Food Authenticity NTT SMPR (Comments)

AOAC INTERNATIONAL FOOD AUTHENTICITY/FRAUD Non-Targeted Testing (NTT) Standard Method Performance Requirements (SMPR®)

Working Group Review (January 2020)

AOAC INTERNATIONAL 2275 Research Blvd., Suite 300 Rockville, MD, 20850

UNITED STATES dboyd@aoac.org

Draft AOAC Standard Method Performance Requirements (SMPR) for Non-Targeted 1 Testing (NTT) of Ingredients for Food Authenticity/Fraud Evaluation of Extra Virgin 2 Olive Oil; version 2; December 27, 2019 5 AOAC SMPRs ® describe the minimum recommended performance characteristics to be used 6 during the evaluation of a method. The evaluation may be an on-site verification, a single- 7 laboratory validation, or a multi-site collaborative study. SMPRs are written and adopted by 8 AOAC using the consensus of stakeholders representing the industry, government, and academic 9 and/or research institutions. AOAC SMPRs are used by AOAC expert review panels in their 10 evaluation of validation study data for method being considered for Performance Tested 11 Methods SM or AOAC Official Methods of Analysis SM and can be used as acceptance criteria for 12 verification at user laboratories. 15 This document contains assessment parameters on the performance of Non-Targeted Testing 16 (NTT) methods to monitor extra virgin olive oil (EVOO) for the probable presence of Economically 17 Motivated Adulterants (EMA). 18 19 Intentionally designed to be generic, this SMPR was designed for Non-Targeted Testing (NTT) 20 methods developed to be applicable to the broadest range of potential methods using innovative 21 analytical platforms and chemometric approaches. Methods submitted based on this SMPR must 22 yield binary analytical results (i.e. “Authentic” or “Not Authentic”). 25 A non-targeted method to be used to evaluate EVOO for possible EMAs. Any method generating 26 a baseline fingerprint of the authentic material and comparing test sample fingerprints to assess 27 differences will be considered. The final binary result identifies test samples as either authentic 28 or potentially adulterated. This method demonstrates reliability using the requirements listed in 29 this SMPR. 30 31 The scope of the NTT method will be defined by the authentic samples used in generating the 32 baseline fingerprint. 35 Applicability Statement — a general statement about the intended purpose and scope of the 36 method entailing key aspects of expected achievements for the specific situation and 37 circumstances. Key points to cover are the intended matrix, the purpose, and an indication of 38 sensitivity, specificity, and significance (USP Appendix XVIII). 39 40 Authentic Samples — Samples representative of the genuine commodity. Ideally these samples 41 should represent the food’s or ingredient’s variability seen naturally in the commodity. The 42 authentic samples used to generate the product baseline fingerprint will be used to properly 43 define the NTT method testing scope. 44 45 Baseline Fingerprint – A food-specific model created by software evaluation of collected 46 analytical data. 47 3 4 1. Purpose 13 14 2. Applicability 23 24 3. Analytical Technique 33 34 4. Definitions

48 Economically Motivated Adulteration —The fraudulent addition of non-authentic substances or 49 removal or replacement of authentic substances without the purchaser's knowledge for 50 economic gain of the seller (USP Appendix XVIII). 51 52 False Origin — Extra Virgin Olive Oil containing mislabeled geographic and botanical sources. 53 54 Authentic EVOO — The type(s) of EVOO used to generate the baseline fingerprint. The method’s 55 scope of authenticity is defined by the EVOO(s) used in generating the baseline fingerprint. 56 57 Single Laboratory Validation — Demonstration by one laboratory of method performance on 58 samples described in Table 1. 59 60 Multilaboratory Validation — Demonstration between laboratories using adulterated samples 61 created by a third-party group and supplied blindly to the participating laboratories.

62 63 64 65 66

5. Method Performance Requirements

Table 1: Method Performance Requirements

Test

Adulterant

%Adulterant in Test Materials

Number of Samples to be Tested 1

Number of Test Results Qualified as Adulterated

Baseline

None (Authentic EVOO)

0%

Establish Baseline Fingerprint 2

Validation using Authentic Samples 3

0%

30

0

None

Validation 4 Validation Validation 4 Validation 4 Validation 4 Validation 4 Validation 4 Validation 4

5% 5% 5% 5% 5% 5% 5% 5%

30 30 30 30 30 30 30 30

30 30 30 30 30 30 30

Sunflower Oil

Validation 4

Corn Oil

Hazelnut Oil

Canola Oil

Safflower Oil Non-EVOO False Origin

30 1. Multiple samples from the same batch of adulterated material can be used for method evaluation. 67 2. Full details on protocol used to establish an authentic fingerprint must be supplied. 68 3. Method validation using authentic samples shall cover the entire scope used in creating the baseline fingerprint. 69 4. Method validation using adulterated samples shall cover the entire scope used in creating the baseline 70 fingerprint.

71 72 73

6. System Suitability Tests and/or Analytical Quality Control

Suitable methods will include blanks, and appropriate check standards. 74 75 7. Validation Guidance 76 a) Data demonstrating method performance is required. 77

78 79 80 81 82 83 84 85 86 87 88 89 90 91 92 93 94 95 96 97 98

b) Samples: Complete documentation for the collection and use of authentic samples is must be supplied by the method authors. The scope of authentic samples used to construct the “authentic” profile must be applicable to the defined scope of the NTT method. Expansion of the scope is possible with the inclusion of additional authentic samples into the baseline calibration, and validation using the protocol listed in this SMPR. c) For single lab validation studies, the method will be evaluated using prescribed adulterated materials as shown in Table 1. Methods approved at this level will proceed to a second level of evaluation where blinded samples containing unknown adulterants will

be sent to participating laboratories.

d) Methods submitted based on these SMPRs must yield binary analytical results (i.e.

“Authentic” or “Not Authentic”). e) Available guidance documents :

a. AOAC INTERNATIONAL Guidelines for Validation of Botanical Identification Methods,

Journal of AOAC International Vol. 95, No. 1, 2012

b. Statistical analysis of interlaboratory studies. LII. Sample size needed to meet performance requirement on proportion. http://lcfltd.com/AOAC/tr347-SAIS-LII-

sample-size-needed-for-PR-for-proportion.pdf

8. Maximum Time-to-Results

None.

9. Reference Materials 99 A defined set of authentic reference samples is used to construct the “authentic” profile. 100 Detailed protocols used to identify reference materials as authentic and to create adulterated 101 samples must be supplied. 102

Draft AOAC Standard Method Performance Requirements (SMPRs) for Non-Targeted 1 Testing (NTT) of Ingredients for Food Authenticity/Fraud Evaluation of Liquid Raw 2 Bovine Milk; version 2; December 27, 2019 5 AOAC SMPRs® describe the minimum recommended performance characteristics to be used 6 during the evaluation of a method. The evaluation may be an on-site verification, a single- 7 laboratory validation, or a multi-site collaborative study. SMPRs are written and adopted by 8 AOAC using the consensus of stakeholders representing the industry, government, and academic 9 and/or research institutions. AOAC SMPRs are used by AOAC expert review panels in their 10 evaluation of validation study data for method being considered for Performance Tested 11 Methods SM or AOAC Official Methods of Analysis SM and can be used as acceptance criteria for 12 verification at user laboratories. 15 This document contains assessment parameters on the performance of Non-Targeted Testing 16 methods to monitor liquid raw bovine milk for the probable presence of Economically Motivated 17 Adulterants (EMA). 18 19 Intentionally designed to be generic, this SMPR was designed for Non-Targeted Testing (NTT) 20 methods developed to be applicable to the broadest range of potential methods using innovative 21 analytical platforms and chemometric approaches. Methods submitted based on this SMPR must 22 yield binary analytical results ( i.e. “Authentic” or “Not Authentic”). 25 A non-targeted method to be used to evaluate bovine milk for possible EMAs. Any method 26 generating a baseline fingerprint of the authentic material and comparing test sample 27 fingerprints to assess differences will be considered. The final binary result identifies test 28 samples as either authentic or potentially adulterated. This method demonstrates reliability 29 using the requirements listed in this SMPR. 30 31 The scope of the NTT method will be defined by the authentic samples used in generating the 32 baseline fingerprint. 35 Applicability Statement – a general statement about the intended purpose and scope of the 36 method entailing key aspects of expected achievements for the specific situation and 37 circumstances. Key points to cover are the intended matrix, the purpose, and an indication of 38 sensitivity, specificity, and significance (USP Appendix XVIII). 39 40 Authentic Samples – Samples representative of the genuine commodity. Ideally these samples 41 should represent the food’s or ingredient’s variability seen naturally in the commodity. The 42 authentic samples used to generate the product fingerprint will be used to properly define the 43 NTT method testing scope. 44 3 4 1. Purpose 13 14 2. Applicability 23 24 3. Analytical Technique 33 34 4. Definitions

Baseline Fingerprint – A food-specific model created by software evaluation of collected 45 analytical data. 46 47 Economically Motivated Adulteration – The fraudulent addition of non-authentic substances or 48 removal or replacement of authentic substances without the purchaser's knowledge for 49 economic gain of the seller (USP Appendix XVIII). 50 51 Authentic Liquid Raw Bovine Milk – The milk used to generate the baseline fingerprint which 52 defines the method’s scope of authenticity. 53 54 Single Laboratory Validation – Demonstration by one laboratory of method performance on 55 samples described in Table 1. 56 57 Multilaboratory Validation – Demonstration between laboratories using adulterated samples 58 created by a third-party group and supplied blindly to the participating laboratories. 61 62 Table 1: Method Performance Requirements for raw bovine milk 5. Method Performance Requirements

59 60 63 64

Test

Adulterant

% Adulterant in Test Materials

Number of Samples to be Tested 1

Number of Test Results Qualified as Adulterated

Baseline

None (Authentic Milk)

0%

Establish Baseline Fingerprint 2

Validation using Authentic Samples 3

None

0%

30

0

Validation 4 Validation 4 Validation 4 Validation 4 Validation 4 Validation 4 Validation 4 Validation 4

Urea

0.06%

30 30 30 30 30 30 30 30

30 30 30 30 30 30

Melamine

0.015%

Water

0.5% 0.1%

Sucrose

Whey

1%

Vegetable Oils (Notably soy oil)

0.1%

Maltodextrin

0.1% 0.1%

30

65 66 67 68 69 70

Starch 30 1. Multiple samples from the same batch of adulterated material can be used for method evaluation. 2. Full details on protocol used to establish an authentic fingerprint must be supplied. 3. Method validation using authentic samples shall cover the entire scope used in creating the baseline

fingerprint.

4. Method validation using adulterated samples shall cover the entire scope used in creating the baseline

fingerprint.

71 73 74 75 76 77 78 79 80 81 82 83 84 85 86 87 88 89 90 91 92 93 94 95 96 97

6. System Suitability Tests and/or Analytical Quality Control 72 Suitable methods will include blanks, and appropriate check standards.

7. Validation Guidance

a) Data demonstrating method performance is required.

b) Samples: Complete documentation of for the collection and use of authentic samples is must supplied by the method authors. The scope of authentic samples used to construct the “authentic” profile must be applicable to the defined scope of the NTT method. Expansion of the scope is possible with the inclusion of additional authentic samples into the baseline calibration, and validation using the protocol listed in this SMPR. c) For single lab validation studies, the method will be evaluated using prescribed adulterated materials as shown in Table 1. Methods approved at this level will proceed to a second level of evaluation where blinded samples containing unknown adulterants will

be sent to participating laboratories.

d) Methods submitted based on these SMPRs must yield binary analytical results (i.e.

“Authentic” or “Not Authentic”). e) Available guidance documents :

a. AOAC INTERNATIONAL Guidelines for Validation of Botanical Identification Methods, Journal of AOAC International Vol. 95, No. 1, 2012 b. Statistical analysis of interlaboratory studies. LII. Sample size needed to meet performance requirement on proportion. http://lcfltd.com/AOAC/tr347-SAIS-LII-

sample-size-needed-for-PR-for-proportion.pdf

8. Maximum Time-to-Results

None.

9. Reference Materials 98 A defined set of authentic reference samples is used to construct the “authentic” profile. 99 Detailed protocols used to identify reference materials as authentic and to create adulterated 100 samples must be supplied. 101

Draft AOAC Standard Method Performance Requirements (SMPR) for Non-Targeted 1 Testing (NTT) of Ingredients for Food Authenticity/Fraud Evaluation of Honey, version 2; 2 December 27, 2019 5 AOAC SMPRs® describe the minimum recommended performance characteristics to be used 6 during the evaluation of a method. The evaluation may be an on-site verification, a single- 7 laboratory validation, or a multi-site collaborative study. SMPRs are written and adopted by 8 AOAC using the consensus of stakeholders representing the industry, government, and academic 9 and/or research institutions AOAC SMPRs are used by AOAC expert review panels in their 10 evaluation of validation study data for method being considered for Performance Tested 11 Methods SM or AOAC Official Methods of Analysis SM and can be used as acceptance criteria for 12 verification at user laboratories. 15 This document contains assessment parameters on the performance of Non-Targeted Testing 16 methods to monitor honey for the probable presence of Economically Motivated Adulterants 17 (EMA). 18 19 Intentionally designed to be generic, this SMPR was designed for Non-Targeted Testing (NTT) 20 methods developed to be applicable to the broadest range of potential methods using innovative 21 analytical platforms and chemometric approaches. Methods submitted based on this SMPR must 22 yield binary analytical results (i.e. “Authentic” or “Not Authentic”). 25 A non-targeted method to be used to evaluate foods and ingredients for possible EMAs. Any 26 method generating a baseline fingerprint of the authentic material and comparing test sample 27 fingerprints to assess differences will be considered. The final binary result identifies test 28 samples as either authentic or potentially adulterated. This method demonstrates reliability 29 using the requirements listed in this SMPR. 30 31 The scope of the NTT method will be defined by the authentic samples used in generating the 32 baseline fingerprint. 35 Applicability Statement – a general statement about the intended purpose and scope of the 36 method entailing key aspects of expected achievements for the specific situation and 37 circumstances. Key points to cover are the intended matrix, the purpose, and an indication of 38 sensitivity, specificity, and significance (USP Appendix XVIII). 39 40 Authentic Samples – Samples representative of the genuine commodity. Ideally these samples 41 should represent the food’s or ingredient’s variability seen naturally in the commodity. The 42 authentic samples used to generate the product baseline fingerprint will be used to properly 43 define the NTT method testing scope. 44 3 4 1. Purpose 13 14 2. Applicability 23 24 3. Analytical Technique 33 34 4. Definitions

Baseline Fingerprint – A food-specific model created by software evaluation of collected 45 analytical data. 46 47 Economically Motivated Adulteration – The fraudulent addition of non-authentic substances or 48 removal or replacement of authentic substances without the purchaser's knowledge for 49 economic gain of the seller (USP Appendix XVIII). 50 51 False Origin – Honeys containing mislabeled geographic and botanical sources. 52 53 Authentic Honey – The type(s) of honey used to generate the baseline fingerprint. The method’s 54 scope of authenticity is defined by the honey(s) used in generating the baseline fingerprint. 55 56 Single Laboratory Validation – Demonstration by one laboratory of method performance on the 57 validation samples described in Table 1. 58 59 Multilaboratory Validation – Demonstration between laboratories using adulterated samples 60 created by a third-party group and supplied blindly to the participating laboratories. 61 62 Sugars – The intentionally-added sugars to be included in a method’s evaluation include high 63 fructose corn syrup, sucrose, fructose, glucose, beet sugar, cane sugar, and invert sugar.

64 65 66 67 68

5. Method Performance Requirements

Table 1: Method Performance Requirements

Test

Adulterant

%Adulterant in Test Materials

Number of Samples to be Tested 1

Number of Test Results Qualified as Adulterated

Baseline

None (Authentic Honey)

0%

Establish Baseline Fingerprint 2

Validation using Authentic Samples 3

None

0%

30

0

Validation 4 Validation 4

5% 5%

30 30

30

Sugars

Molasses 30 1. Multiple samples from the same batch of adulterated material can be used for method evaluation. 69 2. Full details on protocol used to establish an authentic fingerprint must be supplied. 70 3. Method validation using authentic samples shall cover the entire scope used in creating the baseline fingerprint. 71 4. Method validation using adulterated samples shall cover the entire scope used in creating the baseline 72 fingerprint. 75 Suitable methods will include authentic and adulterated material check standards. 6. System Suitability Tests and/or Analytical Quality Control

73 74 76 77

78 79 80 81 82 83 84 85 86 87 88 89 90 91 92 93 94 95 96 97 98

7. Validation Guidance

a) Data demonstrating method performance is required.

b) Samples: Complete documentation for the collection and use of authentic samples is must be supplied by the method authors. The scope of authentic samples used to construct the “authentic” profile must be applicable to the defined scope of the NTT method. Expansion of the scope is possible with the inclusion of additional authentic samples into the baseline calibration, and validation using the protocol listed in this SMPR. c) For single lab validation studies, the method will be evaluated using prescribed adulterated materials as shown in Table 1. Methods approved at this level will proceed to a second level of evaluation where blinded samples containing unknown adulterants will

be sent to participating laboratories.

d) Methods submitted based on these SMPRs must yield binary analytical results (i.e.

“Authentic” or “Not Authentic”). e) Available guidance documents :

a. AOAC INTERNATIONAL Guidelines for Validation of Botanical Identification Methods,

Journal of AOAC International Vol. 95, No. 1, 2012

b. Statistical analysis of interlaboratory studies. LII. Sample size needed to meet performance requirement on proportion. http://lcfltd.com/AOAC/tr347-SAIS-LII-

sample-size-needed-for-PR-for-proportion.pdf

99 100

8. Maximum Time-to-Results

None

9. Reference Materials 101 A detailed description of the process used to obtain and evaluate authentic samples, and of the 102 test protocol establishing the baseline fingerprint must be supplied. 103

AOAC INTERNATIONAL Draft Standard Method Performance Requirements (SMPR®) for Non-Targeted Testing of Ingredients for the following Food Authenticity/Fraud Evaluation of Liquid Raw Bovine Milk, Honey and Extra Virgin Olive Oil (EVOO) Open for Public Comment Period January 15, 2020: AOAC INTERNATIONAL (AOAC) announces the availability of a draft standard method performance requirements (SMPR) for: Non-Targeted Testing of Ingredients for Food Authenticity/Fraud Evaluation of Liquid Raw Bovine Milk, Honey and Extra Virgin Olive Oil (EVOO). The draft SMPR represent the stakeholder panel deliberations. In accordance with AOAC standard developing procedures, the draft document must be posted for an open public comment period. Comment Process 1. For specific comments, please state the line number and/or range of line numbers in each document for which the comment applies. 2. Provide rationale as to why the editor should consider the comment. 3. Please specify if the comment is an editorial, content, or disagreement comment. a. Editorial comments provide additional clarification or correct typographical errors. Please suggest alternative wording or typographical corrections. b. Content-related comments provide technical clarity and comprehensiveness. Please suggest the appropriate technical language. Documents will be reviewed by AOAC for technical accuracy and clarity. c. Disagreement comments reflect a perspective on content documented/undocumented in the drafts. Please provide language that document the perspective or position. 4. All comments are due Friday, January 24, 2020 . The AOAC editorial team will address all questions and reserves the right to not to accept comments received after the deadline. AOAC requests that the following guidelines be observed in providing comments:

1. Click here to view the Draft Standard Method Performance Requirements (SMPR) for Liquid Raw Bovine Milk. 2. Click here to view the Draft Standard Method Performance Requirements (SMPR) for Honey. 3. Click here to view the Draft Standard Method Performance Requirements (SMPR) for Extra Virgin Olive Oil.

To provide comments to the draft Standard Method Performance Requirements (SMPR):

Click to provide comments on the draft StandardMethod Performance Requirements for Food Authenticity/Fraud Non-Targeted Testing Ingredients for Liquid Raw Bovine Milk, Honey and Extra Virgin Olive Oil (EVOO) or copy & paste link in browser: https://form.jotform.com/200128072523140

For technical information on how to provide comments, contact Delia Boyd , Senior Manager at dboyd@aoac.org or via telephone: 301-924-7077 ext. 126.