SPSFAM EXPERT REVIEW PANEL

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METHODS FOR THE DETERMINATION OF BISPHENOL-A (BPA) IN BEVERAGES

ERP CHAIR: MELISSA PHILLIPS NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY & AOAC OFFICIAL METHODS BOARD

SEPTEMBER 26, 2017 | 1:00PM – 5:00PM ET ATLANTA MARRIOTT MARQUIS MEETING ROOM: M106

Atlanta Marriott Marquis 265 Peachtree Center Ave NE Atlanta, GA 30303

AOAC Stakeholder Panel on Strategic Food Analytical Methods Bisphenol A (BPA) Expert Review Panel

Tuesday, September 26, 2017, 1 :00 p.m. – 5:00 p.m. Atlanta Marriott Marquis, Room M106

A G E N D A

1. Welcome and Introductions

Melissa Phillips, NIST (ERP Chair)

2. Review of AOAC Volunteer Policies & ERP Proccess Overview and Guidelines Deborah McKenzie, AOAC INTERNATIONAL

3. Review of Methods For each method, the assigned ERP members will present a review of the revised method manuscripts, after which the ERP will discuss the method and render a decision on the status for each method.

A. BPA-01

a. Ackerman Review b. Cao Review c. Discussion and Vote

B. BPA-02

a. Gumustas Review b. Tang Review c. Discussion and Vote

C. BPA-03

a. Phillips Review b. Seipelt Review c. Discussion and Vote

D. BPA-04

a. Somayajula Review b. Yadlapalli Review c. Discussion and Vote

4. Final Action Requirements for Approved Method(s) 5. Adjourn

SPSFAM BPA ERP 09/15/2017 – v1.0

AOAC SPSFAM BISPHENOL-A EXPERT REVIEW PANEL

METHODS AND SMPR ACCESS

• AOAC SMPR 2017.XXX • METHODACCESS [ERP ONLY - PASSWORD REQUIRED]

AOAC Candidate Method #BPA-01 Bisphenol-A in Water Author(s): N. Reinhound Submitted by: Nico Reinhound, Antec Scientific Method applicability: HPLC with Electrochemical Detection Attachments: 0

Submitter notes:

The attractivity of the method is ease of operation and the sample preparation that improves the detection limit considerably. We can provide additional data, or do additional measurements in case you decide in favor of a method based on electrochemical detection.

Primary reviewer: Luke Ackerman, US FDA/CFSAN Secondary Reviewer: Xu-Liang Cao, Health Canada

AOAC SPSFAM ERP REVIEW: MAIN FORM

Submission Date

2017-09-15 11:19:49

Name

Luke Ackerman

E-mail

Luke.Ackerman@fda.hhs.gov

Organization

FDA

Title of Method

BPA in Water

AOAC Candidate Method Number (e.g. ALN-01)

BPA-01

Applicable SMPR

BPA

I. Summary of the Method

Online SPE - HPLC-ECD to quantify BPA in water. 1mL injection. 5x1mmx5um C18 SPE with 10% ACN wash (50mM Acetate ph 4.8), isocratic elution with 40% ACN (50mM Acetate ph 4.8) on 150x2.1mmx3um c18 column. ECD detection on 2mm glassy carbon electrode at t~5.2 min. External calibration? Method apparently applies to online SPE/LC ready water samples. It is missing any application to beverages other than water and any beverage with particles, emulsions, high TOC/SSC.

II. Review of the Method Only 1. Does the applicability of the method support the applicability of the SMPR? If not, please explain what is missing. 2. Does the analytical technique(s) used in the method meet the SMPR? If not, please specify how it differs from what is stated in the SMPR. 3. Are the definitions specified in the SMPR used and applied appropriately in the method? If no, please indicate how the terms are used. 4. Does the method, as written, contain all appropriate precautions and warnings related to the method's reagents, components, instrumentation, or method steps that may be hazardous? If no, please suggest wording or option(s).

The general technique might be able to meet the SMPR but the submitted method does not provide any data or examples of its ability to meet the accuracy and precision requirements, either across the quantitative range, or in beverage samples. It is highly unclear in its sensitivity determination. It did not address blanks, performance across beverage matrices, and it did not follow SMPR procedures for sensitivity/quantitative limit determination. No. LOD as defined in SMPR is not used and the method does not specify how the reported LOD was determined. LOQ is never mentioned. Accuracy is never assessed or discussed.

No. No mention is made regarding safe handling of organic solvents, neat chemicals, PPE such as eye goggles, gloves, lab coats, closed toe shoes, or hazards of instrumentation (shock or mechanical). Realistically this method probably has minimal hazards relative to some other methods, but standard warnings (especially about preparation of mobile phases and standards) should be included.

III. Review of Supporting Information 1. Are the definitions specified in the SMPR used and applied appropriately in the supporting documentation (manuscripts, method studies, etc...)? If not, please explain the differences and if the method is impacted by the difference. 2. Is there information demonstrating that the method meets the SMPR Method Performance Requirements using the Reference Materials stated in the SMPR? If not, then specify what is missing and how this impacts demonstration of performance of the method. method performs within the SMPR Method Performance REquirements table specifications for all analytes in the SMPR applicability statement? If not, please specify what is missing and whether or not the method's applicability should be modified. IV. General Submission Package 1. Based on the supporting information, were there any additional steps in the evaluation of the method that indicated the need for any additional precautionary statements in the method? 2. Does the method contain system suitability tests or controls as specified by the SMPR? If not, please indicate if there is a need for such tests or controls and which ones. 3. Is there information demonstrating that the

No supporting info attached.

No. method does not provide any data or examples of its ability to meet the accuracy and precision requirements (% recovery, %RSDr or %RSDR), either across the quantitative range, or in beverage samples. It is highly unclear in its sensitivity determination (reported LOD). It did not address blanks, performance across beverage matrices, and it did not follow SMPR procedures for sensitivity/quantitative limit determination. LOD as defined in SMPR is not used and the method does not specify how the reported LOD was determined. LOQ is never mentioned. Accuracy is never assessed or discussed. Details on preparation of a reference material (BPA calibration curves, spiked water) are totally absent. Based on missing all but 1 piece of method performance measures it is impossible to determine if this method is capable of meeting method performance requirements. No. As stated previously, there is only 1 method performance requirement reported (LOD) and it is not clear if SMPR guidelines were followed (3*SD of n=10 blanks). There are some repeatability %RSDs reported, but they are instrumental response variances not sample quantitation variances, they do not span the quantitation range. No (accuracy) recoveries were stated or shown. No LOQ calculated or reported. No reproducibilties (RSD-R) assessed or reported, and nothing done in any of the drink matrices required from Table 3.

No the method contains no specified system suitability tests or controls. The SMPR requires negative controls (blanks) and low and mid-point positive controls. This method contained none of those.

3. Is there information demonstrating that the method system suitability tests and controls as specified in the SMPR worked appropriately and as expected? If no, please specify. 4. Based on the supporting information, is the method written clearly and concisely? If no, please specify the needed revisions. 5. Based on the supporting information, what are the pros/strengths of the method? 6. Based on the supporting information, what are the cons/weaknesses of the method?

No. None were conducted.

It is concise. Overly concise. Much more detail is needed about nearly every aspect of the method. Especially on calibrant, mobile phase, and control (blank and positive control) preparation, as well as data handling and quantification.

It might be sensitive and reproducible enough for packaged water.

It is totally unclear if the method works reliably and whether it works in any other beverage besides water and whether it really is sensitive enough or reproducible enough, especially across the concentration range and sample types.

7. Any general comments about the method?

The method submitted is an application note that wasnt even adapted to meet SMPR requirements. Only the absolute simplest application within the SMPR was attempted (only water, only repeatability, only on standards, no accuracy, no real LOD) and as such to the extent the few method performance numbers do fall within SMPR ranges they are VERY unlikely to remain within ranges if this method was evaluated more thoroughly, correctly, and across the concentration/sample ranges specified in the SMPR.

V. Final Recommendation Do you recommend this method be adopted as a First Action and published in the Official Methods of Analysis of AOAC INTERNATIONAL? Please specify rationale.

No. There is no demonstration of the method being capable of meeting SMPR requirements.

AOAC SPSFAM ERP REVIEW: MAIN FORM

Submission Date

2017-08-31 08:54:01

Name

Xu-Liang Cao

E-mail

xu-liang.cao@hc-sc.gc.ca

Organization

Health Canada

Title of Method

Bisphenol A in water

AOAC Candidate Method Number (e.g. ALN-01)

BPA-01

Applicable SMPR

BPA

Summary:

This HPLC with electrochemical detection method was submitted by Nico Reinhound from Antec Scientific. It is based on an ALEXYS system in combination with a solid phase sample pre-concentration step. A 1 mL loop is filled with sample, which was carried onto the pre-column by a solvent. The concentrated sample from the pre- column was flushed onto the analytical column by another solvent for separation, and the analyte was detected by an electrochemical cell with an electrode at optimum potential of 900 mV. Detection limit is 0.5 nmol/L, or 114 ng/L (0.114 ug/L). The submitted method only demonstrated its application to the analysis of BPA in drinking water, while its applicability to the other beverage products specified in SMPR is unknown due to the missing information on method performance parameters. It is not clear how the detection limit of the submitted method was estimated, and it is unlikely it was estimated according to the procedures specified in the SMPR. It is also not clear whether the claimed detection limit (0.5 nmol/L as stated in the summary or 0.3 nmol/L stated in the text) is LOD or LOQ. The claimed detection limit of 0.3 nmol/L (or 0.0684 ug/L) meets the requirements for both LOD and LOQ specified in SMPR. Repeatability meets the SMPR, but it was demonstrated using the standard solutions instead of real samples.

1. Does the applicability of the method support the applicability of the SMPR? If not, please explain what is missing. 2. Does the analytical technique(s) used in the method meet the SMPR? If not, please specify how it differs from what is stated in the SMPR. 3. Are the definitions specified in the SMPR used and applied appropriately in the method? If no, please indicate how the terms are used. 4. Does the method, as written, contain all appropriate precautions and warnings related to the method's reagents, components, instrumentation, or method steps that may be hazardous? If no, please suggest wording or option(s).

The detection limit of the submitted method may have not been estimated according to the definition specified in the SMPR.

No. The author could refer to some available documents on laboratory safety, such as the AOAC official method of analysis.

1. Are the definitions specified in the SMPR used and applied appropriately in the supporting documentation (manuscripts, method studies, etc...)? If not, please explain the differences and if the method is impacted by the difference. 2. Is there information demonstrating that the method meets the SMPR Method Performance Requirements using the Reference Materials stated in the SMPR? If not, then specify what is missing and how this impacts demonstration of performance of the method. method performs within the SMPR Method Performance REquirements table specifications for all analytes in the SMPR applicability statement? If not, please specify what is missing and whether or not the method's applicability should be modified. 1. Based on the supporting information, were there any additional steps in the evaluation of the method that indicated the need for any additional precautionary statements in the method? 2. Does the method contain system suitability tests or controls as specified by the SMPR? If not, please indicate if there is a need for such tests or controls and which ones. 3. Is there information demonstrating that the method system suitability tests and controls as specified in the SMPR worked appropriately and as expected? If no, please specify. 3. Is there information demonstrating that the

Detection limit may have not been estimated according to the definitions specified in the SMPR. Repeatability was demonstrated using standard solutions (<= 2.5 nmol/L) only instead of real samples spiked with standards.

Other than the standard solutions, there are no additional reference materials used in the method.

The method was demonstrated to perform within the SMPR specifications in terms of detection limit and repeatability only for drinking water, but not for the other beverage products specified in the SMPR.

The detection limit should be estimated according to the definitions specified in the SMPR. Repeatability should also be evaluated using real samples for the analytical ranges specified in the SMPR.

No. Background contamination is very common for BPA analysis, and method blanks should always be included during analysis.

Not available.

4. Based on the supporting information, is the method written clearly and concisely? If no, please specify the needed revisions. 5. Based on the supporting information, what are the pros/strengths of the method? 6. Based on the supporting information, what are the cons/weaknesses of the method?

The method is written clearly, but could be improved by revising it in a format similar to the candidate method BPA-04.

The method demonstrated good sensitivity for BPA analysis, with a detection limit of 0.3 nmol/L for 1 mL of water sample.

Contamination of electrode is an issue at elevated concentrations of BPA, responses decrease by 50% after 100 injections. The method is not linear at levels below 0.5 nmol/L. The method was not demonstrated for its application to beverage products specified in the SMPR other than water.

7. Any general comments about the method?

This method needs specific instrumentation, the ALEXYS BPA analyzer, and thus could be a major limiting factor for its wide applications among laboratories.

MS-based methods are essential to avoid or minimize false positive results due to interferences from challenging samples such as foods. Since more laboratories now have the access to LC or GC based MS instrumentation, this non-MS based method will certainly face challenges for its applications.

Do you recommend this method be adopted as a First Action and published in the Official Methods of Analysis of AOAC INTERNATIONAL? Please specify rationale.

I would not recommend this method be adopted as a First Action and published in the Official Methods of Analysis of AOAC INTERNATIONAL based on the following:

1. The method was demonstrated only for its application to drinking water; 2. Detection limit may have not been estimated according to definitions specified in the SMPR; 3. Repeatability was demonstrated using standard solutions only, not real samples;

4. Most laboratories may not have this specific instrumentation; 5. This is a non-MS based method, potential for false positives.

AOAC Candidate Method #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.

Author(s): J. Liu, Z. Wu, H. Zhang, C. Xi, X. Wang, L. Chen, D. Toth

Submitted by: Darney Toth, Vicam

Method applicability: Determination of BPA regular carbonated soft drink with sugar and caffeine, 100% orange juice with pulp, and whole milk

Attachments: 0

Primary Reviewer: Mehmet Gumustas, Hitit University, Turkey Secondary Reviewer: Jing Tan, Abbott Nutrition

AOAC SPSFAM ERP REVIEW: MAIN FORM

Submission Date

2017-09-16 22:05:30

Name

Mehmet Gumustas

E-mail

mgumustas@hotmail.com

Organization

Ankara University

Title of Method

Determination of free Bisphenol A in commercially packaged ready to consume carbonated/non-carbonated water and beverages by ımmunoaffinity purification and HPLC fluorescent detection

AOAC Candidate Method Number (e.g. ALN-01)

#BPA-02

Applicable SMPR

Bisphenol-A (BPA)

I. Summary of the Method

This is a immunoaffinity purification following HPLC with FL detection method for the determination of free Bisphenol A in commercially packaged carbonated and non carbonated water, as well as non-alcoholic beverages. The method protocol calls for following different sample preparation techniques for carbonated and non carbonated water and other type of samples. After the preparation of samples the analysis has been done by using HPLC with FL detector. From the view point of HPLC system suitability test results were not mentioned. Also the stress degradation studies needs to be added for demonstrating the specificity of the developed method.

Applicability of the developed method support the SMPR

The chosen analytical technique (HPLC-FL) meet the SMPR

All mentioned definitions specified in the SMP used and applied appropriately

4. Does the method, as written, contain all appropriate precautions and warnings related to the method's reagents, components, instrumentation, or method steps that may be hazardous? If no, please suggest wording or option(s). III. Review of Supporting Information 1. Are the definitions specified in the SMPR used and applied appropriately in the supporting documentation (manuscripts, method studies, etc...)? If not, please explain the differences and if the method is impacted by the difference. 2. Is there information demonstrating that the method meets the SMPR Method Performance Requirements using the Reference Materials stated in the SMPR? If not, then specify what is missing and how this impacts demonstration of performance of the method. method performs within the SMPR Method Performance REquirements table specifications for all analytes in the SMPR applicability statement? If not, please specify what is missing and whether or not the method's applicability should be modified. IV. General Submission Package 1. Based on the supporting information, were there any additional steps in the evaluation of the method that indicated the need for any additional precautionary statements in the method? 3. Is there information demonstrating that the

The authors given the reagents, instrumentation etc. But they may mentioned the safety about the ragents such as BPA itself, methanol.

There is not any supporting documentation in this method

Performance requirements meet the SMPR

Carbonated soft drink, 100% orange juice, whole milk analyzed by the method developers. They also demonstrated related tables in their study.

In general there is no need for any additional precautionary statements in this method. However the method developers given the sample preparation step protocols in a clear way to obtain concentrated samples.

2. Does the method contain system suitability tests or controls as specified by the SMPR? If not, please indicate if there is a need for such tests or controls and which ones. 3. Is there information demonstrating that the method system suitability tests and controls as specified in the SMPR worked appropriately and as expected? If no, please specify. 4. Based on the supporting information, is the method written clearly and concisely? If no, please specify the needed revisions. 5. Based on the supporting information, what are the pros/strengths of the method?

The missing point for this method is system suitability test parameters results. The authors should be demonstrate the suitability of the developed HPLC-FL method.

They may be support their results with data

The methods written well, step by step, clearly and concisely. The developers of the method can be used molarity instead of normality while they indicated the concentration of the solutions.

The strengths of the method following: * The HPLC system with FL detection can be found in many analytical laboratories, * Immunoaffinity purification concentrate the samples for better accuracy * Apart from the immunoaffinity columns, the reagents and chemicals can be found easily *The specificity of the method is good enough The weakness of the methods: *Immunoaffinity purification suffers time when the rapidness is essential * The degradation products or possible impurities should be mentioned and the developers could demonstrated the specificity of their method. *Recovery of the method decreased whenever the spiked amount of BPA was increased (May be the immunoaffinity column need to be rechecked and reoptimized) *Some statements like "the type of sample preparation may be used in other type of drinks" not clear. These parts may need to be clarified.

6. Based on the supporting information, what are the cons/weaknesses of the method?

7. Any general comments about the method?

In general the other type of samples like tea, coffee, energy drinks, etc. may be applied and included.

V. Final Recommendation Do you recommend this method be adopted as a First Action and published in the Official Methods of Analysis of AOAC INTERNATIONAL? Please specify rationale.

The method seems easy to operate instead of sample preparation part. However sample preconcentration may be important in some cases and somehow it will be worth to be used. After some revisions this method can be adopted and published.

AOAC SPSFAM ERP REVIEW: MAIN FORM

Submission Date

2017-09-15 11:19:49

Name

Luke Ackerman

E-mail

Luke.Ackerman@fda.hhs.gov

Organization

FDA

Title of Method

BPA in Water

AOAC Candidate Method Number (e.g. ALN-01)

BPA-01

Applicable SMPR

BPA

I. Summary of the Method

No supporting info attached.

No the method contains no specified system suitability tests or controls. The SMPR requires negative controls (blanks) and low and mid-point positive controls. This method contained none of those.

No. None were conducted.

It might be sensitive and reproducible enough for packaged water.

7. Any general comments about the method?

V. Final Recommendation Do you recommend this method be adopted as a First Action and published in the Official Methods of Analysis of AOAC INTERNATIONAL? Please specify rationale.

No. There is no demonstration of the method being capable of meeting SMPR requirements.

AOAC SPSFAM ERP REVIEW: MAIN FORM

Submission Date

2017-09-08 06:18:48

Name

Sudhakar yadlapalli

E-mail

sudhakar@firstsourcels.com

Organization

First source labotatory solutions LLP

Title of Method

Determination of free Bisphenol A(BPA) in commecially packaged ready to consume carbonated water and non alcoholic beverages by using LCMSMS.

AOAC Candidate Method Number (e.g. ALN-01)

BPA-04

Applicable SMPR

Bisphenol-A (BPA)

I. Summary of the Method

Determination of Bisphenol A(BPA) in commercially packaged ready to consume carbonated and Non carbonated water and Non- Alcoholic Beverages using LCMS/MS.

YES

Not required however if provides Raw data (chromatograms ) that may give better clarity for Interpretation of data/ evaluation of the method .

YES

1.Sample preparation is simple and cost effective. 2.. Method Specificity well established as per EC decision 2002/657/EC. 3. To achieve high recoveries developer used labelled internal standards .

Method is most accurate and confirmatory.

Method clearly covered and stated all the parameters mentioned in AOAC BPA SMPR .

6. Based on the supporting information, what are the cons/weaknesses of the method?

May be require to perform recovery at 2 to 5 ug/L to cover entire analytical ranges as mentioned in BPA SMPR.

7. Any general comments about the method?

V. Final Recommendation Do you recommend this method be adopted as a First Action and published in the Official Methods of Analysis of AOAC INTERNATIONAL? Please specify rationale.

YES

AOAC SPDS ERP REVIEW: MAIN FORM

Submission Date

2017-09-14 22:42:09

Name

Jing Tan

E-mail

jtan@abbott.com

Organization

Abbott Nutrition R&D

Title of Method

Immunoaffinity purification and HPLC fluorescent detection

AOAC Candidate Method Number (e.g. ALN-01)

BPA-02

Applicable SMPR

BPA_SMPR_V6

Summary:

In this method, immunoaffinity column (IAC) was used for sample cleanup and concentrating, and BPA was determined by HPLC-FLD. It is of high specificity. The method is relatively easy to implement in term of sample preparation and instrument operation and maintenance. Authors have demonstrated most of the method performance according to the definitions in SMPR. But additional information is needed on system suitability and analytical quality control.

Yes

There is no precaution or warnings written in the method.

Not applicable.

Authors did not provide information on 5) system suitability and or analytical control, i.e. the blank checks and check standards. BPA is known to ubiquitous in the environment. It is very important to demonstrate the minimal cross-contamination during the sample preparation and analysis.

I would request information on blank samples, e.g. chromatograms and concentrations found.

Authors provided information on LOD/LOQ, the sample spikes to demonstrate accuracy, and repeatability, but authors need to supplement the data on system suitability and quality control.

No. no information on sample blanks, control samples, or check standards.

Yes. The method protocol is clearly written.

• IAC is of high specificity, which can significantly reduce interference in chromatography system and the chance of false-identification. • HPLC-FLD is relatively affordable and easy to operate. • The method could be easily adopted by various laboratories.

• IAC column is relatively costly. It also seems very delicate and susceptible to extreme conditions i.e. low pH and high content of organic solvent. Thus additional steps are required for sample preparation (e.g. adjusting the pH, reducing the portion of methanol in sample solution, filtration of sample), which increases the complexity of method and could introduce more errors. • In order to meet the LOD/LOQ requirement, sample concentrating step was performed for juice matrix. The blow-drying and the reconstitution are time-consuming. • Authors did not indicate the unit of LOD and LOQ in table 1, but presumably it is in ppb? • Accuracy was evaluated by spiking the samples. However, authors did not provide information on sample blank. I would like to know whether recovery was calculated by sample spike subtracting sample blank. • I would recommend to replace the filtration step in juice preparation to centrifugation. Methanol may evaporate during the filtration, and causes inaccuracy in volume measurement.

7. Any general comments about the method?

Do you recommend this method be adopted as a First Action and published in the Official Methods of Analysis of AOAC INTERNATIONAL? Please specify rationale.

I would recommended to make decision after reviewing the data on system suitability and analytical qualify control which authors failed to provide.

AOAC Candidate Method #BPA-03 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

Method applicability: Example for cola drink but valid for other drinks. Some article references with relevant drinks for this call are also cited.

Attachments: 0

Primary Reviewer: Melissa Phillips, NIST Secondary Reviewer: Tom Seipelt, Abbott Nutrition

AOAC SPDS ERP REVIEW: MAIN FORM

Submission Date

2017-09-18 07:25:34

Name

Melissa Phillips

E-mail

melissa.phillips@nist.gov

Organization

NIST

Title of Method

Use of AFFINIMIP SPE Bisphenols as clean up method for the determination of Bisphenol A from COLA drinks by Fluorescence detection

AOAC Candidate Method Number (e.g. ALN-01)

BPA-03

Applicable SMPR

Bisphenol A (v7)

Summary:

BPA is isolated from samples using AFFINIMIP SPE Bisphenols cartridge. Cleaned up samples are analyzed by LC with fluorescence detection.

1. Does the applicability of the method support the applicability of the SMPR? If not, please explain what is missing.

The method describes briefly a method for determination of BPA in "cola drinks" (unclear if regular or diet, assuming regular) and also infant formula. The following matrices from Table 3 of the SMPR are not addressed: carbonated soft drinks, diet 100% juices (with and without pulp) teas

dairy-based coffee drinks sports drinks (for hydration) energy drinks grain-based beverages meal replacement beverages

An addendum is included that describes application to numerous other foods and beverages but none in this list. The authors also provide a reference to other published methods that may include more matrices.

2. Does the analytical technique(s) used in the method meet the SMPR? If not, please specify how it differs from what is stated in the SMPR. 3. Are the definitions specified in the SMPR used and applied appropriately in the method? If no, please indicate how the terms are used. 4. Does the method, as written, contain all appropriate precautions and warnings related to the method's reagents, components, instrumentation, or method steps that may be hazardous? If no, please suggest wording or option(s).

Yes

No safety information is provided. The only potential hazard would be working with flammable solvents and weak acids.

Yes

No commercial reference materials are identified in the SMPR, and no reference material (commercial or in-house prepared) was used in the method.

For the 2 matrices and 3 concentrations tested, yes.

cola at 5 ug/L; 90.8% recovery, 1.0% RSDr formula at 1 ug/L; 88.4% recovery, 1.5% RSDr formula at 2 ug/L; 85.7% recovery, 2.7% RSDr

formula at 1 ug/L; 84.4% recovery, 7.4% RSDR formula at 2 ug/L; 85.8% recovery, 5.3% RSDR

No LOD, LOQ, or analytical range is given. LOQ is reported as 0.5 ug/L based on a similar method reported in the literature using canned energy drinks.

Additional matrices should be tested, and higher concentrations should be tested. I have concerns about the loading capacity of the SPE cartridges, and would like to see explicit instructions about sample dilution if necessary.

No information provided about calibration at all. This should be included as well.

Some blank samples were included. No check standards were tested.

Blank samples appear to be blank. I would like to see calibration information as well as recovery of a BPA solution from the SPE cartridge. Some of the chromatograms are very busy - I would like to see criteria around the identification of the BPA peak as well.

Much more information is needed. The method is very bare bones. Information about solution preparation and calibration is the most glaring omission.

Straightforward, and appears to work for spikes in cola and infant formula.

No LOD, LOQ, or analytical range data. No samples tested in the high range (5-20 ug/L). This concerns me from a standpoint of SPE cartridge overload - specific instructions are needed related to cartridge capacity for BPA and whether samples should be diluted. How would one know if an unknown sample (with an unknown amount of BPA) has overloaded the cartridge?

I would also like to see data in more of the matrices.

7. Any general comments about the method?

This method has potential, but more work is needed before the SMPR is met.

Do you recommend this method be adopted as a First Action and published in the Official Methods of Analysis of AOAC INTERNATIONAL? Please specify rationale.

Not at this time.

I would recommend that the authors provide the following information and resubmit:

1. Information about calibration and analytical range 2. Information about LOD and LOQ 3. Testing of samples at higher concentrations (5-20 ug/L) 4. Testing of additional matrices in Table 3 5. submit procedures used for background assessment and control, and frequency of analysis of method blanks

AOAC SPDS ERP REVIEW: MAIN FORM

Submission Date

2017-09-15 21:45:37

Name

Tom Seipelt

E-mail

tom.seipelt@abbott.com

Organization

Abbott Nutrition

Title of Method

Method for the determination of Bisphenol A in drinks by Fluorescence detection

AOAC Candidate Method Number (e.g. ALN-01)

BPA-03

Applicable SMPR

Bisphenol A (BPA)

Summary:

The method is applicable to the determination of bisphenol A (BPA) from soft drinks, foods, and other beverages with extraction and clean-up using SPE followed by HPLC with fluorescence detection. The specificity of the extraction is realized using a molecularly imprinted polymer which is selective for BPA and related compounds. Sensitivity from canned energy drinks is reported with an LOQ of 0.5 ug/L.

No. Data are shown for canned soft drinks, energy drinks, etc. but all requirements are not addressed for any single matrix type.

The data presented do not support meeting all aspects of the SMPR. For example, adequate LOQ is claimed for canned energy drinks, but the accuracy and precision do not meet SMPR for this matrix.

This is not clear. Method performance was stated "under conditions of RSDr", but the conditions of the experiment are not stated.

No, the method as presented does not contain a safety section that would address appropriate handling of acids or organic solvents. A safety section must be added to indicate the use of appropriate personal protective equipment like gloves and safety glasses.

The manuscript states that RSDr was estimated based on analysis of multiple samples (n=3) on 2 different days (total n=6). This

Yes. Spike recovery data are provided, for canned energy drinks in the attached publication. Within day (n=3) and day to day (n=6) data are used to demonstrate accuracy and precision in the absence of a reference material.

Yes. Method meets the requirements for one of the matrices listed in the SMPR. Data for other matrices would be needed to demonstrate broad applicability to other beverages listed.

Specificity of the method is reliant on the clean up using SPE with molecularly imprinted polymers. Data presented demonstrate binding of other bisphenol A related compounds (e.g., BPB, BPF, BADGE, and BFDGE). Specificity in other matrices should be demonstrated to minimize potential for false positive results.

Supporting document describes procedure blanks and glass washing procedures to monitor background contamination. Final method should include these steps as requirements.

Yes. Background contamination was not reported based on the controls used.

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