Microsoft Word - Candidates for 2017 ERP of the Year

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STAKEHOLDER PANEL ON STRATEGIC FOOD ANALYTICAL METHODS EXPERT REVIEW PANEL ON ETHANOL IN KOMBUCHA

METHODS FOR CONSIDERATION: Conclusion: The Expert Review Panels reviewed five (5) Kombucha methods, which were submitted in response to the Call for Methods. Methods Reviewed: Each method collected by AOAC for consideration by this ERP was assigned a set of reviewers. Methods reviewed included: KOM-01: Ethanol in Kombucha o Author(s): Blake Ebersole o Submitted by: Blake Ebersole, NaturPro Scientific • KOM-02: Fluorescent Detection of Ethanol in Kombucha via Alcohol Dehydrogenase o Author(s): Michael Valley, Jolanta Vidugiriene, James Cali o Submitted by: Michael Valley • KOM-03: Ethanol Analysis in Kombucha Drinks o Author(s): Samuel J. LaBonia o Submitted by: Samuel J. LaBonia • KOM-04: Determination of ethanol in Kombucha by Gas Chromatography-Flame Ionization Detector: Intra-Laboratory Validation o Author(s): Xin Du and Yonglin Ren o Submitted by: Xin Du • KOM-05: Determination of Alcohol Content in Kombucha Tea by Headspace Solid Phase Microextraction and Gas Chromatography-Mass Spectrometry o Author(s): Katherine K. Stenerson o Submitted by: Katherine Stenerson, Millipore Sigma •

All methods were reviewed against AOAC SMPR 2016.001, Standard Method Performance Requirements (SMPRs®) for Determination of Ethanol in Kombucha. The decisions of the September 18, 2016 ERP are shown below.

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KOMBUCHA ERP MEETING – SEPTEMBER 18, 2016

Kombucha ERP Members Present:

Kombucha ERP Members Absent:

Sneh Bhandari, Mérieux Nutrisciences (Chair) Hannah Crum, KBI Blake Ebersole, NaturPro Scientific LLC George Joseph, AssureQuality New Zealand Armen Mirzoian, TTB Katherine Stenerson, Millipore Sigma Rachel Stryffeler, The Coca Cola Company Michael Valley, Promega Corporation

Rasu Jayabalan, National Institute of Technology Rourkela (India)

Observers: Paula Brown, BCIT; Bob Clifford, Shimadzu; AJ Evinger, Health-Ade; Said Goueli, Promega Corp.; Cathy Halverson, TTB; Thomas Hektor, R-Biopharm; Norma Hill, TTB (Ret.); Ruth Ivory, Megazyme; Linda Monaci, CNR Italy; Maged Sharaf, APHA; Hemanth Shenoi, Promega Corp.; Jeff Shippar, Covance; Christopher Smith, Coca-Cola; Darryl Sullivan, Covance; John Szpylka, Mérieux Nutrisciences; Justin Trout, Health-Ade; Amelia Winslow, HealthAde; Shannon Wurfel, Coca-Cola; Rich Zywicki, Covance AOAC Staff: Scott Coates, Christopher Dent, Dawn Frazier, Deborah McKenzie

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Kombucha Method Reviews and Decisions

ERP Decisions

Consensus

Decision Date

AOAC Method #

Manuscript Title, Submitter and Reviewer

KOM-01 Ethanol in Kombucha – Gas Chromatographic Method

The ERP agreed to move this method to First Action Official Methods of Analysis Status.

MOTION to move KOM-01 to First Action Official Methods of Analysis Status (Stryffeler / Valley). 6 in favor, 0 opposed, 1 abstention. Motion passed. MOTION to accept the Final Action Requirements for KOM-

Submitted by Blake Ebersole, NaturPro Scientific LLC Primary Reviewer: Sneh Bhandari

Final action requirements: Additional information on calibration curve and associated Quantitation calculations must be provided.

01 (Valley / Stryffeler) 6 in favor, 0 opposed, 1 abstention. Motion passed.

Notes from Chair: •

The method may state precautions and safety statements. • System suitability criteria may be mentioned clearly as specific requirements. • Two different versions of the method provided one as the “method submission” and other part of the SLV data package. The former lacks many of the specific details. The method provided with the data package is the one intended to be processed for further action. The ERP agreed not to move this method to First Action Official Methods of Analysis Status. First Action Requirements: • Provision of additional data • Demonstrate that it meets the SMPR requirements • Support specificity in the method

09/18/2016

KOM-02 Fluorescent Detection of Ethanol in Kombucha via Alcohol Dehydrogenase Submitted by: Michael Valley Primary Reviewer: Armen Mirzoian Secondary Reviewer: Katherine Stenerson

MOTION not to move KOM-02 to First Action Official Methods of Analysis (Mirzoian / Stryffeler). 6 in favor, 0 opposed, 1 abstention. Motion passed. MOTION to accept the First

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Action Requirements for KOM- 02 (Stryffeler/Bhandari). 6 in favor, 0 opposed, 1 abstention. Motion passed . MOTION not to move KOM-03 to First Action Official Methods of Analysis. (Stryffeler/Joseph). 7 in favor, 0 opposed, 0 abstentions. The motion passed. MOTION to accept the First Action Requirements for KOM- 03 (Joseph / Bhandari). 7 in favor, 0 opposed, 0 abstentions. The motion passed.

KOM-03 Ethanol Analysis in Kombucha Drinks Submitted by: Samuel LaBonia Primary Reviewer: Stryffeler Secondary Reviewer: Joseph

The ERP agreed not to move this method to First Action Official Methods of Analysis Status. First Action Requirements: • Additional details regarding sample prep and instrumentation • Clarification with unit conversion and calculations • Volume by volume % should be reported • Validation data as defined by the SMPR (Analytical Range, Precision and Accuracy in Particular) • Demonstration of suitability for Kombucha • Review of suitability of methanol as internal standard

09/18/2016

KOM-04 Determination of Ethanol in Kombucha by Gas Chromotagraphy-Flame Ionization Detector: Intra-Laboratory Validation Submitted by: Xin Du Primary Reviewer: Sneh Bhandari

Method and Reviews Withdrawn

N/A

N/A

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KOM-05 Determination of Alcohol Content in Kombucha Tea by Headspace Solid Phase Micro-extraction and Gas Chromatography-Mass Spectrometry Submitted by: Katherine Stenerson Primary Reviewer: Stryffeler Secondary Reviewer: Jayabalan

The ERP agreed not to move this method to First Action Official Methods of Analysis Status. First Action Requirements: • Additional repeatability and/or reproducibility data in the appropriate matrix (Kombucha tea) • Method accuracy, mean spike recovery in Kombucha tea across matrix and analytical range.

MOTION not to move KOM-05 to First Action Official Methods of Analysis (Stryffeler/Valley). 7 in favor, 0 opposed, 0 abstentions. The motion passed. MOTION to accept the KOM-05 First Action Requirements (Valley / Ebersole). 6 in favor, 0 opposed, 1 abstention. The motion passed.

09/18/2016

• Action Items: AOAC staff to inform method authors of outcomes, including follow up actions

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STAKEHOLDER PANEL ON STRATEGIC FOOD ANALYTICAL METHODS (SPSFAM): EXPERT REVIEW PANEL (ERP) FOR ETHANOL IN KOMBUCHA

OFFICIAL CHAIR’S EXPERT REVIEW PANEL REPORT ACKNOWLEDGMENT

The undersigned Chair hereby confirms that the following document has been reviewed and constitutes the final revised version of the Official Chair’s Report for the SPSFAM Ethanol in Kombucha Expert Review Panel held on September 24, 2017.

_____________________________________________________________ SNEH BHANDARI, SPSFAM KOMBUCHA ERP CHAIRMAN

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STAKEHOLDER PANEL ON STRATEGIC FOOD ANALYTICAL METHODS EXPERT REVIEW PANEL ON ETHANOL IN KOMBUCHA

METHODS FOR CONSIDERATION: Conclusion: The Expert Review Panels reviewed five (5) Kombucha methods, which were submitted in response to the Call for Methods. Methods Reviewed: Each method collected by AOAC for consideration by this ERP was assigned a set of reviewers. Methods reviewed included: • KOM-04: Determination of ethanol in Kombucha by Gas Chromatography-Flame Ionization Detector: Intra-Laboratory Validation o Resubmission o Author(s): Xin Du and Yonglin Ren o Submitted by: Xin Du • KOM-05: Determination of Alcohol Content in Kombucha Tea by Headspace Solid Phase Microextraction and Gas Chromatography-Mass Spectrometry o Resubmission o Author(s): Katherine K. Stenerson o Submitted by: Katherine Stenerson, Millipore Sigma •

KOM-06: Enzymic method for measurement of Ethanol in Kombucha o Author(s): R. Ivory, E. Delaney, J. Larkin, V. McKie and B.V. McCleary o Submitted by: Ruth Ivory, Megazyme • KOM-07: Enzytec ™ Liquid Ethanol o Author(s): Markus Lacorn and Thomas Hektor o Submitted by: Patricia Meinhardt, R-Biopharm, Inc. • KOM-08: AP-Chrom-GCMS-Kombucha-ABV o Author(s): Michael J. Goodrich o Submitted by: Michael Goodrich, Cornerstone Labs

All methods were reviewed against AOAC SMPR 2016.001, Standard Method Performance Requirements (SMPRs®) for Determination of Ethanol in Kombucha. The decisions of the September 24, 2017 ERP are shown below.

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I.

KOMBUCHA ERP MEETING – SEPTEMBER 24, 2017

Kombucha ERP Members Present:

Kombucha ERP Members Absent:

Sneh Bhandari, Mérieux Nutrisciences (Chair) Hannah Crum, KBI Blake Ebersole, NaturPro Scientific LLC George Joseph, AssureQuality New Zealand Armen Mirzoian, TTB Katherine Stenerson, Millipore Sigma Sudhakar Yadlapalli, First Source Laboratory Solutions

Rasu Jayabalan, National Institute of Technology Rourkela (India)

Observers: Cristina Amarillas, Traditional Medicinals ; Arthur Bettge, Megazyme; Hillel Brandes. MilliporeSigma; Hannah Crum, Kombucha Brewers International; Blake Ebersole, NaturPro Scientific; Jordi Figueras, Insanitea Kombucha; Cathy Halverson, TTB; Thomas Hektor, R-Biopharm AG; Ruth Ivory, Megazyme; Scott Krepich, Phenomenex; Nancey Legg, Better Kombucha; Patricia Meinhardt; R-Biopharm Inc.; Sidney Sudberg, Alkemist Labs; Amanda Sutton, Golda Kombucha; Melanie Wadd, Golda Kombucha AOAC Staff: Scott Coates, Christopher Dent, Dawn Frazier, Tien Milor

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Kombucha Method Reviews and Decisions

#

Manuscript Title, Submitter and Reviewer

ERP Decisions

Consensus

KOM-04 Determination of Ethanol in Kombucha by Gas Chromatography-Flame Ionization Detector: Intra- Laboratory Validation

MOTION not to move this method to First Action OMA Status. (Mirzoian / Bhandari)

The ERP agreed not to move this method to First Action OMA Status for the following reasons: • Unclear how LOQ and LOD were evaluated/defined • Multiple definitions are lacking • Specificity and robustness were not addressed • No Method accuracy evaluation data using reference material available. • No data about analytical range, method precision. % Recovery data limited and require clarification as indicated in ERP review. • In summary, does not meet SMPR The ERP had no further recommendations for this method. The ERP agreed not to move this method to First Action Official Methods of Analysis Status. The ERP agreed that this method could be acceptable as a First Action OMA if additional precision data could be provided, specifically: • Repeatability study for minimum of eight (8) kombucha commercial samples. Range of 0.5% – 2% ABV. Minimum triplicate for two different days. • Provide data to demonstrate sample integrity with respect to ethanol concentration. The ERP agreed not to move this method to First Action Official Methods of Analysis Status. Key points: • Lacking safety precautions Lacking sufficient precision data •

7 in favor, 0 opposed, 0 abstentions.

The motion passed.

Submitted by: Xin Du, Murdoch University Primary Reviewer: Mirzoian Secondary Reviewer: Bhandari

KOM-05 Determination of Alcohol Content in Kombucha Tea by Headspace Solid Phase Micro-extraction and Gas Chromatography-Mass Spectrometry

MOTION to accept the KOM-05 First Action Requirements (Bhandari / Ebersole).

6 in favor, 0 opposed, 1 abstention.

The motion passed.

Submitted by: Katherine Stenerson, Millipore Sigma Primary Reviewer: Ebersole Secondary Reviewer: Jayabalan

Enzymic method for measurement of Ethanol in

MOTION not to move this method to First Action OMA Status. (Bhandari /

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Kombucha

Mirzoian) 7 in favor, 0 opposed, 0 abstentions. The motion passed.

KOM-06

The ERP agreed that the following must be addressed prior to a resubmission of this method: • RSD iR value obtained is closer to RSD R requirement of 6% and higher than RSDr requirements of <4%. • No information on accuracy of method using reference materials. • Data about demonstration of the method selectivity, no interference from kombucha components • Provide clarity to the method as per reviews • Reaction time data demonstrating the method’s required reaction time to be included in the SLV • System suitability requirement to be defined • Stability of the kit The ERP voted to adopt this method for First Action OMA Status.

Submitted by: Ruth Ivory, Megazyme Primary Reviewer: Bhandari Secondary Reviewer: Ebersole

Enzytec™ Liquid Ethanol

MOTION to move this method to First Action OMA Status. (Joseph / Mirzoian) 7 in favor, 0 opposed, 0 abstentions. MOTION to accept the Final Action Requirements for KOM—07 as presented (Joseph / Crum)

Submitted by: Patricia Meinhadrt, R-Biopharm Primary Reviewer: Joseph Secondary Reviewer: Mirzoian

Final Action requirements:

KOM-07

• The method should clearly state the potential interferants as demonstrated in the SLV. • The units of measurement should be in % ABV.

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AP-Chrom-GCMS-Kombucha-ABV

MOTION to not move this method forward to First Action OMA Status (Stenerson / Joseph) 6 in favor, 0 opposed, 1 abstention. The motion passed.

The ERP voted not to adopt this method for First Action OMA Status. The ERP voted on the following requirements which must be met prior to a resubmission of this method: • Precision data with at least 8 different kombucha samples, 3 replicates over 2 days. • Limit of quantitation (LOQ) needs to be calculated using the standard deviation of replicate data. • Units should be expressed as % ABV. • Calculations need to be corrected. • Accuracy need to be established with certified reference material as specified in SMPR • Linearity should be stated in the SLV report • Improve presentation of the SLV report

Submitted by: Michael Goodrich, Cornerstone Labs Primary Reviewer: Stenerson Secondary Reviewer: Jayabalan

KOM-08

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STAKEHOLDER PANEL ON STRATEGIC FOOD ANALYTICAL METHODS EXPERT REVIEW PANEL ON HEAVY METALS

OFFICIAL CHAIR’S EXPERT REVIEW PANEL REPORT

ACKNOWLEDGMENT

The undersigned chair hereby confirms that the following document has been reviewed and constitutes the final revised version of the Official Chair’s Report for the Heavy Metals Expert Review Panel held on February 11, 2015.

Rick Reba, Expert Review Panel Chair

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STAKEHOLDER PANEL ON STRATEGIC FOOD ANALYTICAL METHODS EXPERT REVIEW PANEL ON HEAVY METALS

METHODS FOR CONSIDERATION:

Conclusion: The Expert Review Panel reviewed one (1) heavy metals method, which had been resubmitted as recommended at the December 2, 2014 Heavy Metals ERP Meeting. Methods Reviewed: Each heavy metals method collected by AOAC for consideration by this ERP was assigned a primary and secondary reviewer. The decisions of the February 11, 2015 ERP are shown below.

Method No.

Manuscript Title

ERP Decisions (ERP Motions, Actions for Other & Additional Final Action Requirements) Required prior to First Action vote as per December 2, 2014 ERP teleconference:: 1. Data for Infant Formula (See #6 in “Recommended Actions”) 2. Internal standard clarification (Lu) 3. Verbiage around microwave digestion parameters 4. Ionization buffers carbon effect

Consensus

Decision Date

HVYM-001

Determination of Heavy Metals in Food by Inductively Coupled

ERP voted to accept HVYM-001 as a First Action Official Method of Analysis (9 in favor, 0 oppose, 1 abstain.)

Plasma – Mass Spectrometry

02/11/2015

February 11, 2015: All four requirements met as agreed by consensus.

Follow Up Actions: •

AOAC staff to move method forward to publication. • Members of the ERP can independently volunteer to assist with the provision of data in support of a final action method.

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STAKEHOLDER PANEL ON DIETARY SUPPLEMENTS EXPERT REVIEW PANEL ON HEAVY METALS

Conclusion: The Expert Review Panel reviewed five (5) methods relating to Arsenic Speciation. These methods were reviewed against AOAC SMPR 2015.006, Quantitation of Arsenic Species in Selected Food and Beverages. Methods Reviewed: Each method collected by AOAC for consideration by this ERP was assigned a primary and secondary reviewer. The decisions of the March 14, 2016 ERP are shown below. ERP Members Present: Rick Reba, Nestle (Chair); Michelle Briscoe, Brooks Applied Labs; Min Huang, Frontage; Farzaneh Maniei, Coca-Cola; Bill Mindak, FDA; Jenny Nelson, Agilent; Jenny Scifres, USDA; Christopher Smith, The Coca-Cola Company ERP Members Absent: Sneh Bhandari, M é rieux NutriSciences; Cory Murphy, CFIA; Li Sheng, EPL Analytical Services; Darryl Sullivan, Covance Observers: Joe Boison, CFIA; Min Huang, Frontage; Greg Jaudzems, Nestle; Sookwang Lee, FDA; Elaine Marley, R-Biopharm; Josh Messerly, Eurofins; Paul Milne, Keurig; Bill Mindak, FDA; Deepali Mohindra, Thermo; Jenny Nelson, Agilent; Lawrence Pacquette, Abbott; Melissa Phillips, NIST; Steve Tennyson, Perrigo Nutritionals; Socrates Trujillo, FDA; Jason Wubben, ADM; Dorothy Yang, Agilent Technologies; Jinchaun Yang, Waters; Chunyan Zhang, Abbott I. METHODS FOR CONSIDERATION:

AOAC Method #

Manuscript Title & Organization

ERP Decisions

Consensus

Decision Date March 14, 2016

ARS-01 Title: Analytical Method for the Determination of Various Arsenic Species in Rice, Rice Food Products, Apple Juice, and Other Juices by Ion Chromatography- Inductively Coupled Plasma/Mass Spectrometry.

MOTION, Mindak/Nelson, not to move ARS-01 to First Action. 8 in favor, 0 opposed, 0 abstained. The motion passed.

The ERP agreed not to take action on this method at this time. The ERP suggested that the following actions must be completed before this method can reconsidered for First Action Official Methods status: • Arsenic V contamination must be addressed.

Organization: Covance

Demonstrate use of internal standards Use of alkaline carbonate is a concern Should address total inorganic AsB peak is split. This needs to be

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resolved.

AOAC Method #

Manuscript Title / Organization

ERP Decisions

Consensus

Decision Date March 14, 2016

ARS-02 Title: High Performance Liquid Chromatography-Inductively Coupled Plasma-Mass

MOTION, Smith/Maniei, to move ARS-02 to First Action. 7 in favor, 0 opposed, 1 abstain. The motion passed. MOTION, Mindak/Smith, that the ERP agrees with the final action requirements discussed. 7 in favor, 0 opposed, 1 abstained. The motion passed.

The ERP agreed to take action on this method at this time. The ERP determined that the following actions must be completed before this method can considered for Final Action Official Methods status: • 4.10.3- More descriptive • List of equipment include a

Spectrometric Determination of Four Arsenic Species in Fruit Juice

Organization: US FDA

refractometer measuring brix if determining juice concentrate. 4.10, table 2. Provide a range for the helium flow rate. Instrument setup – add paragraph on instrument tuning. Measurement of LOD/LOQ needs clarification. Report LOQ using multiplication factor 10 instead of FDA factor 30 to align with AOAC. Precautionary statement needed around pH and co-elution and check reagents for contamination prior to use. Include acceptable range Arsenate contamination in the phosphate buffer. Matrix spikes that include AsB as Analytical range should be included in method. Robustness data for mobile phase pH range.

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well as the other species for sample spike.

AOAC Method #

Manuscript Title / Organization

ERP Decisions

Consensus

Decision Date March 14, 2016

ARS-03 Title: Speciation and

MOTION, Briscoe/Smith not to move ARS-03 to First Action. 8 in favor, 0 opposed, 0 abstained. The motion passed.

The ERP agreed not to take action on this method at this time. The ERP suggested that the following actions must be completed before this method can reconsidered for First Action Official Methods status: • Improve LOQ and precision to meet SMPR.

Determination of Inorganic Arsenic in Rice Using Liquid Chromatography-Inductively Coupled Plasma/ Mass Spectrometry: Collaborative Study Organization: Ministry of Agriculture, Forestry and Fisheries of Japan

Include SLV study reports, including accuracy and reference material. Instead of reporting inorganic species separately they should be combined.

•

•

AOAC Method #

Manuscript Title / Organization

ERP Decisions

Consensus

Decision Date March 14, 2016

ARS-04 Title: Arsenic Speciation Analysis in Beverages and Rice Based Products Ion Chromatography-Inductively Coupled Plasma–Mass Spectrometry

The ERP agreed not to take action on this method at this time. The ERP suggested that the following actions must be completed before this method can reconsidered for First Action Official Methods status: • Reevaluate LOD/LOQ and

MOTION, Scifres/Nelson not to move ARS-04 to First Action. 2 in favor, 5 opposed, 1 abstained. The motion failed.

Organization: Brooks Applied Labs

repeatability; clean this section up.

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Separation chromatogram must be included. Report formatting issues / editing errors must be addressed. Suggest authors obtain ERP reviewers summaries and address comments and concerns. Authors encouraged to re-submit method provided the above actions are completed

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AOAC Method #

Manuscript Title / Organization

ERP Decisions

Consensus

Decision Date March 14, 2016

ARS-05 Title: Arsenic Speciation in Rice and Rice Products Using High Performance Liquid Chromatography-Inductively Coupled Plasma-Mass Spectrometric Determination

The ERP agreed not to take action on this method at this time, however, the ERP also agreed that the Working Group should reconsider the limits set for rice. The ERP suggested that the following actions must be completed before this method can reconsidered for First Action Official Methods status: • Recalculate LOQ using multiplication factor 10 instead of FDA 30. • Calibrate lower to include point nearer to the LOD. • Authors encouraged to re-submit method provided the above actions are completed.

MOTION, Smith/Scifres to move ARS-05 to First Action. 3 in favor, 3 opposed, 1 abstained. The motion failed.

Organization: US FDA

II.

ACTION ITEMS: 1. Staff to inform method authors of ERP decisions. 2. Reba to provide an update to stakeholder panel and include the limits for rice in the SMPR may need additional consideration . (Completed)

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Report on the Bisphenol A (BPA) Expert Review Panel, 09/26/2017

AOAC Stakeholder Panel on Strategic Food Analytical Methods -

AOAC I N TERN AT I ON AL

STAKEHOLDER PANEL ON STRATEGIC FOOD ANALYTICAL METHODS (SPSFAM): EXPERT REVIEW PANEL (ERP) FOR Bisphenol-A (BPA)

OFFICIAL CHAIR’S EXPERT REVIEW PANEL REPORT

ACKNOWLEDGMENT

The undersigned Chair hereby confirms that the following document has been reviewed and constitutes the final revised version of the Official Chair’s Report for the SPSFAM BPA Expert Review Panel held on September 26, 2017. m MELISSA PHILLIPS, SPSFAM BPA ERP CHAIR

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STAKEHOLDER PANEL ON STRATEGIC FOOD ANALYTICAL METHODS EXPERT REVIEW PANEL ON SELECTED FOOD ALLERGENS

METHODS FOR CONSIDERATION: Conclusion: The Expert Review Panel reviewed four (4) methods for selected detection of BPA, which were submitted in response to an AOAC Call for Methods claiming to meet the AOAC SMPR XXX., Determination of free Bisphenol A (BPA) in commercially packaged ready to consume carbonated and non-carbonated water and non-alcoholic beverages. Methods Reviewed: Each method collected by AOAC for consideration by this ERP was assigned a set of reviewers. Methods reviewed included: BPA-01: Bisphenol-A in Water o Author(s): N. Reinhound o Submitted by: Nico Reinhound, Antec Scientific • BPA-02: Determination of free Bisphenol A in commercially packaged ready to consume carbonated/non-carbonated water and beverages by immunoaffinity purification and HPLC fluorescent detection o Author(s): J. Liu, Z. Wu, H. Zhang, C. Xi, X. Wang, L. Chen, D. Toth o Submitted by: Darney Toth, Vicam • BPA-03: Use of AFFINIMIP ® SPE Bisphenols as clean up method for the determination of Bisphenol A from COLA drinks by Flourescence Detection o Author(s): Kaynoush Naraghi, Sami Bayoudh, Michel Arotçaréna o Submitted by: Michel Arotçaréna • BPA-04: Determination of Bisphenol A (BPA) in Commercially Packaged Ready to Consume Carbonated and Non-Carbonated Water and Non-Alcoholic Beverages using LCMS/MS o Author(s): Siheng Li, Jeffrey Shippar, and Katerina Mastovska o Submitted by: Katerina Mastovska, Covance The methods were reviewed against AOAC SMPR XXX., Determination of free Bisphenol A (BPA) in commercially packaged ready to consume carbonated and non-carbonated water and non-alcoholic beverages. The decisions of the September 26, 2017 ERP session are shown below. •

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BPA ERP MEETING – SEPTEMBER 26, 2017 BPA ERP Members Present: Melissa Phillips, NIST (Chair) Luke Ackerman, FDA/CFSAN Xu-Liang Cao, Health Canada Mehmet Gumustas, University of Ankara Siheng Li, Covance Katerina Mastovska, Covance

BPA ERP Members Absent:

Darryl Sullivan, Covance (recused self)

Tom Siepelt, FDA Jing Tan, Abbott

Tomasz Tuzimski, Medical University of Lublin, Poland Sudhakar Yadlapalli, First Source Laboratory Solutions

Observers: Keith Griswold, Pepsico; Philip Haselberger, Abbott ; Adam Horkey, Nature’s Way; Sara Hylton, Hardy Diagnostics; Maia Jack, American Beverage Association; Hari Narayanan, Metrohm USA; Jeff Shippar, Covance Labs AOAC Staff: Scott Coates, Christopher Dent, Dawn Frazier, Tien Milor

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Bisphenol-A Method Reviews and Decisions

Manuscript Title, Submitter and Reviewers Title: Bisphenol-A in Water Author(s): N. Reinhound Submitted by: Nico Reinhound, Antec Scientific Primary Reviewer: Luke Ackerman, US FDA / CFSAN Secondary Reviewer: Xu-Liang Cao, Health Canada

ERP Decisions / Consensus

AOAC Method #

MOTION NOT to move this method to First Action Official Methods of Analysis Status (Ackerman/Cao) 9 in favor, 0 opposed, 2 abstentions. The motion passed. Reasoning/Summary: The ERP did not see data on the beverages required by the SMPR, nor was there a limit of quantitation specified or safety information. Further, the method has high potential for false positives. ____________________________________________________________ Further Recommendations / Requirements: None.

BPA-01

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Title: Determination of free Bisphenol A in commercially packaged ready to consume carbonated/non-carbonated water and beverages by immunoaffinity purification and HPLC fluorescent detection. Author(s): J. Liu, Z. Wu, H. Zhang, C. Xi, X. Wang, L. Chen, D. Toth Submitted by: Darney Toth, Vicam Primary Reviewer: Mehmet Gumustas, Ankara University Secondary Reviewer: Jing Tan, Abbott Nutrition

MOTION NOT to move this method to First Action Official Methods of Analysis Status (Ackerman/Cao) 9 in favor, 0 opposed, 2 abstentions. The motion passed. Reasoning/Summary: Although the authors have demonstrated that the methods meet most of the SMPR, there were several issues the ERP would like to see addressed prior to moving this method to First Action Official Methods Status. ____________________________________________________________ Further Recommendations / Requirements: • Repeating the spiking study without stripping the matrices. • Characterize in-house matrix based reference materials (Guidance in OMA) • LOD study with sample that has low levels of BPA already in it is acceptable.

BPA-02

• Units must be stated • Brand names removed • System suitability

• Chromatograms of blanks and spiked samples • Rephrase some of the sentences (e.g. “maybes”) • Safety caveats • Recovery bias • Additional matrices (e.g. coffee based dairy beverages) are encouraged

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Title : Use of AFFINIMIP®SPE Bisphenols as clean up method for the determination of Bisphenol A from COLA drinks by Fluorescence detection Author(s): Kaynoush Naraghi, Sami Bayoudh, Michel Arotçaréna Submitted by: Michel Arotçaréna, AFFINISEP Primary Reviewer: Melissa Phillips, NIST

MOTION NOT to move this method to First Action Official Methods of Analysis Status (Ackerman/Seipelt) 9 in favor, 0 opposed, 2 abstentions. The motion passed. Reasoning/Summary: The ERP did not see data on any of the matrices besides cola drinks. There was no safety information. There was no calibration information. Energy drinks did not meet the SMPR. There was concern about the capacity of the column. ____________________________________________________________ Further Recommendations / Requirements: None .

BPA-03

Secondary Reviewer: Tom Seipelt, Abbott

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MOTION NOT to move this method to First Action Official Methods of Analysis Status (Ackerman/Seipelt) 5 in favor, 2 opposed, 3 abstentions. The motion passed. Reasoning/Summary: Although the authors have demonstrated that the methods meet most of the SMPR, there were several issues the ERP would like to see addressed prior to moving this method to First Action Official Methods Status. ____________________________________________________________ Further Recommendations / Requirements: • Safety about ammonium fluoride • LOQ calculation in matrices (as a minimum, in coffee matrix) • Blank concentration • Chromatograms for blanks, particularly coffee • Quality control standard preps • Correction on typo re: balance • Significant figures on sample amount MOTION to accept the first action recommendations as presented (Ackerman / Yadlapalli). 8 in favor, 0 opposed, 3 abstentions. The motion passed.

Title: Determination of Bisphenol A (BPA) in Commercially Packaged Ready to Consume Carbonated and Non-Carbonated Water and Non-Alcoholic Beverages using LCMS/MS Author(s): Siheng Li, Jeffrey Shippar, and Katerina Mastovska Submitted by: Katerina Mastovska

Primary Reviewer: Kasi Somayajula, Coca-Cola Secondary Reviewer: Sudhakar Yadlapalli, 1 st Source Solutions, India

BPA-04

Action Items: AOAC staff to inform method authors of outcomes. AOAC staff to work to organize another meeting of the BPA ERP.

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AOAC I N TERN AT ION AL

STAKEHOLDER PANEL ON STRATEGIC FOOD ANALYTICAL METHODS (SPSFAM):

EXPERT REVIEW PANEL (ERP) FOR Bisrhenol-A (BPA)

OFFICIAL CHAIR’S EXPERT REVIEW PANEL REPORT

ACKNOWLEDGMENT

The undersigned Chair hereby confirms that the following document has been reviewed and constitutes the final revised version of the Official Chair’s Report for the SPSFAM BPA Expert Review Panel held on December 18, 2017.

BPA ERP CHAIR

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STAKEHOLDER PANEL ON STRATEGIC FOOD ANALYTICAL METHODS  EXPERT REVIEW PANEL ON BISPHENOL‐A (BPA) 

METHODS FOR CONSIDERATION:  Conclusion:   The Expert Review Panel (ERP) reviewed one (1) method for detection of BPA, which was a resubmitted method based  on the guidance given to the method authors at the previous meeting of this ERP on September 26, 2017.   Methods Reviewed:   Each method collected by AOAC for consideration by this ERP was assigned a set of reviewers.  Methods  reviewed included:   BPA‐04:   Determination of Bisphenol A (BPA) in Commercially Packaged Ready to Consume Carbonated and Non‐Carbonated  Water and Non‐Alcoholic Beverages using LCMS/MS  o Author(s):  Siheng Li, Jeffrey Shippar, and Katerina Mastovska  o Submitted by:  Katerina Mastovska, Covance  The method was reviewed against AOAC SMPR 2017.018., Determination of free Bisphenol A (BPA) in commercially packaged ready  to consume carbonated and non‐carbonated water and non‐alcoholic beverage.   The decisions of the December 18, 2017 ERP  session are shown below.  

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BPA ERP MEETING – DECEMBER 18, 2017  BPA ERP Members Present:    Melissa Phillips, US NIST (Chair) Luke Ackerman, FDA/CFSAN  Mehmet Gumustas, Ankara University   Siheng Li, Covance Laboratories  Katerina Mastovska, Covance Laboratories  Darryl Sullivan, Covance Laboratories  Tom Seipelt, Abbott Nutrition  Kasi Somayajula, The Coca‐Cola Company  Jing Tan, Abbott Nutrition 

BPA ERP Members Absent: 

Xu‐Liang Cao, Health Canada 

Tomasz Tuzimski, Medical University of Lublin, Poland  Sudhakar Yadlapalli, First Source Laboratory Solutions 

AOAC Staff:   Scott Coates, Christopher Dent, Dawn Frazier, Deborah McKenzie, Tien Milor 

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Bisphenol‐A Method Reviews and Decisions

AOAC  Method # 

Manuscript Title, Submitter and  Reviewers 

ERP Decisions / Consensus 

MOTION to move this method to First Action Official Methods of Analysis Status (Ackerman/Seipelt)   7 in favor, 0 opposed, 1 abstentions.  The motion passed. 

Title:   Determination of Bisphenol A (BPA) in  Commercially Packaged Ready to Consume  Carbonated and Non‐Carbonated Water and  Non‐Alcoholic Beverages using LCMS/MS

Reasoning/Summary:  The method authors have met or exceeded all of the First Action Official Methods of Analysis ® Requirements and clearly explained how they have done so. 1 ____________________________________________________________  Final Action Requirements:     Additional information about reproducibility   Ensure that juice with pulp and dairy based coffee beverages are used as matrices in the  collaborative study.    Final Action Suggestions:   Encourage use of single standard in the collaborative study, preferable a standard with qNMR  purity.   Omission of diet carbonated beverages as a matrix is acceptable.   Use of energy drinks as a matrix in the collaborative study is encouraged.   Include relevant detail about data processing.    MOTION to accept the Final Action Official Methods  recommendations and suggestions as  presented (Ackerman / Yadlapalli).  7 in favor, 0 opposed, 1 abstentions.  The motion passed.  

Author(s): Siheng Li, Jeffrey Shippar, and  Katerina Mastovska  

Submitted by: Katerina Mastovska 

Primary Reviewer:    Kasi Somayajula, The Coca‐Cola  Company

Secondary Reviewer:  Sudhakar Yadlapalli, First Source  Laboratory Solutions, India 

  BPA‐04 (Resubmission)

1  List of Revisions to BPA‐004 

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Action Items:     Method author will proceed to collaborative study.  Method author will contact AOAC prior to formal submission of collaborative study to organize a discussion with ERP Chair and AOAC staff about the Final Action Official Methods of Analysis ® submission.

Attachments: • BPA-004 Method Revision Summary (provided by method authors)

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BPA-04 Revision Summary

We appreciate the thoughtful comments made by the ERP. Please see below for our responses to the comments and the summary of the changes in the revised report (highlighted in yellow).

Safety about ammonium fluoride

•

We have added “In particular, prepare mobile phase A (1 mM ammonium fluoride in UPW) in a fume hood with appropriate personal protective equipment. Do not mix mobile phase A with an acidic solution. Flush the LC system with a 50:50 (v/v) water-acetonitrile mixture after using mobile phase A.” in the Safety section.

• LOQ calculation in matrices (as a minimum, in coffee matrix)

We have included the LOQ calculation by LOQ = blank mean + 10 standard deviations using the result obtained by 10 analysis of blank coffee drink samples. The LOQ was calculated to be 0.245 µg/L, which met the LOQ requirement of ≤ 0.5 µg/L in the SMPR.

Blank concentration

•

We have addressed the reagent blank concentration in the System Suitability/Analytical Quality Control section. For the determination of the LOQ, the mean blank coffee drink concentration is provided in Table 5. It was < 10% of the estimated LOQ.

• Chromatograms for blanks, particularly coffee

The chromatograms for all ten matrices evaluated in this study, together with the corresponding LOQ level spikes, are shown in Appendix II.

Quality control standard preps

•

The preparation of the quality control sample is described in step 2 of the Sample Preparation procedure.

Correction on typo re: balance

•

The balance accuracy typo has been corrected.

Significant figures on sample amount

•

The significant figures of sample amount have been corrected to reflect the pipet precision.

03/12/2018

STAKEHOLDER PANEL ON STRATEGIC FOOD ANALYTICAL METHODS (SPSFAM): EXPERT REVIEW PANEL (ERP) FOR Bisphenol-A (BPA)

OFFICIAL CHAIR’S EXPERT REVIEW PANEL REPORT ACKNOWLEDGMENT

The undersigned Chair hereby confirms that the following document has been reviewed and constitutes the final revised version of the Official Chair’s Report for the SPSFAM BPA Expert Review Panel held on May 22, 2018.

STAKEHOLDER PANEL ON STRATEGIC FOOD ANALYTICAL METHODS EXPERT REVIEW PANEL ON SELECTED FOOD ALLERGENS

METHODS FOR CONSIDERATION: Conclusion: The Expert Review Panel (ERP) reviewed one (1) method for detection of BPA, which was a resubmitted method based on the guidance given to the method authors at the previous meeting of this ERP on September 26, 2017. Methods Reviewed: Each method collected by AOAC for consideration by this ERP was assigned a set of reviewers. Methods reviewed included: • BPA-02: Determination of Free Bisphenol A (BPA) in Commercially Packaged Ready to Consume Carbonated/Non- Carbonated Water and Non-Alcoholic Beverages by Immunoaffinity Purification and UPLC/Fluorescence Detector • Author(s): J. Liu, Z. Wu, H. Zhang, C. Xi, X. Wang, L. Chen, D. Toth • Submitted by: Danrey Toth, Vicam The method was reviewed against AOAC SMPR 2017.018, Determination of free Bisphenol A (BPA) in commercially packaged ready to consume carbonated and non-carbonated water and non-alcoholic beverage. The decisions of the May 22, 2018 ERP session are shown below.

AOAC SPSFAM Bisphenol-A (BPA) ERP MEETING –MAY 22, 2018

BPA ERP Members Present:

BPA ERP Members Absent:

Melissa Phillips, US NIST (Chair) Luke Ackerman, FDA/CFSAN Xu-Liang Cao, Health Canada Siheng Li, Covance Laboratories Darryl Sullivan, Covance Laboratories Jing Tan, Abbott Nutrition

Mehmet Gumustas, Ankara University Katerina Mastovska, Covance Laboratories Tom Seipelt, Abbott Nutrition Kasi Somayajula, The Coca-Cola Company

Tomasz Tuzimski, Medical University of Lublin, Poland Sudhakar Yadlapalli, First Source Laboratory Solutions

AOAC Staff: Scott Coates, Christopher Dent, Dawn Frazier, Deborah McKenzie

Method # Manuscript Title, Submitter and Reviewers

ERP Decisions / Consensus

MOTION not to move candidate method BPA-02 to First Action Official Methods of Analysis Status (Ackerman/Yadlapalli) 7 in favor, 0 opposed, 1 abstentions. The motion passed. Reasoning/Summary : The method authors have provided written documentation explaining how they have addressed the original concerns expressed by the ERP on September 26, 2017 1 . However, the ERP asserted that several points required further attention prior to being voted to First Action Official Methods of Analysis ® status. These requirements and recommendations were agreed as follows: Requirements for First Action: • Authors must conduct a LOD/LOQ study using a lower concentration blank beverage sample. The LOD/LOQ must be calculated as indicated in the SMPR using the blank mean plus the standard deviation. They do not need to repeat the recovery study using this sample. • System suitability requirements must be included in the method as written to provide specific instructions to the user. For example, provide acceptance requirements for criteria listed in the SMPR. • Additional detail needed about lower level calibrant that was used in the study but preparation not described in the method. • Add information about necessary PPE in the safety section. • In Figure 4, axis labels must be added. • Parameters for immuno-affinity column should be added, including capacity and as much detail as possible. While this may be the only size/capacity offered by the manufacturer at this time, it should be clearly stated in such a way that future method users can identify the correct cartridges. Recommendations for First Action: • A concern was raised that no spiking study was conducted at the LOQ level. The ERP acknowledges that this is not a requirement of the SMPR, and when the LOD/LOQ study is repeated with a spiked lower level sample, the recovery can be inferred from that data. • In Figure 4, all three curves, including regression lines and standard deviations for coefficients “a” and “b”, should be added. • Concerns were expressed about the separation of BPA peak from the non-retained peak. Authors may want to consider modifying the chromatography to increase retention of BPA. • Concerns were expressed about the specificity of the method for BPA compared to related compounds. Authors may want to consider a quick study with some pure materials for related compounds to demonstrate selectivity either via the cleanup cartridge or the separation scheme.

Title: Determination of Free Bisphenol A (BPA) in Commercially Packaged Ready to Consume Carbonated/Non-Carbonated Water and Non-Alcoholic Beverages by Immunoaffinity Purification and UPLC/Fluorescence Detector Author(s): J. Liu, Z. Wu, H. Zhang, C. Xi, X. Wang, L. Chen, D. Toth

Submitted by: Danrey Toth

Primary Reviewer:

Mehmet Gumustas, Hitit University, Turkey

Secondary Reviewer:

Jing Tan, Abbott Nutrition

BPA-02 (Resubmission)

1 List of Revisions to BPA-002

Action Items: • AOAC Staff will provide e-ballot to ERP members to vote on requirements and recommendations. • Method author will work to incorporate recommendations into a future revision.

AOAC ERP Report Attachment 1

Address to review panel’s questions

1. “Repeating the spiking study without stripping the matrices.” All data in this report were generated by using matrices without stripping, including both LOD/LOQ and spiking study. 2. “Characterize in-house matrix based reference materials (Guidance in OMA)” Determination of BPA in blank samples and testing samples was performed following the instruction from AOAC Technical Division on Reference Materials (TDRM) and ISO/Guide 80:2014(en): Guidance for the in-house preparation of quality control materials, including homogeneity, stability, preparation and analysis. 3. “LOD study with sample that has low levels of BPA already in it is acceptable.” Following instructions from the review panel, we selected the least BPA contaminated samples (without stripping) to identify the LOD an LOQ. A total of 10 replicates were analyzed for each sample type, and the mean and SD were calculated. Since the blank samples were contaminated with BPA, the blank mean reflect the actual contamination levels of the samples, not noise generated by the sample matrix or instruments. The blank mean was subtracted for the LOD and LOQ calculation. 4. “Units must be stated” All units are stated. 5. “Brand names removed” Brand names are removed. 6. “System suitability” According to email communication with AOAC review panel, “The ERP would like to see some guidance for the user related to understanding and demonstrating that the system is working as expected. This often includes analysis of a standard sample (such as an in-house reference material as described above) and/or a calibrant, with tolerance limits for peak area, resolution, retention time, linearity, etc. in addition to blank checks. As well, the SMPR requires negative controls (blanks) and low and mid-point positive controls”. In this report, standard samples were tested every day the test was performed to generate a standard curve. Negative controls (blanks) and low, mid-point and high positive controls (for example, samples spiked at 0, 1, 4, 16 and 32 ng/mL BPA levels) were tested in three different

matrices. The chromatograms showed consistent retention time, symmetric and narrow peaks, reproducible peak area, with no background interference. Both the recovery and precision met the AOAC requirements. The test results of the spiked samples correlated well to the spiked levels with R-squared values close to 1 in the detection range from 0 to 32 ng/mL. Please refer to the report for more information on the system suitability of the method. 7. “Chromatograms of blanks and spiked samples” The chromatogram of blanks (0 ppb spiked samples, and 0 ppb blank control) and spiked samples was shown in Fig 1, 2, 3. 8. “Rephrase some of the sentences (e.g. “maybes”)” Rephrased. 9. “Safety caveats” In this report, we stated “acid, base and organic solvents were prepared in the ventilation hood” under “Reagent Preparation” in the section of “Method”. 10. “Recovery bias” Mentioned in email communication with AOAC review panel, “It was noted by the ERP that the recovery of BPA decreased when the level of BPA increased. This should be thoroughly investigated.” Based on study and the results in this report, there is no significant recovery difference between low (1µg/mL) and high spiking level (32µg/mL). Please see Table 6 of this report. Additionally, all biases in this report are within the range required by AOAC criteria. 11. “Additional matrices (e.g. coffee based dairy beverages) are encouraged” In this report, dairy based coffee was evaluated.

AOAC I NT E RNAT! ON AL

STAKEHOLDER PANEL ON STRATEGIC FOOD ANALYTICAL METHODS (SPSFAM): EXPERT REVIEW PANEL (ERP) FOR Cannabinoid Quantitation

in Extracts and/or Plant Material

OFFICIAL CHAIR’S EXPERT REVIEW PANEL REPORT

ACKNOWLEDGMENT

The undersigned Chair hereby confirms that the following document has been reviewed and constitutes the final revised version of the Official Chair’s Report for the SPSFAM Cannabis Expert Review Panel held on November 19, 2018.

MELISSA PHILLIPS, SPSFAM CANNABIS ERP CHAIR

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STAKEHOLDER PANEL ON STRATEGIC FOOD ANALYTICAL METHODS  EXPERT REVIEW PANEL ON QUANTITATION OF CANNIBINOIDS IN EXTRACTS AND PLANT MATERIALS 

METHODS FOR CONSIDERATION:  Summary:   The Expert Review Panel (ERP) reviewed two (2) methods for cannabinoid quantitation, which were originally submitted  in response to an AOAC Call for Methods issued on June 9, 2017.  On December 15, 2017, the ERP reviewed these methods and  provided feedback to the authors on what would be required to obtain First Action Official Methods of Analysis status.  These methods  were resubmitted for ERP review during a teleconference on August 13, 2018, after which an electronic ballot was issued to all ERP  members.  The ballot results were not unanimous, so the ERP reconvened on November 19, 2018 ,  to discuss ballot results and conduct  another vote, which can override the original vote with a 2/3 majority.    Resubmitted Methods Reviewed:    CAN‐01:   Quantitation of Cannabinoids in Cannabis Dried Plant Materials and concentrates Using Liquid Chromatography –  Diode Array Detection Technique with Optional Mass Spectrometric Detection  o Author(s):  Lukas Vaclavik, Frantisek Benes, Ales Krmela, Veronika Svobodova, Jana Hajslova and Katerina Mastovska  o Submitted by:  Katerina Mastovska, Covance   CAN‐02 :  Leaner and Greener Analysis of Cannabinoids  o Author(s):  E Mudge, SJ Murch, PN Brown  The methods were reviewed against AOAC SMPR 2017.001, Quantitation of Cannabinoids in Cannabis Concentrates and/or AOAC  SMPR 2017.002, Quantitation of Cannabinoids in Dried Plant Materials.   The decisions of the November 18, 2018 , ERP session are  shown below.

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CANNABIS ERP MEETING – November 19, 2018 Cannabis ERP Members Present:    Quorum established  Melissa Phillips, US NIST (Chair)  Susan Audino, S.A. Audino & Associates  Yohei Arao, Shimadzu  Nour‐Eddine ES‐SAFI, Mohammad V University, Rabat  Heather Harris, Forensic Chemistry Consultant  Chris Hudalla, Proverde Labs  Holly Johnson, Alkemist Labs  Katerina Mastovska, Covance  Elizabeth Mudge, BCIT  Curtis Phinney, Curtis S. Phinney CNS  Paul Reibach, Smithers Viscient  Kate Rimmer, US NIST  Christian Sweeney, Cannabistry  Tomasz Tuzimski, Medical University of Lublin  Sudhakar Yadlapalli, First Source Laboratory Solutions

Cannabis ERP Members Absent: 

Peter Indick, Microbak Laboratories  Markus  Roggen, OutCo 

AOAC Staff:   Christopher Dent, Dawn Frazier, Deborah McKenzie

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