PONE-D-20-40901

Application of micro-nanostructured magnetite in separating tetrabromobisphenol A and hexabromocyclododecane from environmental water by magnetic solid phase extraction

PLOS ONE

Dear Dr. yu,

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9- What are the reasons behind choosing these spiking levels (5, 10, 20)? Justification is needed. What are the MRL (maximum permissible level) of the tested analytes? This should be added and discussed in the text in relation to the sensitivity of the developed method

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A. M. Abd El-Aty

Academic Editor

PLOS ONE

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Reviewers' comments:

Reviewer's Responses to Questions

Comments to the Author

1. Is the manuscript technically sound, and do the data support the conclusions?

The manuscript must describe a technically sound piece of scientific research with data that supports the conclusions. Experiments must have been conducted rigorously, with appropriate controls, replication, and sample sizes. The conclusions must be drawn appropriately based on the data presented.

Reviewer #1: Yes

Reviewer #2: Yes

Reviewer #3: Partly

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2. Has the statistical analysis been performed appropriately and rigorously?

Reviewer #1: Yes

Reviewer #2: Yes

Reviewer #3: N/A

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3. Have the authors made all data underlying the findings in their manuscript fully available?

The PLOS Data policy requires authors to make all data underlying the findings described in their manuscript fully available without restriction, with rare exception (please refer to the Data Availability Statement in the manuscript PDF file). The data should be provided as part of the manuscript or its supporting information, or deposited to a public repository. For example, in addition to summary statistics, the data points behind means, medians and variance measures should be available. If there are restrictions on publicly sharing data—e.g. participant privacy or use of data from a third party—those must be specified.

Reviewer #1: Yes

Reviewer #2: Yes

Reviewer #3: Yes

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4. Is the manuscript presented in an intelligible fashion and written in standard English?

PLOS ONE does not copyedit accepted manuscripts, so the language in submitted articles must be clear, correct, and unambiguous. Any typographical or grammatical errors should be corrected at revision, so please note any specific errors here.

Reviewer #1: Yes

Reviewer #2: Yes

Reviewer #3: Yes

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5. Review Comments to the Author

Please use the space provided to explain your answers to the questions above. You may also include additional comments for the author, including concerns about dual publication, research ethics, or publication ethics. (Please upload your review as an attachment if it exceeds 20,000 characters)

Reviewer #1: The paper "Application of micro-nanostructured magnetite in separating tetrabromobisphenol A and hexabromocyclododecane from environmental water by magnetic solid phase extraction" is a good paper.

All analytical figure of merit were reported and the whole project is clearly presented.

The new material is completely characterized.

The major point that require a deep revision is the validation procedure.

The Authors must follow the international guidelines in order to fully validate precision, trueness, LOD and LOQ.

These values must be validated considering the back-calculated concentrations and not merely the S/N ratios.

I suggest major revisions even if the paper merit the acceptance (but after these mandatory revisions)

Reviewer #2: In this study micro-nanostructured magnetite particles (MNMPs) were successfully synthesized with surface modification by citric acid molecules. Then the synthesized composites served as an adsorbent for the extraction of TBBPA and HBCD from environmental water samples followed by gas chromatography-mass spectrometry (GC-MS) analysis. The results indicated that MNMPs magnetic solid phase extraction (MSPE) method had advantages of simplicity, good sensitivity and high efficiency for the extraction of the two BFRs from environmental water. The manuscript is suitable for PLoS One.

Minor comments:

1. The established method only covers two BFRs, what about the applicability for the other BFRs?

2. Can this method be used for urine or blood samples in the future?

3. What is the meaning of “Environmental water”? River, lake or sea water? What about drinking water or tap water?

Reviewer #3: * Authors should check all significant digits throughout manuscript

* Effect of pH should be explained with pKa values of molecules in medium

* Is there any explanation from authors about desorption volume? Because, it is so high.(6 mL) for GC-MS analysis.

* How was LOD and LOQ values calculated? Which protocol was followed?

* All sections of figure 4 needs more comments? Why, How?

* In table 2, Recovery and RSD values should be corrected such as 102.9 instead of 102.886.

* These references may be added to introduction.

https://doi.org/10.1080/01496395.2019.1623254

https://doi.org/10.1016/j.microc.2018.11.056

https://doi.org/10.3390/molecules24244621

https://doi.org/10.1039/C9AY01504C

https://doi.org/10.1016/j.jchromb.2018.03.030

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Reviewer #1: No

Reviewer #2: No

Reviewer #3: No

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Application of micro-nanostructured magnetite in separating tetrabromobisphenol A and hexabromocyclododecane from environmental water by magnetic solid phase extraction

PONE-D-20-40901R1

Dear Dr. yu,

We’re pleased to inform you that your manuscript has been judged scientifically suitable for publication and will be formally accepted for publication once it meets all outstanding technical requirements.

Within one week, you’ll receive an e-mail detailing the required amendments. When these have been addressed, you’ll receive a formal acceptance letter and your manuscript will be scheduled for publication.

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Kind regards,

A. M. Abd El-Aty

Academic Editor

PLOS ONE

Additional Editor Comments (optional):

Reviewers' comments:

Reviewer's Responses to Questions

Comments to the Author

1. If the authors have adequately addressed your comments raised in a previous round of review and you feel that this manuscript is now acceptable for publication, you may indicate that here to bypass the “Comments to the Author” section, enter your conflict of interest statement in the “Confidential to Editor” section, and submit your "Accept" recommendation.

Reviewer #1: All comments have been addressed

Reviewer #2: All comments have been addressed

Reviewer #3: All comments have been addressed

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2. Is the manuscript technically sound, and do the data support the conclusions?

The manuscript must describe a technically sound piece of scientific research with data that supports the conclusions. Experiments must have been conducted rigorously, with appropriate controls, replication, and sample sizes. The conclusions must be drawn appropriately based on the data presented.

Reviewer #1: Yes

Reviewer #2: Yes

Reviewer #3: Yes

**********

3. Has the statistical analysis been performed appropriately and rigorously?

Reviewer #1: Yes

Reviewer #2: Yes

Reviewer #3: Yes

**********

4. Have the authors made all data underlying the findings in their manuscript fully available?

The PLOS Data policy requires authors to make all data underlying the findings described in their manuscript fully available without restriction, with rare exception (please refer to the Data Availability Statement in the manuscript PDF file). The data should be provided as part of the manuscript or its supporting information, or deposited to a public repository. For example, in addition to summary statistics, the data points behind means, medians and variance measures should be available. If there are restrictions on publicly sharing data—e.g. participant privacy or use of data from a third party—those must be specified.

Reviewer #1: Yes

Reviewer #2: Yes

Reviewer #3: Yes

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5. Is the manuscript presented in an intelligible fashion and written in standard English?

PLOS ONE does not copyedit accepted manuscripts, so the language in submitted articles must be clear, correct, and unambiguous. Any typographical or grammatical errors should be corrected at revision, so please note any specific errors here.

Reviewer #1: Yes

Reviewer #2: Yes

Reviewer #3: Yes

**********

6. Review Comments to the Author

Please use the space provided to explain your answers to the questions above. You may also include additional comments for the author, including concerns about dual publication, research ethics, or publication ethics. (Please upload your review as an attachment if it exceeds 20,000 characters)

Reviewer #1: All requested reviwions were reported in the current paper that, now, can be accepted for publication

Reviewer #2: (No Response)

Reviewer #3: (No Response)

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7. PLOS authors have the option to publish the peer review history of their article (what does this mean?). If published, this will include your full peer review and any attached files.

If you choose “no”, your identity will remain anonymous but your review may still be made public.

Do you want your identity to be public for this peer review? For information about this choice, including consent withdrawal, please see our Privacy Policy.

Reviewer #1: No

Reviewer #2: No

Reviewer #3: Yes: Prof.Dr. Halil İbrahim Ulusoy