Acetylcholine esterase inhibitory activity of green synthesized nanosilver by naphthopyrones isolated from marine-derived Aspergillus niger

Ghada Mahmoud Abdelwahab; Amira Mira; Yuan-Bin Cheng; Tarek A. Abdelaziz; Mohamed Farid I. Lahloub; Ashraf Taha Khalil

doi:10.1371/journal.pone.0257071

Peer Review History

Original SubmissionFebruary 16, 2021
1 Apr 2021 Decision Letter - Yogendra Kumar Mishra, Editor PONE-D-21-05273 Acetylcholine esterase inhibitory activity of green synthesized nanosilver by naphthopyrones isolated from marine-derived Aspergillus Niger PLOS ONE Dear Dr. Abdelwahab, Thank you for submitting your manuscript to PLOS ONE. After careful consideration, we feel that it has merit but does not fully meet PLOS ONE’s publication criteria as it currently stands. Therefore, we invite you to submit a revised version of the manuscript that CAREFULLY addresses the points raised during the review process. Referees might have suggested some literature citations, authors are free to decide upon. Please submit your revised manuscript by May 16 2021 11:59PM. If you will need more time than this to complete your revisions, please reply to this message or contact the journal office at plosone@plos.org. When you're ready to submit your revision, log on to https://www.editorialmanager.com/pone/ and select the 'Submissions Needing Revision' folder to locate your manuscript file. Please include the following items when submitting your revised manuscript: A rebuttal letter that responds to each point raised by the academic editor and reviewer(s). You should upload this letter as a separate file labeled 'Response to Reviewers'. A marked-up copy of your manuscript that highlights changes made to the original version. You should upload this as a separate file labeled 'Revised Manuscript with Track Changes'. An unmarked version of your revised paper without tracked changes. You should upload this as a separate file labeled 'Manuscript'. If you would like to make changes to your financial disclosure, please include your updated statement in your cover letter. Guidelines for resubmitting your figure files are available below the reviewer comments at the end of this letter. If applicable, we recommend that you deposit your laboratory protocols in protocols.io to enhance the reproducibility of your results. Protocols.io assigns your protocol its own identifier (DOI) so that it can be cited independently in the future. For instructions see: http://journals.plos.org/plosone/s/submission-guidelines#loc-laboratory-protocols. Additionally, PLOS ONE offers an option for publishing peer-reviewed Lab Protocol articles, which describe protocols hosted on protocols.io. Read more information on sharing protocols at https://plos.org/protocols?utm_medium=editorial-email&utm_source=authorletters&utm_campaign=protocols. We look forward to receiving your revised manuscript. Kind regards, Yogendra Kumar Mishra, Ph. D. Academic Editor PLOS ONE Journal Requirements: When submitting your revision, we need you to address these additional requirements. 1. Please ensure that your manuscript meets PLOS ONE's style requirements, including those for file naming. The PLOS ONE style templates can be found at https://journals.plos.org/plosone/s/file?id=wjVg/PLOSOne_formatting_sample_main_body.pdf and https://journals.plos.org/plosone/s/file?id=ba62/PLOSOne_formatting_sample_title_authors_affiliations.pdf 2. In your Methods section, please provide additional information regarding the permits you obtained for the work. Please ensure you have included the full name of the authority that approved the field site access and, if no permits were required, a brief statement explaining why. 3. In your Methods section, please provide additional location information, including geographic coordinates for the data set if available. [Note: HTML markup is below. Please do not edit.] 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: Partly ******** 2. Has the statistical analysis been performed appropriately and rigorously? Reviewer #1: Yes Reviewer #2: No ****** 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 ****** 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: No ****** 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: In the present work Abdelwahab et. Al. described the separation and characterization of six naphtho-�-pyrones (2 monomers and 4 dimers) and one pyridine-4-one alkaloid from solid culture of marine-derived Aspergillus niger for application in acetylcholine esterase inhibitory activity (AChEI). Further Ag nanoparticles were also synthesized and tested for AChEI. The results are interesting. However, there are some defects needed to be further revised. Including: 1. Characterization of Ag NPs are poor. Authors should provide XRD, Raman and XPS analysis for proper characterization. 2. There is absent of mechanism interpretation and analysis to support the conclusion 3. The quality of ALL OF FIGURES should be further decorated. The following literature should be consulted and employed: 4. The English should be carefully polished. Also, many format problems should be addressed. ACS Biomaterials Science & Engineering, 2020, 6, 5527–5537; Theranostics, 2020, 10, 7841-7856; Journal of Biomedical Nanotechnology, 2020, 16, 283-303. Reviewer #2: The manuscript entitiled “Acetylcholine esterase inhibitory activity of green synthesized nanosilver by naphthopyrones isolated from marine-derived Aspergillus Niger” submitted by Abdelwahab et al is an nice submission regarding advancement in nanotechnology. The idea , concept and the methodology of the manuscript is novel as well as well defined however as manuscript , it consist of many flaws that needs to be corrected before acceptance. The comments are : 1. The whole manuscript should be screened and rewritten with proper English. The quality of the English is really poor which is ruining the quality of the work. 2. Abstract needs to be rewritten defining the novelty of work with some quantitative data. 3. The first para of the introduction is full of typos and grammatical error. Moreover, the content are rewritten. `This paragraph must be rewritten with a full formatting. 4. Paragraph 3, Write the hypothesis of the work and the novelty. 5. Number of recent manuscript has been published in silver nanoparticles, Authors should cite the recent papers. Some of the suggestion are in the last comment. 6. Don’t keep the section 2.3. It looks odd to give heading and saying it has been mentioned previously. 7. Combine section 2.4 and 2.5 under one subheading. 8. Section 2.9, use proper annotations and numerical. 9. Materials and methods section needs to be written in more details. 10. Please don’t use compound number in result section. Use the full name or an short name of the compound. 11. Table 1 needs to be presented as an graph. It should be not presented in this way. What was the SPR peak of the scan? 12. Figure 2 needs to be redrawn. The resolution is too poor. 13. Table 2 is not OK. Description and data is not matching. 14. Figure 4 is not okay.. resolution needs to be improved. 15. Where is the discussion? The authors has no where defined and discussed the significance of their finding. It seems that the manuscript is incomplete. 16. Lastly, the authors are suggested to cite recent papers like DOI: 10.1039/C7RA05943D, https://doi.org/10.1093/toxsci/kfx204, https://doi.org/10.1016/j.msec.2018.07.037,https://doi.org/10.1080/21691401.2018.1503598 , DOI: 10.1016/j.msec.2021.111888 , DOI: 10.1016/j.bioorg.2020.104535 , DOI: 10.2217/nnm-2020-0138, DOI: 10.1016/j.mtchem.2020.100299; DOI: 10.1016/j.mtchem.2020.100345; https://doi.org/10.1021/acsomega.7b01522 ****** 6. 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 [NOTE: If reviewer comments were submitted as an attachment file, they will be attached to this email and accessible via the submission site. Please log into your account, locate the manuscript record, and check for the action link "View Attachments". If this link does not appear, there are no attachment files.] While revising your submission, please upload your figure files to the Preflight Analysis and Conversion Engine (PACE) digital diagnostic tool, https://pacev2.apexcovantage.com/. PACE helps ensure that figures meet PLOS requirements. To use PACE, you must first register as a user. Registration is free. Then, login and navigate to the UPLOAD tab, where you will find detailed instructions on how to use the tool. 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Revision 1
18 Jun 2021 Author Response Reviewer #1:. 1- (a) X-ray diffraction (XRD) analysis is used to check the crystalline nature of silver nanoparticles. So, it should be done on the dried powder. In our case, after lyophilization, it was a sticky material at the end of the wasserman test tube (as seen in Figure 3) because the amount of starting compound entering the synthesis was very little so, it cannot be in a crystal or powder form. In addition, other published papers performed (XRD) analysis because they used total extract in green synthesis of silver nanoparticles. Consequently, they have large amount but in our experiment we used pure isolated compounds with little yield. (b) XPS is used for elemental analysis using solid surface and Raman is used for chemical structure identification as well as detection of contamination and impurities and give information about phase and polymorphism. In case of silver nanoparticles synthesized by total extract, Raman and XPS were performed as the total extract may contain different organic metabolites and other elements as impurities but here we used pure organic compounds which were isolated by pure organic solvents as proved by their NMR data attached in the supplementary file. Therefore, the probability of the presence of other elements is almost non-existent. Also these analyses are too expensive in our country due to low facilities and lack of funding. There is only one available equipment and it is reserved for several months. 2- Regarding the mechanism interpretation and analysis to support the conclusion; the effect of silver nanoparticles alone on acetylcholine esterase enzyme was performed and its IC50 is 2.29 ± 0.013 uM/ml. This confirms that the pure isolated organic compounds have synergistic effect on acetylcholine esterase inhibition after capping with silver nanoparticles possibly by stabilizing them for a longer time to exert its effect. 3- The quality of all figures was improved and resolution was adjusted between 300-600 dpi to meet PLOS ONE's style figure requirements. Reviewer #2: 1- The whole manuscript was screened and some were rewritten with proper English. 2- Abstract was rewritten defining the novelty of work with some quantitative data. 3- The first paragraph was revised with a full formatting. 4- In paragraph 3, the hypothesis and the novelty of the work were added. 5- Some recent papers of your suggestions were added. 6- Section 2.3 was added to section 2.2. 7- Section 2.5 was combined with section 2.4 under one sub-heading. 8- Proper annotations were used as possible as we can. 9- Some details were added in Methods section. 10- The compound number was replaced by the full name of the compound in the result section. 11- Table 1 presented as a graph in Figure 4. The SPR was between 440 to 462 nm and was added to the manuscript. 12- Figure 2 was changed to Figure 3 and was re-drawn. The resolution was adjusted between 300-600 dpi to meet PLOS ONE's style figure requirements. 13- Table 2 became Table 1 and was revised. 14- Figure 4 became Figure 6 and was re-drawn. The resolution was adjusted between 300-600 dpi to meet PLOS ONE's style figure requirements. 15- Discussion was revised, clarified and significance of the findings was discussed in section 3.3 16- Recent papers were cited. Attachments Attachment Submitted filename: Response to Reviewers.docx https://doi.org/10.1371/journal.pone.0257071.r002
16 Jul 2021 Decision Letter - Mohammad Shahid, Editor PONE-D-21-05273R1 Acetylcholine esterase inhibitory activity of green synthesized nanosilver by naphthopyrones isolated from marine-derived Aspergillus niger PLOS ONE Dear Dr. Abdelwahab, Thank you for submitting your manuscript to PLOS ONE. After careful consideration, we feel that it has merit but does not fully meet PLOS ONE’s publication criteria as it currently stands. Therefore, we invite you to submit a revised version of the manuscript that addresses the points raised during the review process. Please submit your revised manuscript by Aug 30 2021 11:59PM. If you will need more time than this to complete your revisions, please reply to this message or contact the journal office at plosone@plos.org. When you're ready to submit your revision, log on to https://www.editorialmanager.com/pone/ and select the 'Submissions Needing Revision' folder to locate your manuscript file. Please include the following items when submitting your revised manuscript: A rebuttal letter that responds to each point raised by the academic editor and reviewer(s). You should upload this letter as a separate file labeled 'Response to Reviewers'. A marked-up copy of your manuscript that highlights changes made to the original version. You should upload this as a separate file labeled 'Revised Manuscript with Track Changes'. An unmarked version of your revised paper without tracked changes. You should upload this as a separate file labeled 'Manuscript'. If you would like to make changes to your financial disclosure, please include your updated statement in your cover letter. Guidelines for resubmitting your figure files are available below the reviewer comments at the end of this letter. If applicable, we recommend that you deposit your laboratory protocols in protocols.io to enhance the reproducibility of your results. Protocols.io assigns your protocol its own identifier (DOI) so that it can be cited independently in the future. For instructions see: http://journals.plos.org/plosone/s/submission-guidelines#loc-laboratory-protocols. Additionally, PLOS ONE offers an option for publishing peer-reviewed Lab Protocol articles, which describe protocols hosted on protocols.io. Read more information on sharing protocols at https://plos.org/protocols?utm_medium=editorial-email&utm_source=authorletters&utm_campaign=protocols. We look forward to receiving your revised manuscript. Kind regards, Mohammad Shahid, Ph.D. Academic Editor PLOS ONE [Note: HTML markup is below. Please do not edit.] 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 #2: (No Response) ******** 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 #2: Partly ****** 3. Has the statistical analysis been performed appropriately and rigorously? Reviewer #2: No ****** 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 #2: Yes ****** 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 #2: 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 #2: The author has tried to response the queries well however, the discussion part is still not convincing. Authors are suggested to describe the results in a how and why pattern. Right now , only results are there. I will suggest them to separate the result and discussion section and provide a detail discussion. In my opinion, its a crucial part for any manuscript and can't be ignored. Manuscript may be accepted after that followed by review. ****** 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 #2: No [NOTE: If reviewer comments were submitted as an attachment file, they will be attached to this email and accessible via the submission site. Please log into your account, locate the manuscript record, and check for the action link "View Attachments". If this link does not appear, there are no attachment files.] While revising your submission, please upload your figure files to the Preflight Analysis and Conversion Engine (PACE) digital diagnostic tool, https://pacev2.apexcovantage.com/. PACE helps ensure that figures meet PLOS requirements. To use PACE, you must first register as a user. Registration is free. Then, login and navigate to the UPLOAD tab, where you will find detailed instructions on how to use the tool. If you encounter any issues or have any questions when using PACE, please email PLOS at figures@plos.org. Please note that Supporting Information files do not need this step. https://doi.org/10.1371/journal.pone.0257071.r003
Revision 2
21 Aug 2021 Author Response Response to reviewers 1- Adressed to reviewer #2. (Previous round). 2- Adressed to reviewer #2. (Technically sound). 3- Adressed to reviewer #2. (Statistical analysis). 4- Adressed to reviewer #2. (Data availability). 5- Adressed to reviewer #2. (Standard English). 6- The reviewer suggested a more focus on discussion part and separate it from results which were actullay did. The results (P.6) and discussion (P.9) section was separated and the results were described in how and why pattern. Really, it is a crucial part. Thank you for your opinion and effort. 7- This item also was addressed to reviewer #2. We did our maximum efforts to improve the manuscript guided by editor and reviewers' comments and we hope that the final version will be satisfactory for respected editor and reviewers. Thank you Attachments Attachment Submitted filename: Response to reviewers.docx https://doi.org/10.1371/journal.pone.0257071.r004
24 Aug 2021 Decision Letter - Mohammad Shahid, Editor Acetylcholine esterase inhibitory activity of green synthesized nanosilver by naphthopyrones isolated from marine-derived Aspergillus niger PONE-D-21-05273R2 Dear Dr. Abdelwahab, 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. An invoice for payment will follow shortly after the formal acceptance. To ensure an efficient process, please log into Editorial Manager at http://www.editorialmanager.com/pone/, click the 'Update My Information' link at the top of the page, and double check that your user information is up-to-date. If you have any billing related questions, please contact our Author Billing department directly at authorbilling@plos.org. If your institution or institutions have a press office, please notify them about your upcoming paper to help maximize its impact. If they’ll be preparing press materials, please inform our press team as soon as possible -- no later than 48 hours after receiving the formal acceptance. Your manuscript will remain under strict press embargo until 2 pm Eastern Time on the date of publication. For more information, please contact onepress@plos.org. Kind regards, Mohammad Shahid, Ph.D. Academic Editor PLOS ONE 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 #2: All comments have been addressed ******** 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 #2: Yes ****** 3. Has the statistical analysis been performed appropriately and rigorously? Reviewer #2: 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 #2: Yes ****** 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 #2: 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 #2: The authors have addressed now all the queries and nicely revised the manuscript. The manuscript can now be accepted followed by the supervision of editor. ****** 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 #2: No https://doi.org/10.1371/journal.pone.0257071.r005
Formally Accepted
31 Aug 2021 Acceptance Letter - Mohammad Shahid, Editor PONE-D-21-05273R2 Acetylcholine esterase inhibitory activity of green synthesized nanosilver by naphthopyrones isolated from marine-derived Aspergillus niger Dear Dr. Abdelwahab: I'm pleased to inform you that your manuscript has been deemed suitable for publication in PLOS ONE. Congratulations! Your manuscript is now with our production department. If your institution or institutions have a press office, please let them know about your upcoming paper now to help maximize its impact. If they'll be preparing press materials, please inform our press team within the next 48 hours. Your manuscript will remain under strict press embargo until 2 pm Eastern Time on the date of publication. For more information please contact onepress@plos.org. If we can help with anything else, please email us at plosone@plos.org. Thank you for submitting your work to PLOS ONE and supporting open access. Kind regards, PLOS ONE Editorial Office Staff on behalf of Dr. Mohammad Shahid Academic Editor PLOS ONE https://doi.org/10.1371/journal.pone.0257071.r006

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