XXX; Version 6; March 11, 2020. 1 2 Method Name: 3
Determination of Heavy Metals in a Variety of Cannabis
4 5 6 7 8 9
and Cannabis Derived Products
Approved by:
Final version date : Effective date:
10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55
Intended Use :
Surveillance methods for routine monitoring
1. Applicability :
Determination of total cadmium (CAS No. 7440-43-9), total arsenic (CAS No. 7440- 38-2), total lead (CAS No. 7439-92-1), and total mercury (CAS No. 7439-97-6).
Additional elements in Table 1 may be included.
2. Analytical Technique :
Inductively Coupled Plasma based instrumentation or alternative methodology that
meets the performance requirements
3. Definitions :
Limit of Quantitation (LOQ)
The minimum concentration or mass of analyte in a given matrix that can be reported
as a quantitative result.
Repeatability
Variation arising when all efforts are made to keep conditions constant by using the same instrument and operator, and repeating during a short time period. Expressed as the repeatability standard deviation (SD r ); or % repeatability relative standard
deviation (%RSD r ).
Reproducibility
The standard deviation or relative standard deviation calculated from among- laboratory data. Expressed as the reproducibility relative standard deviation (SD R ); or
% reproducibility relative standard deviation (% RSD R ).
Recovery
The fraction or percentage of spiked analyte that is recovered when the test sample
is analyzed using the entire method.
Current state ‐ by ‐ state regulatory levels of elemental contaminants in cannabis products CA CA MO MO MA MA RI RI
CO CO CO AR
IA
MN MD MD OK
ppm ppm ppm ppm ppm ppm ppm ppm ppm ppm ppm ppm ppm ppm µg/kg
Bw/day ppm ppm
As Cd Pb Hg Cr Ba Ag Se Sb Cu Ni Zn As Cd Pb Hg Cr Ba Ag Se Sb Cu Ni Zn
0.2 0.2 0.5 0.1
1.5 0.5 0.5
0.2 0.2 0.5 0.1 0.6
1.5 0.5 0.5
0.2 0.2 0.5 0.1
1.5 0.5
0.2 0.2 0.5 0.1
1.5 0.5
0.2 0.2 0.5 0.1
3 3
1.5 0.5
0.2 0.2 0.5 0.1
1.5 0.3
1.5 0.3
0.14 0.09 0.29 0.29
0.4 0.4 0.2 0.6 1
0.4
0.44
1/10
10
10
1
1
1
1
3
3 2
1.5
1.5
1
1.5
0.5
0.5
0.2
60
1.4
26
‐ ‐ ‐ ‐
PA
CT
LA
ME
ME
ME
MI
MI
MI
MI
MT
NV
NM NY
ND OH WA
ppm µg/kg Bw/day
ppm ppm ppm ppm ppm
ppm ppm ppm µg/day ppm µg/kg Bw/day
ppm ppm ppm µg/day
0.4 0.3
0.14 0.09 0.29 0.29
10
0.2 0.2
1.5 0.5
1 5
1.5 0.5 0.5
0.2 0.2 0.5 0.1 0.6
0.14 0.09 0.29 0.29
0.98 0.63 2.03 2.03
10
2
0.14 0.09 0.29 0.29
0.2 0.2 0.2 0.2
0.4 0.3
0.14 0.09 0.29 0.29
10
4.1
4.1
0.82
4.1
1
10
0.5 0.5/10
10
6 2
1.2 0.4
1
6 2
0.2
2
0.1
3/1.5
1
3 2
0.2
2
‐ ‐ ‐
2 2 2
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Julie Kowalski Chair, CASP Chemical Contaminants Working Group
March 11, 2020
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CASP Chemical Contaminants - Mycotoxins • Engage AOAC mycotoxin expertise outside of CASP
• January 28, 2020 working group call • Initial discussion about mycotoxins SMPRs • Analytes and Matrices • Need for consolidated information
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General discussion –Two SMPRs: 1. Screening/semi ‐ quant method (e.g. ELISA) 2. Quantitative analytical method (e.g. LC ‐ MS/MS)
Working group will use the Applicability Statement of the SMPR to recommend confirmation of positive results that fail maximum regulatory limit
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Analytes*: mycotoxins are toxic metabolites of fungi aflatoxin B 1 aflatoxin B 2 aflatoxin G 1 aflatoxin G 2 (total aflatoxins) ochratoxin A *members of working group to provide additional compounds before next call
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Matrices for both SMPRs:
• Plant material (flower) –high THC and hemp
• Processed products – concentrates, extracts, etc.
• Finished products • Edibles including beverages • Vaping products
*members of working group to provide additional compounds before next call
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Need for consolidated information: • per state for United States, Canada & other legal cannabis countries • Analytes • Reporting individual or total aflatoxins • Maximum residue limits • Required matrices We will be scheduling 2nd call, if interested in helping contact: Julie Kowalski JAKScience@outlook.com
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