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Article
Peer-Review Record

Synthesis and Characterization of a Polydioxanone-Coated Dipeptide-Functionalized Magnetic γ-Fe2O3 Nanoparticles-Modified PES Membrane and Its Biological Applications

Catalysts 2022, 12(10), 1261; https://doi.org/10.3390/catal12101261
by Özlem Demirci 1, Serpil Gonca 2, Veysel Tolan 3, Sadin Özdemir 4, Nadir Dizge 5,* and Ersin Kılınç 6,7,*
Reviewer 1: Anonymous
Reviewer 2: Anonymous
Reviewer 3:
Catalysts 2022, 12(10), 1261; https://doi.org/10.3390/catal12101261
Submission received: 25 September 2022 / Revised: 13 October 2022 / Accepted: 14 October 2022 / Published: 17 October 2022
(This article belongs to the Special Issue Advanced Catalytic Material for Water Treatment)

Round 1

Reviewer 1 Report

The authors of "Synthesis and characterization of polydioxanone coated dipep-2 tide functionalized magnetic γ-Fe2O3 nanoparticles modified 3 PES membrane and its biological applications" prepared a PES-based mixed matrix membrane for antimicrobial photodynamic therapy. The authors state their membrane shows a high antifouling against BSA and E. coli. While they addressed some interesting experimental results (cell viability, photodynamic therapy, etc.), the overall quality of the writing does not meet the expectation, and additional validation must be considered; therefore, this version should not be published in MDPI Catalyst.

 

Main comments (pg#-line#)

2-69 Can you elaborate on what γ-Fe2O3-CA-Leu-Gly-PDX is?

2-77 You mentioned E. Coli in the abstract.

2-87 Can you briefly explain the method?

3-121 Can you add more explanation about this method?

5-197~202 This should be in the intro

5-203~207 This should be in the method

6-230~231 What is your base for this statement?

14-441 What is the standard deviation? What do you mean by NPs not blocking the pores? What do you think the internal structure of the blended membrane looks like? 

14-442 Why do you think the BSA flux increased in the blended membrane? Could it be because the NPs escaped from the PES and created large pores that BSA can freely move through?

14-449 This increased water flux may indicate the free volume within the membrane became larger.

Did you notice any volume change within the swollen membrane after the experiments?

14-452 If the rejection difference is 0.1%, why is your blended membrane novel?

How much NPs diffuse out from PES after 2 hours of the experiment?

 

 

Minor comments

1-18,27 write out PES up-front

1-41 various, please consider running a grammar check

2-51 hydrophobic

3-117,124,4-152 Can you match the font size and style?

Equations 1-4 are quite simple; I would consider incorporating them within the main text.

3-124 Consider calling it Metal Chelating Activity as you discuss in 7-264

4-152 x 100 %

5-180 membranes were

5-187 I would add this to the paragraph.

5-197 naturally

8-300 change the font size

14-440,451 pristine

Author Response

Reviewer 1: The authors of "Synthesis and characterization of polydioxanone coated dipep-2 tide functionalized magnetic γ-Fe2O3 nanoparticles modified 3 PES membrane and its biological applications" prepared a PES-based mixed matrix membrane for antimicrobial photodynamic therapy. The authors state their membrane shows a high antifouling against BSA and E. coli. While they addressed some interesting experimental results (cell viability, photodynamic therapy, etc.), the overall quality of the writing does not meet the expectation, and additional validation must be considered; therefore, this version should not be published in MDPI Catalyst.

 Main comments (pg#-line#)

2-69 Can you elaborate on what γ-Fe2O3-CA-Leu-Gly-PDX is? 

Answer: Corrected

 

2-77 You mentioned E. Coli in the abstract.  

Answer: Corrected

 

2-87 Can you briefly explain the method?

Answer: Corrected

 

3-121 Can you add more explanation about this method?

Answer: More explanation was added

 

5-197~202 This should be in the intro

Answer: The paragraph was moved to the intro section.

 

5-203~207 This should be in the method  

Answer: The paragraph was moved to the intro section.

 

6-230~231 What is your base for this statement?

Answer: The components of γ-Fe2O3-CA-Leu-Gly-PDX are γ-Fe2O3, citric acid, Leu-Gly amino acid and polydioxanone (biodegradable polymer). It is known that all of the components are well known and tolerable on body mechanism. Among them γ-Fe2O3 as member of superparamagnetic iron oxide nanoparticles have been used on therapy as contrast agent for magnetic resonance imaging (MRI). In addition, literature studies showed that the functionalized superparamagnetic iron oxide nanoparticles are a strong candidate for drug delivery for a variety of medicine. Thus, we can conclude that the recommended design could be a candidate for diagnostic and therapy: theranostic.

 

14-441 What is the standard deviation? What do you mean by NPs not blocking the pores? What do you think the internal structure of the blended membrane looks like? 

Answer: The standard deviations were added. Some NPs can be clustered and pore blocking can be occurred. We could not do SEM analysis for this study. However, in our study which was similar to this study, nanocomposite membrane had the finger-like structure                                                                                                   (https://doi.org/10.12989/mwt.2017.8.1.051).

 

14-442 Why do you think the BSA flux increased in the blended membrane? Could it be because the NPs escaped from the PES and created large pores that BSA can freely move through?

Answer: Membrane became more hydrophilic due to blended NPs. The mean pore radius and porosity of the pristine and NPs blended membranes are presented in Table 2. The pore size of the prepared membranes was approximately in the range of UF membranes. The pore radius and porosity of NPs blended membrane were higher than the pristine membrane. In addition, the amount of iron released during the filtration process was determined by AAS analysis, and it was determined that nanoparticle diffusion from the membrane was negligible 2 h of the experiment.

Table 2. Effect of NPs amount on the mean pore size and porosity properties

Membrane sample

Mean pore radius (nm)

Porosity                 (%)

Released iron in permeate (µg/L)

Pristine membrane

22.2±0.5

58.13±2.85

-

NPs blended membrane

20.9±0.4

61.12±3.22

88±9

 

14-449 This increased water flux may indicate the free volume within the membrane became larger. Did you notice any volume change within the swollen membrane after the experiments?

Answer: We did not observe any volume change within the swollen membrane after the experiments

 

14-452 If the rejection difference is 0.1%, why is your blended membrane novel? 

Answer: Rejection is so close but NPs blending preserved the membrane against fouling compared to pristine membrane (Fig. 8). In our opinion, membrane fouling is more important issue than rejection.

How much NPs diffuse out from PES after 2 hours of the experiment?

Answer: Table 2 was added. Please see Table 2.

Minor comments

1-18,27 write out PES up-front

Answer: Corrected

 

1-41 various, please consider running a grammar check

Answer: The language of the MS was critically controlled and corrected by native speaker.

 

2-51 hydrophobic

Answer: Corrected

 

3-117,124,4-152 Can you match the font size and style?

Answer: Corrected

 

Equations 1-4 are quite simple; I would consider incorporating them within the main text.

Answer: Corrected

 

3-124 Consider calling it Metal Chelating Activity as you discuss in 7-264

Answer: Corrected

 

4-152 x 100 %

Answer: Corrected

 

5-180 membranes were

Answer: Corrected

 

5-187 I would add this to the paragraph. Could not understood.

Answer: Corrected

 

5-197 naturally

Answer: Corrected

 

8-300 change the font size

Answer: Corrected

 

14-440,451 pristine

Answer: Corrected

Reviewer 2 Report

In this article, authors mentioned about the on the synthesis of leucyl-glycine functionalized γ-Fe2O3 magnetic nanoparticles coated by polydioxanone (γ-Fe2O3-CA-Leu-Gly-PDX) as PES membrabe for biotech- nological applications. Before publication, there are many points which should be considered, as follows:

 

Need to improve the language of manuscript.

In introduction, need to elaborate  about, why the author choose this material? and mention some other related studies.

Need to replace the blur figure with high quality. Specially Figure 1.

Some errors regarding the sub/super script, spacing and typo need to consider.

Author Response

Reviewer 2: In this article, authors mentioned about the on the synthesis of leucyl-glycine functionalized γ-Fe2O3 magnetic nanoparticles coated by polydioxanone (γ-Fe2O3-CA-Leu-Gly-PDX) as PES membrane for biotechnological applications. Before publication, there are many points which should be considered, as follows:

Need to improve the language of manuscript.

Answer: The language of the MS was critically controlled and corrected by native speaker.

 

In introduction, need to elaborate about, why the author chooses this material? and mention some other related studies.

Answer: Corrected

 

Need to replace the blur figure with high quality. Specially Figure 1.

Answer: The poor quality of Fig. 1 was due to that it was the combination of 4 different spectra-images in an image. If editorially it is ok, we can submit the related pictures as separately. The resolution will be increase.

Some errors regarding the sub/super script, spacing and typo need to consider.

Answer: The MS is completely controlled and corrected.

 

Reviewer 3 Report

In this work, the author successfully synthesized leucyl-glycine functionalized γ-Fe2O3 magnetic nanoparticles coated by polydioxanone (γ-Fe2O3-CA-Leu-Gly-PDX) as PES membrane for biotechnological applications. The as-synthesized samples exhibited excellent inhibition activity. On the whole, the findings are of considerable interest and well done. I recommend it to be published after a major revision. 

1. The novelty needs to refinement and should be highlighted in the introduction part.

2. The authors are responsible for the English, which should be polished throughout the manuscript to clear some minor typo/grammar errors.

- line 18 membrane not membrabe

- Line 25 significant not significiant

- Line 30 pristine not piristine

Please revise all the manuscript.

3. Maybe the author should compare their results clearly with other reported works, highlighting the advantage and disadvantages of their novel composite.

4. Introduction part, if possible, some important and relative reports about Photocatalysis could helped: https://doi.org/10.1016/j.jtice.2021.08.034, https://doi.org/10.1007/s10904-022-02389-8,  https://doi.org/10.1016/j.heliyon.2022.e09652.

5. The conclusion is also not targeted to the important aspects described in the manuscript; please rephrase it.

6. There are many abbreviations in the text that are not explained when they first appear such as BSA, DPPH, ...

7. The author should better improve the beauty and quality of the figures in the manuscript.

 

 

Author Response

Reviewer 3: In this work, the author successfully synthesized leucyl-glycine functionalized γ-Fe2O3 magnetic nanoparticles coated by polydioxanone (γ-Fe2O3-CA-Leu-Gly-PDX) as PES membrane for biotechnological applications. The as-synthesized samples exhibited excellent inhibition activity. On the whole, the findings are of considerable interest and well done. I recommend it to be published after a major revision.

  1. The novelty needs to refinement and should be highlighted in the introduction part.

Answer: The novelty was revised.

 

  1. The authors are responsible for the English, which should be polished throughout the manuscript to clear some minor typo/grammar errors.

Answer: The language of the MS was critically controlled and corrected by native speaker.

 

- line 18 membrane not membrabe

Answer: Corrected

 

- Line 25 significant not significiant

Answer: Corrected

 

- Line 30 pristine not piristine

Answer: Corrected

 

Please revise all the manuscript.

  1. Maybe the author should compare their results clearly with other reported works, highlighting the advantage and disadvantages of their novel composite.

Answer: Table 3 shows the performance comparison of γ-Fe2O3-CA-Leu-Gly-PDX blended PES membrane with other reported modified PES membranes. From the table, the competitive performance of the PES/γ-Fe2O3-CA-Leu-Gly-PDX composite membrane in terms of improved BSA and E. coli rejection is evident.

Table 3. Performance comparison of PES membranes blended with different NPs.

Material

Model solution

NPs amount

Main results for modified membrane

Reference

γ-Fe2O3-CA-Leu-Gly-PDX

BSA

E. coli

1.0 wt%

·                     Pure water permeability: 49.3 L/(m2 h bar

·                     BSA removal: 100%

·                     E. coli removal: 100%

  • Porosity: 61.12%
  • Mean pore radius:  20.9 nm

This study

Fe3O4 decorated halloysite nanoclay (Fe-HNC)

Humic acid (HA)

0.1 wt%

·                     Pure water permeability: 294.4 L/(m2 h bar

·         HA removal: 90.1%

  • High fouling recovery: 70.4 %
  • Porosity: 77.5%
  • Mean pore radius:  57.9 nm

Ouda et. al. 2022

Polydopamine coated ZnFe2O4

HA

4 wt%

·                     Pure water permeability: 687 L/(m2 h bar

·         HA removal: 82%

  • Porosity: 80%
  • Mean pore radius:  69 nm

Kallem et. al. 2021

PHEMA-grafted SiO2

BSA

10 wt%

·                     Pure water permeability: 190 L/(m2 h bar

·         BSA removal: 75.5%

Zhu et. al. 2014

 

  1. Introduction part, if possible, some important and relative reports about Photocatalysis could helped: https://doi.org/10.1016/j.jtice.2021.08.034, https://doi.org/10.1007/s10904-022-02389-8, https://doi.org/10.1016/j.heliyon.2022.e09652.

Answer: Thanks for contribution, two of them are directly related with MS and cited.

 

  1. The conclusion is also not targeted to the important aspects described in the manuscript; please rephrase it.

Answer: The conclusion was revised.

  1. There are many abbreviations in the text that are not explained when they first appear such as BSA, DPPH, ...

Answer: Corrected

 

  1. The author should better improve the beauty and quality of the figures in the manuscript.

Answer: The poor quality of Fig. 1 was due to that it was the combination of 4 different spectra-images in an image. If editorially it is ok, we can submit the related pictures as separately. The resolution will be increase.

Round 2

Reviewer 1 Report

Looks great to me.

My only suggestion is to consider aligning your photos. I bet the Height:Width ratio is not 1:1 for most of your figures. 

If you are using Words, right-click on the picture -> Size and Position -> Layout -> Size -> Scale, make sure all photos are in the same ratio and click Lock aspect ratio to avoid this issue.

Reviewer 3 Report

accepted in present form

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