(spsfam)...meat powder and related materials; and –finished products including infant formula,...
TRANSCRIPT
Draft, Do Not Distribute
Stakeholder Panel on Strategic Food Analytical Methods
(SPSFAM)
Stakeholder Panel Meeting
March 12, 2018, 1:00pm – 5:00pm
SPSFAM Chairman: Erik Konings, Nestlé Research Centre, Lausanne, Switzerland
Attendees (Present During All or Part of the Meeting)
Susan Audino, S.A. Audino & Associates Lei Bao, AOAC China Section Charles Barber, NIST Brad Barrett, LECO Corporation Sneh Bhandari, Mérieux NutriSciences Joe Boison, Independent Consultant Sara Bryson, Conagra Brands Dominik Burger, DSM Nutritional Products Esther Campos Gimenez, Nestlé Bob Clifford, Shimadzu Jo Marie Cook, Florida Department of Agriculture Hans Cruijsen, FrieslandCampina Jennifer Donelson, VUV Analytics Jon Draher, Abbott Nutrition Aurelie Dubois, International Dairy Federation Janie Dubois, University of Maryland Jaap Evers, International Dairy Federation Steven Gendel, US Pharmacopeia Ed George, Thermo Fisher Scientific Brendon Gill, Fonterra Co-Operative Group Richard Gray, Neogen
Keith Griswold, Pepsico Philip Haselberger, Abbott Nutrition Thomas Hektor, R-Biopharm Anthony Hitchins, US FDA (Ret.) Ferro Imola, MicroVal Ruth Ivory, Megazyme Holly Johnson, American Herbal Products Association Estela Kneetman, INTI Erik Konings, Nestlé Joe Konschnik, RESTEK Scott Krepich, Phenomenex Mary Kay Krogull, Eurofins Soo Kwang Lee, US FDA Chengzhu Liang, AOAC China Section Alex Liu, SCIEX Elaine Marley, R-Biopharm Katerina Mastovska, Covance Joanne Mayer, ADM Sean McClure, Abbott Nutrition Patricia Meinhardt, R-Biopharm Josh Messerly, Eurofins Scientific Bill Mindak, Mindak Professional Services Melissa Phillips, US NIST Curtis Phinney, Cutis S. Phinney, CNS
Robert-Jan Raterink, Triskelion B.V. Catherine Rimmer, US NIST Joe Romano, Waters Corporation Andre Santos, Agilent Technologies, Inc. Tom Seipelt, Abbott Nutrition Victoria Siegel, Eurofins Jayant Shringapure, Tyson Foods, Inc. Dustin Starkey, Abbott Nutrition Katherine Stenerson, MilliporeSigma Cheryl Stephenson, Eurofins Scientific John Szpylka, Mérieux NutriSciences Nancy Thiex, AAFCO Marina Torres, LATU Martine Van Gool, FrieslandCampina Morgan Wallace, Rheonix Wayne Wargo, Abbott Nutrition Nicole Wawrzyniak, Rheonix Thomas Weiss, R-Biopharm Landon Wiest, Restek Joost Witsenburg, MicroVal Laura Wood, US NIST Sudhakar Yadlapalli, First Source Laboratory Solutions Jinchuan Yang, Waters Corporation Joyce Zhu, Jamieson Laboratories
AOAC Staff (Present During All or Part of the Meeting)
Scott Coates, Christopher Dent, Dawn Frazier, Jonathan Goodwin, Nora Marshall, Deborah McKenzie, Tien Milor, La’Kia Phillips, Robert Rathbone
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Draft, Do Not Distribute
I. Welcome and Introductions
Konings welcomed all to the 2018 AOAC Mid-Year Meeting’s Stakeholder Panel on Strategic FoodAnalytical Methods (SPSFAM, or Food Panel). Konings advised that there would be a minor change to theagenda: Boison will present on veterinary drug residues ahead of the other scheduled presentations.Konings then asked for a motion to approve the meeting minutes from the September 24, 2017 SPSFAMMeeting.
MOTION to approve September 24, 2017 SPSFAM Meeting Minutes (Szpylka/Mindak)19 in favor, 0 opposed, 1 abstention. The motion passed.
II. Working Group Update: Veterinary Drug Residues
Boison took the floor with a presentation1 to review the veterinary drug residue project fitness forpurpose, action items from the kick-off meeting in Atlanta, working group’s proposed drug groupings,concentration levels, and next steps. He advised that the group has been meeting by teleconference andis in the process of developing an SMPR for detection as well as identification of 151 drugs in food andfinished products. Because of the qualitative aspect, research based on AOAC Official Methods of AnalysisAppendices H and N was required. The group has attempted to group them together to take advantageof their chemical makeups. Boison said the group will now move on to complete the SMPR and bring itbefore SPSFAM in August at the AOAC Annual Meeting.
III. SMPRs for Approval: Sugar Working Group
Sugar Working Group Co-Chairs Szpylka and Thiex took the floor with their presentation2 to provideupdates on their working group and to present the first two SMPRs their group has developed. Szpylkaand Thiex noted that one of AOAC’s largest working groups ever, with a roster of almost 100 individuals.The chairs reviewed the original fitness for purpose statements (one for sugar, one for fructan, and one forlow-lactose), the working group’s work to date, background of the analytes (sugar and fructan) and theSMPR key points for each. Comments submitted during the public comment period were addressed, twoof which resulted in changes to the SMPR. The first comment resulted in adding the language “Methoddata packages must include relevant data regarding interferences and instabilities, such as those listed inTable 2. Data packages must include data to demonstrate that the sugar composition in the extract is arepresentation of the true sugar composition in the food product and assess the stability of extracts over theduration of the test.” The second comment indicated that the reference materials section had been leftout of the Sugar SMPR, so this has been replaced with AOAC’s standard guidance on reference materials.Others present at the meeting had additional suggestions for reference materials. Gendel of USP statedthat they possess reference materials – ACTION for AOAC in conjunction with Thiex to incorporate theseinto the SMPR prior to publication.
1 Attachment 1:- Boison Presentation 2 Attachment 2:- Szpylka / Thiex Presentation
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MOTION to approve the document Standard Method Performance Requirements for Sugars in Animal Feed, Pet Foot, and Human Food as amended at this meeting (Szpylka/Gendel).
20 in favor, 0 opposed, 1 abstention. The motion passed.
Thiex stated that AOAC currently has two methods for fructan, but neither are sufficient for the community’s present needs, partly because they do not break down inulin, whereas the applicability statement of this SMPR clearly states the inulin must be measured. Thiex reviewed the Fructans SMPR key points, including the addition of agavins. Thiex advised that only one comment was submitted for this SMPR, that being that there was a typo in the operating range section, and this has now been corrected. The co-chairs then opened the floor for discussion. A SPSFAM member suggested adding “greater than” (>).
MOTION to approve the document Standard Method Performance Requirements for Fructans in Animal Food (Animal Feed, Pet Food, and Ingredients) as amended at this meeting (Szpylka/Rimmer)
21 in favor, 0 opposed, 0 abstentions. The motion passed.
Konings then introduced Cruijsen as the newest co-chair of the Sugars working group. Cruijsen is leading the low-lactose SMPR development and provided a brief presentation3 to the group. Cruijsen explained that the efforts of this working group are to develop an international standard suitable for the determination of lactose (low and free) in dairy products and ingredients. He said the group is making progress and expects to complete the draft SMPR at the working group’s next meeting.
IV. Update on Cannabis Working Group
Audino, Chair of the SPSFAM Cannabis Working Group, then took the floor with an update presentation4
on the activities of that working group. She said that the group has, to date, completed three SMPRs5, allof which are now published. The group is not working on an SMPR for detection of pesticides in dry plantmaterial. More work is needed on this new SMPR, however, it is expected that it will be brought forSPSFAM approval during the SPSFAM session during the AOAC Annual Meeting in Toronto. Audinocontinued, stating she hopes that we will be able to launch a new Cannabis initiative once the pesticideSMPR is complete.
V. Future Topics of Interest for SPSFAM
Konings took the floor to discuss future topics of interest. To start this conversation, he gave apresentation6 on furan and alkyl furans in a variety of matrices. Furan, he explained, is the parentcompound of a class of related substances collectively known as “furan.” It is present in a variety ofcooked foods, as well as baby food and coffee. Rodent studies have shown that it is a potent livertoxin and carcinogen, which may be carcinogenic to humans. Current methods are insufficient andunstandardized, and this is an important area where SPSFAM could get involved. He asked ifanyone in the room would be interested in supporting such a project, please contact AOAC staff.
3 Attachment 3:- Cruijsen Presentation 4 Attachment 4:- Audino Presentation 5 SMPR 2017.001, SMPR 2017.002, SMPR 2017.019 6 Attachment 5:- Konings Presentation
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List of Attachments
• Attachment 1:- Boison Presentation
• Attachment 2:- Szpylka / Thiex Presentation
• Attachment 3:- Cruijsen Presentation
• Attachment 4:- Audino Presentation
• Attachment 5:- Konings Presentation
• Attachment 6:- Approved SMPRs with Changes from 3/12
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AOAC INTERNATIONALSTAKEHOLDER PANEL ON STRATEGIC
FOOD ANALYTICAL METHODS (SPSFAM)
DR JOE BOISON, Working Group ChairDetection of Selected Veterinary Drug Residues in Food Project
March 13, 2018
Gaithersburg Marriott Washingtonian Hotel
Project Milestones for the 2017 Annual Meeting and Beyond
• September 2017 Annual Meeting: The Working Group Chair presented a “Launch Presentation” Initiative to the Stakeholders
• Past President of the China Section of the AOAC shared developments in that region to veterinary drug residues analysis
• October 2017 to February 2018: The Working group met by teleconferences to develop strategies for the project and draft SMPRs
• March 2018 Mid‐Year Meeting: Working Group Chair to present an update and draft SMPRs for approval by SPSFAM .
• April 2018 to August 2018: Working Group will meet by Teleconferences to draft SMPRs
• August 2018 at the Annual Meeting in Toronto: Working Group Chair will present Draft SMPRs for approval by SPSFAM
• Following the Annual Meeting in August 2018: A call for Methods and Call for Experts and the creation of an AOAC Expert Review Panel to review submitted methods for consideration
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Action Items from 2017 Annual Meeting Held in Atlanta, Georgia
• A draft Fitness for Purpose Statement was developed and accepted by the Stakeholder Panel for the method which was to be based on LC‐tandem MS.
• The method must be capable of checking the compliance with respect to worldwide regulatory limits.
• Fitness For Purpose Statement: The method should be applicable to the analysis of veterinary drugs in:– Raw food materials such as raw milk, meat, fish, seafood and eggs;
– Semi finished food products such as skimmed milk powder, whey protein concentrate/hydrolysate, lactose, meat powder and related materials; and
– Finished products including infant formula, milk and meat‐based infant cereals, and baby foods
Working Group Activities since the 2017 Annual Meeting
• It was clarified that the LC‐MS/MS method to be developed should be capable of detecting the presence and/or absence of a target analyte in the applicable matrix with the capacity to provide identification of the analyte of interest.
• In that respect, it will have to meet the guidelines for qualitative chemistry methods published as– Appendix N (2013; ISPAM Guidelines for Validation of Qualitative Binary Chemistry Methods) and
– Appendix H (2012; Probability of Detection as a Statistical Model for the Validation of Qualitative Chemistry Methods)
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Working Group Activities since the 2017 Annual Meeting
• To facilitate the development of the multi‐residue analytical method for the 151 compounds initially provided by the Sponsors of the project, the working group has sorted out the analytes into 17 principal veterinary drug families as follows:
Working Group Activities since the 2017 Annual Meeting
Drug Family Number of Drugs Included
Aminoglycosides 7
Anthelmintics/Avermectins 23
Beta‐Lactams 18
Benzamidazoles/Anthelmintics 5
Beta Agonists/Growth Promoters 5
Coccidiostats 21
Fluoroquinolones/Quinolones 6
Glycopeptides/Polypeptides 6
Hormones 12
Lincosamides 2
Macrolides 11
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Working Group Activities since the 2017 Annual Meeting
Drug Family Number of Drugs Included
Non‐Steroidal Anti‐inflammatory Drugs (NSAIDs) 9
Organophospahtes/Pyrethroids 17
Sulfonamides 18
Tetracyclines 4
Tranquilizers 3
Miscellaneous 17
Total Number of Drugs in List 187
Working Group Activities since the 2017 Annual Meeting
• It was also clarified that the compounds to be considered in this validation exercise will be those veterinary drugs that have approved veterinary medicinal use in food animal production.
• In that respect, the Working Group has defined the threshold concentration (target testing level) based on the lowest established maximum residue limit (MRL) that will be used to establish the criteria for the positive detection and identification of an analyte in a sample.
• The analytical testing range has also been defined where appropriate from 0.5 or 0.1* the lowest established MRL (Target Testing level) to 10 * Target Testing Level
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Target Concentration Levels for the Compounds of Interest in Milk
Fluid Milk
Concentration Range (ppb) Number of Compounds within the Target Range
0.05 ‐ 10 35
11 – 50 42
51 ‐ 100 28
101 – 200 11
201 – 600 1
Muscle Tissue Concentration
0.15 ‐ 10 37
11 ‐ 50 42
51 ‐ 100 68
101 ‐ 200 20
201 ‐ 1000 26
1001 ‐ 6000 4
Strategies for Next Steps
• Identify the number of these compounds that should be present in a method for raw milk using the criterion that the drug must be approved for use in dairy production
• Identify the number of these compounds that should be present in a tissue method using the criterion that they should be approved for livestock and poultry and egg production
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Strategies for Next Steps
• Develop SMPRs for the different groups of veterinary drugs in the different matrices:
• Raw food materials • Semi finished products• Finished products• Working Group Chair to present SMPRs to Stakeholder Panel for approval at the 2018 Annual meeting
• Following the Annual Meeting, a call for methods and expert reviewers will be initiated by the AOAC staff.
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AOAC STAKEHOLDER PANEL ON
STRATEGIC FOOD ANALYTICAL METHODS
Sugar Working Group – SMPR PresentationMarch 13, 2018
Co‐Chairs:
John Szpylka, Mérieux NutriSciencesNancy Thiex, Thiex Laboratory Solutions
Marriott Washingtonian Center, Gaithersburg, Maryland, USA
Fitness for Purpose As Agreed March 13, 2017
Fitness for purpose for sugar: Individually measure free nutritional sugars, minimally: fructose, glucose, sucrose, maltose, lactose, and galactose found in ingredients and foods consumed by animals, pets, and humans. The analytical method must account for common interferences, such as sugar alcohols in these matrices.
Fitness for Purpose for Dietary Fructan in Animal Feed, Pet Food, and Ingredients: Measure total dietary fructan such as inulin and fructooligosaccharides in animal feed, pet food, and the corresponding ingredients. The method must distinguish this compound from interfering compounds such as free glucose, fructose, sucrose and other carbohydrates.
Lactose: Measure the amount of lactose in dairy products, including products containing daily ingredients that are low lactose or lactose-free.
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SPSFAM Sugar Working Group Work To Date
•6 teleconferences (December 2017 – March 2018)
•2 SMPR Drafts Completed
•Public comment period (February, 2018)
•SMPRs made ready for SPSFAM review and approval
SPSFAM Sugar Working Group Members
John Szpylka Merieux NutriSciences Nancy Thiex Thiex Laboratory Solutions
Belisario Acevedo ASINAL SAS Douglas Lloyd Holt Dr Pepper Snapple Group Mariusz Sliwinski Instytut Innowacji Przemyslu Mleczarskiego Sp. z o.o.
Parul Angrish Thermo Fisher Jeff G. Horst Agri‐King Inc Georgina Smyth Public Analysts Laboratory
Sean Austin Nestle Research Center Martha Jennens Covance Laboratories Kathryn Stanley Archer Daniels Midland Company
Knuk Erik Bach Knudsen Aarhus University Diana C. Kavolis The Hershey Company Monique Steegmans Tiense Suikerraffnaderji Analytical Services
Charles A. Barber NIST Erik J. M. Konings Nestle Research Center Hiroko Suzuki Japan Food Research Laboratories
Daniel Berg Covance Scott Krepich Phenomenex Kathy Swartout VUV Analytics
Sneh D. Bhandari Merieux NutriSciences Dana A. Krueger Krueger Food Laboratories, Inc. Naim Tahiri Birra Peja
Sharon L. Brunelle AOAC INTERNATIONAL (Contractor) Markus Lacorn R‐Biopharm AG Richard Ten Eyck AAFCO
Kaitl in Cahil l Q Laboratories, Inc. Cheryl L. Lassitter NOAA ‐ DOC, NMFS, NSIL Rodriguez LATU ‐ Chromatography And Mass Spectrometry Department
Jane Caldwell Midwest Laboratories Sookwang Lee FDA Peter J. Van Soest Cornell University
Christian Campargue Danone Research Alex Liu SCIEX Tom Vennard Covance Laboratories
France Cho Maxxam Analytics Kai Liu Eurofins Nutrition Analysis Center Roberta Vidal Pepsico
Mark W. Coll ison Archer Daniels Midland Company Bozena D. Lusiak Nestle Purina Hedegaard IDF
Hans Cruijsen FrieslandCampina Eva Lynch Rock River Laboratory Ioannis Vrasidas Eurofins Food Testing The Netherlands
Manisha Das U.S. FDA Katerina Mastovska Covance Laboratories Yannis Vrasidas Eurofins Food Testing Netherlands
Marcel De Vreeze Institute (NEN) Barry V. McCleary Megazyme Paul Wehling Medallion Labs / General Mills
Jennifer Donelson VUV Analytics Gaston M. Mercier Canada THEO WICLEF KAGISHA RWANDA BUREAU OF STANDARDS
Dr. Aurelie Dubois International Dairy Federation Pierre L. Metra Merieux NutriSciences Paul Winkler SCIEX
Dr. Gustaaf S. Duchateau Unilever Research Vlaardingen Lucia Monti CREA‐ZA Ronald Winter FDA
David Ell ingson, M.S. Covance Laboratories Hari Narayanan Metrohm USA Inc Bryan Wirthwine Q Laboratories, Inc.
Mr. Jay Gandhi Metrohm‐Peak, Inc Salvatore Parisi COIF Association, Italy Doug Wolfe McCoy & McCoy Laboratories, Inc.
Dr. Frank Gottsleben Anton Paar OptoTec GmbH Giampaolo Perinello Merieux NutriSciences Laura Wood NIST
Jonathan Hache Canadian Food Inspection Agency Melissa Meaney Phil l ips NIST David C. Woollard Eurofins New Zealand Laboratories
Ms. Gale Hagood Mississippi State University Miachael Raessler MPI Biochemie Sudhakar Yadlapall i First Source Laboratory Solutions LLP
Mohamed Hamad Microbac Laboratories Inc. Lars M. Reimann Eurofins Scientific, Inc. Xun Yan Amway Corp
Phil ip Andrew Haselberger Abbott Nutrition Catherine A. Rimmer NIST Jinchuan Yang Waters Corporation
Thomas Hektor R‐Biopharm AG Alejandra Rodriguez International Dairy Federation Zheng Yang Cargil l
Ryan Hoefling ICM Tech Development Joe Romano Waters Corporation Guhong Zhao Northland Laboratories
Dr. Steve Holroyd Fonterra Co‐operative Group Ltd. Sandra Salleres Biolan Microbiosensors
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Background: Sugar
• For animal feeds, current sugar analyses typically rely on extraction, acid hydrolysis of solubilized carbohydrates, and measurement as reducing sugars, or measurement of total extracted carbohydrates using condensation reactions.
– Inappropriately includes oligosaccharides and other solubilized carbohydrate in the sugar measurement. Also for some feeds, active amylases digest carbs into sugars thus artificially increasing the measured sugar amount.
• For measuring individual sugars in foods, traditional HPLC methods have difficulty
– separating some monosaccharides from each other, and
– resolving sugars from interfering compounds such as sugar alcohols
Background: Sugar
• Currently there are no approved methods for individually measuring mono- and di-saccharides in animal feed or pet food.
• RI methods do not achieve desired level for low level sugar guarantees.
• AOAC Official Method 974.06 Sugars (Total) in Animal Feed Modified Fehling Solution Method
• Several issues on accounting for different sugars being present
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Sugar SMPR Key Points
Applicability
• Individually measure free nutritional sugars, minimally: fructose, galactose, glucose, sucrose, maltose, and lactose found in selected ingredients and foods consumed by animals, pets, and humans. The analytical method must account for potential interferences (see list provided) in these matrices. Methods that target a narrower matrix scope will also be considered when appropriate.
Sugar SMPR Key Points
Potential Interferants• Non‐target mono, di‐ and tri‐ saccharides (e.g., maltotriose interfering
with maltose)
• Enzymatic activity (amylase, invertase)
• Hydrolytic activity (e.g., acidic)
• Organic acids
• Glucose with higher degrees of polymerization
• Sugar alcohols, such as: glycerol, erythritol, xylitol, sorbitol, mannitol, maltitol, lactitol, isomalt
• Hydroxylated compounds (non‐targeted carbohydrates, sugar alcohols, sugar acids, sucralose, etc.)
• Salts, such as sodium chloride
• Amine containing compounds (glucosamine HCl, amino acids, peptides, glycoproteins, etc.)
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Sugar SMPR Key Points
• Method data packages must include performance data covering the method claimed matrices. A useful tool can be found in food pyramid concept described in Annex F of Appendix F the AOAC Official Methods of Analysis. Matrix variations in non‐sugar carbohydrate and moisture content must be investigated and data provided. For example, using the food pyramid in sector 7, a matrix may be either high in sugar or high in non‐sugar carbohydrates (e.g., starch, sugar alcohols), each of which may affect method performance.
• Method data packages must include relevant data regarding interferences and instabilities.
Comments Submitted for Sugar SMPR
Comment Response
There should be significant evaluation of the method for finished pet foods before it is accepted, to avoid significant problems with interferants. Otherwise, there are quite a few common ingredients in pet food which would cause interference.
SMPR states “Method data packages must include relevant data regarding interferences and instabilities”, and includes a list of classes of potential interents with clear examples. Recommend no change to SMPR.
Can you please provide clarification in the SMPR if the method must be written to encompass all sugars in one?
The SMPR implies a single method to measure the at least six free sugars. The working group agreed to a minimum set of six free sugars. Recommend no change to SMPR.
SMPR should state somewhere that submission of methods that only cover a subgroup of sugars in selected matrices are also of interest.
The minimum number of sugars is clearly defined" . . . minimally: fructose, galactose, glucose,sucrose, maltose, and lactose . . .“. Recommend no change to SMPR.
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Comments Submitted for Sugar SMPR
Comment Response
Sample stability needs to be evaluated for extraction time (depending on solution) and also overall shelf life after extraction due to enzymes and microbial activities in these matrices.
A paragraph was added to Section 7. “Method data packages must include relevant data regarding interferences and instabilities, such as listed in Table 2. Data packages must include data to demonstrate that the sugar composition in the extract is a representation of the true sugar composition in the food product and assess the stability of extracts over the duration of the test.“
Comments Submitted for Sugar SMPR
Comment Response
No change but an ERP should get some guidance when judging a method to be in accordance to this SMPR. Otherwise an endless discussion would occur which is not due to a non‐validated method but to an unclear SMPR.If a method developer submits a method for sucrose‐glucose‐fructose quantification in bread and Cookies, it is up to a method user if this "narrower matrix range" is appropriate or not.
1) If the submitted method is applicable only to a subset of foods or feeds, that information must be clearly described to allow ERP deliberation if the method satisfies Stakeholder needs.2) As written, the minimum number of sugars that must be measured by a method is six regardless of the "narrower matrix scope" clause.Recommend no change to SMPR.
I am concerned that there is no section for reference materials in this SMPR.
This was an oversight by the working group. A reference material section was added as Section 8 and includes example Reference Materials Appendix F in OMA.
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Method Performance Requirements: Sugar
Recovery, repeatability and reproducibility parameters *
Analytical range 0.1% ‐ 5% 5 % ‐ 50 % 50 % ‐ 100%
Recovery, % 90 ‐ 110 95‐105 97 – 103
RSDr, % ≤7 ≤5 ≤3
RSDR, % ≤10 ≤8 ≤4
* Reported as the individual sugars (fructose, glucose, sucrose, maltose, lactose and galactose.
Discussion?
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Motion for Sugar SMPR
Move to approve the Standard Method Performance Requirements (SMPRs) for Sugars in Animal Feed, Pet Food, and Human Food
Background: Dietary Fructans
• Dietary fructan is water‐soluble class encompassing oligosaccharide
and polysaccharide carbohydrates
– Comprised predominantly of DP>3 fructose molecules and containing no
more than one‐third glucose molecules.
• This polymer of fructose molecules may or may not contain a terminal
glucose molecule, and includes inulin and FOS.
– Fructans are not digested by enzymes in the small intestine but can be
fermented in the large intestine.
• Nutritionally and compositionally distinct from other carbohydrates
such as sugars, starch, and other forms of dietary fiber.
• Primary sources of fructan are cool season grasses, chicory, and
onions.
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Background: Fructans
Currently two AOAC methods for fructan in foods (999.03 and 997.08); however, not fit-for-purpose for animal food.
• Acid hydrolysis is more effective than use of inulinase (effective on inulin) for analysis of fructans in cool season grasses.
• Hydrolysis of current methods may be modified for use in animal food
Fructans SMPR Key Points
Applicability
• Measure total dietary fructan, such as inulin, levan, branched fructans, agavins (agave fructans) and fructooligosaccharides, in animal feed, pet food, and the corresponding ingredients. The method must be capable of distinguishing this compound from interfering compounds such free glucose, fructose, sucrose and other polysaccharides.
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Fructans SMPR Key Points
Validation Guidance
• Method data packages must include performance data covering the method claimed matrices. A useful tool can be found in food pyramid concept described in Annex F of Appendix F the AOAC Official Methods of Analysis.
• Method data packages must include relevant data regarding interferences from other carbohydrates. Method developers are responsible for assessing interferences with their method.
Comments Submitted for Fructans SMPR
• A typo was corrected in the operating range and LOQ. Corrected to:
• Operating range 0.2% ‐ 100 % (2g/kg to 1000 g/kg) of dry matter
• Limit of quantitation (LOQ)* 0.2% (2g/kg) of dry matter
• No additional comments received.
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Method Performance Requirements: Fructans
Analytical range, LOQ and linearity requirements
Operating range 0.2% ‐ 100 % (2 mg/kg to 1000 mg/kg) of
dry matter
Limit of quantitation (LOQ) 0.2% (2 mg/kg) of dry matter
Linearity of standard curve r ≥ 0.999, and 95 % confidence limit of
the y intercept includes zero
Recovery, repeatability and reproducibility parameters
Range 0.2% ‐ 1 % 1% ‐ 10 % 10 % ‐ 100%
Recovery, % 90 ‐ 110 93 ‐ 107 95 ‐ 105
RSDr, % ≤7 ≤5 ≤3
RSDR, % ≤14 ≤10 ≤6
Discussion?
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Motion for Fructans SMPR
Move to accept the Standard Method Performance Requirements for Standard Method Performance Requirements (SMPRs) for Fructans in Animal Food (Animal Feed, Pet Food, and Ingredients)
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AOAC‐SPSFAM Sugars working group update
Low‐ LACTOSE
Hans Cruijsen, John Szpylka and Nancy Thiex
March , 2018
2
• Objective
Develop an international standard suitable for the determination of lactose (low and free) in Dairy Products and ingredients.
This project on lactose is a joint AOAC and ISO/IDF collaboration
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Lactose
Fitness for Purpose Statement as Agreed on September 24, 2017
“Measure the amount of lactose in dairy products, including products containing dairy ingredients that are low lactose or lactose‐free.”
Standard Method Performance Requirements (SMPR)
Call for methods etc.
Analytical Needs-Low level lactose
Infant formula and follow-on-formula “lactose free” <10 mg/100 kcalca. 6.5 mg/100 ml (Ready to feed)
2
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SMPR & Applicability (draft)
Standard Method Performance Requirements (SMPRs) for Lactose in low lactose or lactose free Milk , milk products, and products containing dairy ingredients.
ApplicabilityMeasure lactose found in milk , milk products, and products containing dairy ingredients that are low lactose or lactose free. The analytical method must account for potential interferences (See Table 1) in these matrices. This scope does include “lactose free” infant formulas and adult nutritionals.
Next time in Working group
Method Performance Requirements
Call for reference materials
Tuesday, March 13 at 12:00pm ET
(Salon G & Remote participation)
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Thank youfor your attention
Back –up slides
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Analytical Methods (for info only)
Polarimetric methods (AOAC 896.01‐ lactose in milk)
Gravimetric methods (AOAC 930.28‐ lactose in milk)
Mid‐infrared spectrophotometric method (AOAC 972.16 and ISO 9622 |IDF 141)
Enzymatic methods (both AOAC and ISO/IDF)
GC methods
Capillary electrophoreses‐ Electrochemical detection (CE‐ED)
HPLC‐RI reference method for milk, dried milk and cream (ISO 22662 |IDF 198)
High performance anion‐exchange chromatography (HPAEC) –pulsed amperometric detection (PAD)
Options for products
“Lactose free” milk
Cultured milk drinks including yoghurts
Processed and natural (aged) cheeses
Cottage and ricotta cheese
Infant formula (lactose free)
Ingredients
Edible casein products (codex stan 234)
Whey protein (isolate)
Whey protein concentrate
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Cannabis Working Group Updates
AOAC MID‐YEAR MEETING – ROCKVILLE, MD
SUSAN AUDINO, PHD
MARCH 12, 2018
Working Group Accomplishments
AOAC SMPR® 2017.001: Identification & Quantitation of Cannabinoids in
Cannabis Concentrates
AOAC SMPR® 2017.002: Identification & Quantitation of Cannabinoids in
Dried Plant Materials
AOAC SMPR® 2017.019: Identification & Quantitation of Cannabinoids in
Edible Chocolate
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Working Group AccomplishmentsIn progress: SMPR – Pesticide Residue(s) in Dried Flower
Pilot Project in Progress:
•SPEX and Restek offered multi‐pesticide mixes to 10 volunteer labs.
•Mixes are (1) 73 required throughout the US, and (2) ~100 required in Canada
•No expectations for method or validation.
•Results will be reviewed, summarized, and presented to WG.
Expected SMPR Completion: May 2018
More Attention is NeededVeterinary Applications
Heavy Metals
Additional Food Matrices
Residual Solvents
Spectroscopic Methods
Rapid Tests Suitable for Grow Facilities
Rapid Tests for Dispensaries
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Why is this Important to AOAC?
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US CANNABIS ‐ 2013
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Alaska
Hawaii
California
Oregon
Washington
Montana
Idaho
Nevada
Utah
Arizona New Mexico
Colorado
Wyoming
North Dakota
South Dakota
Nebraska
Kansas
Oklahoma
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US CANNABIS ‐ 2015
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Maps translate to:
*Approximately:
2165 Dispensaries
890 Grow/Cultivation Facilities
91 Third Party Testing Laboratories
*As gathered by quick internet search in March 2018
THANK YOU
Questions? Discussion?
410‐459‐9208
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Dr. Erik Konings
Nestlé Research Centre, Lausanne, Switzerland
March 12, 2018
AOAC Midyear Meeting, Rockville, MD, March 12‐16, 2018
Stakeholder Panel on Strategic Food Analytical Methods
Potential Working Group Launch: Furan and Alkyl Furans in Coffee, Cereal Products, and Baby Foods
Furan
Furan is the parent compound of a class of structurally‐related substances collectively known as ‘furans’, which are found in a wide assortment of foods, contributing to their sensory characteristics.
Structuraly‐related alkyl furans (e.g. 2‐methyl, 3‐methyl, etc.)
The term "furans" is frequently used to describe a larger class of compounds of varying structures including, for example, nitrofurans. "Furans" is also used as an abbreviation for the dioxin‐like substances, dibenzofurans. Furan is clearly different from many of these "furans", in terms of structure, toxicology and exposure.
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Furan in foods
• Furan is present in a variety of cooked and/or heat processed foods, including canned and jarred foods (soups, sauces, gravies, pasta) as well as baby food in jars, baked bread, breakfast cereals and coffee.
• First detected in the 1960s, furan is part of the human diet as it can be formed through traditional cooking methods.
Health concern Furan and methylated analogs
• Rodent studies indicate that furan is a potent liver toxin and carcinogen, which is possibly carcinogenic to humans (IARC Group 2B).
• Genotoxicity cannot currently be excluded with certainty, and no safe level of exposure determined.
• Similar concerns raised for some alkylated furans: 2‐and 3‐methylfuran, 2,5‐dimethylfuran, and 2‐pentylfuran.
• According to EFSA (2017): furan and methylated analogues share similar liver toxicities with similar potencies and should be grouped together human health concern due to low MoE.
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Exposure based on EFSA, 2017
• Most important contributors: baby foods in jars (in infants and toddlers), and coffee (in adults and elderly).
• Grains and grain‐based products is the most contributing for toddlers, other children, and adolescents.
• Inclusion of methylated furans into overall exposure assessment substantially increases (3 times) exposure in adults (levels in coffee).
Furan Testing in foods
• Sampling, sample preparation and handling largely contribute to variability due to the volatility of furan and its analogues.
• Reliability of testing methods, non‐availability of standard method for furan analogues, needs to be addressed.
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Analytical methods
• Analytical data used for current risk assessment are largely based on non‐standardized analytical methods and sampling/sample handling procedures.
• No Certified Reference Materials available.
• However, dietary furan exposure assessments provided by different authorities worldwide are generally in agreement.
Methods available
• EN‐16629:2015: Determination of furan in coffee and coffee products by headspace gas chromatography and mass spectrometry (HS GC‐MS).
• US‐FDA: Determination of Furan in foods (2004).
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SOME CHALLENGES FOR ANALYSIS
Which analytes to cover in addition to furan?
• 2‐ and 3‐methyl Furan, Health Canada (2010)‐ Baby foods, Coffee, Canned foods
• furan, 2‐methylfuran, 2‐ethylfuran, 2‐butylfuran, 2‐pentylfuran, 2‐acetylfuran, furfural and furfuryl alcohol, University Messina Italy (2018)‐ baby foods
• furan, 2‐methylfuran and 2‐pentylfuran, Guelf Canada (2016) –fruit juices
• furan, 2‐methylfuran, 2,5‐dimethylfuran, vinyl furan, 2‐methoxymethyl‐furan and furfural; Department of Food Science and Technology Iran (2015) – Coffee products
• furan and 2‐methylfuran, 2‐ethylfuran, 2, 5‐dimethylfuran, 2‐propylfuran, 2‐butylfuran, 2‐pentylfuran; State Key Laboratory of Food Science and Technology China (2016)‐ Heat Processed food
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What and when to measure?
• Each ingredient/finished product “as consumed” considering volatility of compounds?
• 50% level reduction in coffee preparation due to dilution, evaporation, and partial extraction (Goldmann et al. 2005)
Goldmann et al. 2005
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Technology to measure?
• Generally used: Headspace‐Solid Phase Microextraction‐Gas Chromatography‐ Mass Spectrometry (HS‐SPME‐GC‐MS).
• Preference for isotope dilution approach for quantification.
• Commercial availability of all labeled internal standards?
Matrices to include?
• Coffee
–Whole roasted beans, roast & ground, soluble coffee and the beverage.
• Cereal products
– Limited information on type of products/age categories.
• Jarred baby foods
– Vegetables, meat‐based higher compared to fruit.
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If you are interested to support Standard development on Furan please contact:
Or
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Version 3, 2/26/18 1 2 Standard Method Performance Requirements (SMPRs) for Fructans in Animal Food 3 (Animal Feed, Pet Food, and Ingredients) 4 5 Intended Use: Reference/regulatory method. 6 7 1. Purpose 8
AOAC SMPRs describe the minimum recommended performance characteristics to be 9 used during the evaluation of a method. The evaluation may be an on-site verification, a 10 single-laboratory validation, or a multi-site collaborative study. SMPRs are written and 11 adopted by AOAC stakeholder panels composed of representatives from the industry, 12 regulatory organizations, contract laboratories, test kit manufacturers, and academic 13 institutions. AOAC SMPRs are used by AOAC expert review panels in their evaluation of 14 validation study data for method being considered for Performance Tested MethodsSM 15 or AOAC Official Methods of AnalysisSM, and can be used as acceptance criteria for 16 verification at user laboratories. 17
18 2. Applicability 19
Measure total dietary fructan, such as inulin, levan, branched fructans, agavins (agave 20 fructans) and fructooligosaccharides, in animal feed, pet food, and the corresponding 21 ingredients. The method must be capable of distinguishing this compound from 22 interfering compounds such free glucose, fructose, sucrose and other polysaccharides. 23
24 3. Analytical Technique 25
26 Any analytical technique(s) that measures the analyte(s) of interest and meets the 27 following method performance requirements is/are acceptable. 28 29 4. Definitions 30 31 Animal and Pet Foods.—Material consumed or intended to be consumed by animals 32 other than humans that contributes nutrition, taste, or aroma or has a technical effect 33 on the consumed material. This includes raw materials, ingredients, and finished 34 product. (AAFCO) 35 36
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Fructans.- Any DP ≥ 3 carbohydrate with one or more fructosyl-fructose linear or 37 branched linkages which constitute a majority of the linkages in which fructose is the 38 major constituent and glucose content is 33% or less. Examples include inulin, levan, 39 branched fructans (e.g. agave fructans), and fructooligosaccharides (FOS). 40 41 Ingredients.- The base materials used in the formulation of animal and pet foods. 42 43 Limit of quantitation (LOQ).— LOQ is the lowest level of analyte in a test sample that can 44 be quantified at a specified level of precision. 45 46 Repeatability.-- Variation arising when all efforts are made to keep conditions constant 47 by using the same instrument and operator (in the same laboratory) and repeating during 48 a short time period. Expressed as the repeatability standard deviation (SDr); or % 49 repeatability relative standard deviation (%RSDr). 50 51 Reproducibility.-Variation arising when identical test materials are analyzed in different 52 laboratory by different operators on different instruments. The standard deviation or 53 relative standard deviation calculated from among-laboratory data. Expressed as the 54 reproducibility standard deviation (SDR); or % reproducibility relative standard deviation 55 (% RSDR). 56 57 Recovery.-The fraction or percentage of analyte that is measured when the test sample 58 is analyzed using the entire method. 59 60 5. Method Performance Requirements 61 62
Table 1. Analytical range, LOQ and linearity requirements Operating range 0.2% - 100 % (2 g/kg to 1000 g/kg) of dry matter Limit of quantitation (LOQ)* 0.2% (2 g/kg) of dry matter Linearity of standard curve r ≥ 0.999, and 95 % confidence limit of the y intercept includes zero *Methods that do not achieve this LOQ will still be considered
63 Table 2. Recovery, repeatability and reproducibility parameters Range 0.2% - 1 % >1 % - 10 % >10 % - 100% Recovery, % 90 - 110 93 - 107 95 - 105 RSDr, % ≤7 ≤5 ≤3 RSDR, % ≤14 ≤10 ≤6
64 6. System Suitability Tests and/or Analytical Quality Control 65 66
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Suitable methods will include blanks, and appropriate check standards. 67 68 7. Reference Material(s): 69 70 Refer to Annex F: Development and Use of In-House Reference Materials in Appendix F: 71 Guidelines for Standard Method Performance Requirements, 19th Edition of the AOAC 72 INTERNATIONAL Official Methods of Analysis (2012). Available at: 73 http://www.eoma.aoac.org/app_f.pdf 74 75 8. Validation Guidance 76
Method data packages must include performance data covering the method claimed 77 matrices. See table 3 for suggested matrices. A useful tool can be found in food 78 pyramid concept described in Annex F of Appendix F the AOAC Official Methods of 79 Analysis. 80
Method data packages must include relevant data regarding interferences such as from 81 sugars, sugar alcohols and other carbohydrates. Method developers are responsible for 82 assessing interferences with their method. 83
84 9. Maximum Time-to-Results 85 None. 86 87 Table 3: Suggested Matrices 88 89
• Wet and dry animal foods for a variety of species (swine, ruminants, poultry, fish, 90 equine, dog, cat, etc.) 91
• Pet treats 92 • Forages, including cool season grasses 93 • Both linear (inulin and levan) and branched fructans 94 • Feed ingredients including fructan containing vegetables 95
96 97
98 99
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Version 5, 01/17/2018 1 2 Standard Method Performance Requirements (SMPRs) for Sugars in Animal Feed, Pet 3 Food, and Human Food 4 5 Intended Use: Reference/regulatory method to measure individual mono- and di-6 saccharides, in animal feed, pet food, and human food. 7 8 1. Purpose 9
AOAC SMPRs describe the minimum recommended performance characteristics to 10 be used during the evaluation of a method. The evaluation may be an on-site 11 verification, a single-laboratory validation, or a multi-site collaborative study. SMPRs are 12 written and adopted by AOAC stakeholder panels composed of representatives from the 13 industry, regulatory organizations, contract laboratories, test kit manufacturers, and 14 academic institutions. AOAC SMPRs are used by AOAC expert review panels in their 15 evaluation of validation study data for method being considered for Performance Tested 16 MethodsSM or AOAC Official Methods of AnalysisSM, and can be used as acceptance 17 criteria for verification at user laboratories. 18
2. Applicability 19
Individually measure free nutritional sugars, minimally: fructose, galactose, glucose, 20 sucrose, maltose, and lactose (see table 1 for additional information on analytes) found 21 in selected ingredients and foods consumed by animals, pets, and humans. The 22 analytical method must account for potential interferences (See Table 2) in these 23 matrices. Methods that target a narrower matrix scope will also be considered when 24 appropriate. 25
3. Analytical Technique 26 Any analytical technique(s) that measures the analyte(s) of interest and meets the 27
following method performance requirements is/are acceptable. 28 29 4. Definitions 30
31 Animal and Pet Foods.—Material consumed or intended to be consumed by animals 32 other than humans that contributes nutrition, taste, or aroma or has a technical effect 33 on the consumed material. This includes raw materials, ingredients, and finished 34 product. (AAFCO) 35 36 Human Food.—Material consumed or intended to be consumed by adult humans. For 37 the purpose of this SMPR, this does not include infant formulas nor adult nutritionals. 38 39
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Ingredients.- The base materials used in the formulation of animal food and human 40 food. 41 42 Sugars.— The sugars in the analytical scope are minimally fructose, galactose, glucose, 43 sucrose, maltose, and lactose. 44
45 Repeatability.-- Variation arising when all efforts are made to keep conditions constant 46 by using the same instrument and operator (in the same laboratory) and repeating 47 during a short time period. Expressed as the repeatability standard deviation (SDr); or 48 % repeatability relative standard deviation (%RSDr). 49 50 Reproducibility.-Variation arising when identical test materials are analyzed in different 51 laboratory by different operators on different instruments. The standard deviation or 52 relative standard deviation calculated from among-laboratory data. Expressed as the 53 reproducibility standard deviation (SDR); or % reproducibility relative standard deviation 54 (% RSDR). 55 56 Recovery.-The fraction or percentage of analyte that is measured when the test sample 57 is analyzed using the entire method. 58
59 60 5. Method Performance Requirements 61 62
Table 3. Recovery, repeatability and reproducibility parameters*
Analytical range 0.1% - 5% >5 % - 50 % >50 % - 100%
Recovery, % 90 - 110 95-105 97 – 103
RSDr, % ≤7 ≤5 ≤3
RSDR, % ≤10 ≤8 ≤4
* Reported as the individual sugars [fructose, glucose, sucrose, maltose, lactose, and galactose]. 63 64 6. System Suitability Tests and/or Analytical Quality Control 65 Suitable methods will include blanks, and appropriate check standards. 66 67 68 69 70 7. Validation Guidance 71
Method data packages must include performance data covering the method claimed 72 matrices. A useful tool can be found in food pyramid concept described in Annex F of 73 Appendix F the AOAC Official Methods of Analysis. Matrix variations in non-sugar 74 carbohydrate and moisture content must be investigated and data provided. For 75
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example, using the food pyramid in sector 7, a matrix may be either high in sugar or high 76 in non-sugar carbohydrates (e.g., starch, sugar alcohols), each of which may affect 77 method performance. 78
Method data packages must include relevant data regarding interferences and 79 instabilities, such as listed in Table 2. Data packages must include data to demonstrate 80 that the sugar composition in the extract is a representation of the true sugar 81 composition in the food product and assess the stability of extracts over the duration of 82 the test. 83
8. Reference materials 84 85 Refer to Annex F: Development and Use of In-House Reference Materials in Appendix F: 86 Guidelines for Standard Method Performance Requirements, 19th Edition of the AOAC 87 INTERNATIONAL Official Methods of Analysis (2012). Available at: 88 http://www.eoma.aoac.org/app_f.pdf 89 90 Potential reference materials, depending on method scope, may include the following: 91 92 NIST 3233 – Breakfast cereal 93 NIST 2383A – Baby Food 94 NIST 3282 – Juice 95 NIST 1849A – Infant Formula 96 IRMM BCR644 – Artificial foodstuff 97 Add USP reference materials 98 99 100
9. Maximum Time-to-Results 101 None. 102 103 104
105
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Table 1: Additional Information on Analytes 106 Common Name
IUPAC Name CAS Number
Molecular Structure
Fructose (3S,4R,5R)-1,3,4,5,6-Pentahydroxyhexan-2-one
57-48-7
Galactose (3R,4S,5R,6R)-6-(hydroxymethyl)oxane-2,3,4,5-tetrol
59-23-4
Glucose (2R,3S,4R,5R)-2,3,4,5,6-Pentahydroxyhexanal 50-99-7
Sucrose
(2R,3R,4S,5S,6R)-2-[(2S,3S,4S,5R)-3,4-dihydroxy-2,5-bis(hydroxymethyl)oxolan-2-yl]oxy-6-(hydroxymethyl)oxane-3,4,5-triol
57-50-1
Maltose
2-(hydroxymethyl)-6-[4,5,6-trihydroxy-2-(hydroxymethyl)oxan-3-yl]oxyox ane-3,4,5-triol
69-79-4
Lactose β-D-galactopyranosyl-(1→4)-D-glucose 63-42-3
107
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Table 2: Potential Interferants 108 109 • Non-target mono, di- and tri- saccharides (e.g., maltotriose interfering with maltose) 110 • Enzymatic activity (amylase, invertase). 111 • Hydrolytic activity (e.g., acidic) 112 • Organic acids 113 • Glucose with higher degrees of polymerization 114 • Sugar alcohols, such as: 115
o glycerol 116 o erythritol 117 o xylitol 118 o sorbitol 119 o mannitol 120 o maltitol 121 o lactitol 122 o isomalt 123
• Hydroxylated compounds (non-targeted carbohydrates, sugar alcohols, sugar acids, 124 sucralose, etc.) 125
• Salts, such as sodium chloride. 126 • Amine containing compounds (glucosamine HCl, amino acids, peptides, glycoproteins, etc.) 127
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