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Article
Peer-Review Record

Study on the Stability of Antibiotics, Pesticides and Drugs in Water by Using a Straightforward Procedure Applying HPLC-Mass Spectrometric Determination for Analytical Purposes

Separations 2021, 8(10), 179; https://doi.org/10.3390/separations8100179 (registering DOI)
by Salvatore Barreca *, Carola Forni, Luisa Colzani, Laura Clerici, Daniela Daverio and Pierluisa Dellavedova
Reviewer 1: Anonymous
Reviewer 2: Anonymous
Reviewer 3: Anonymous
Separations 2021, 8(10), 179; https://doi.org/10.3390/separations8100179 (registering DOI)
Submission received: 7 September 2021 / Revised: 27 September 2021 / Accepted: 1 October 2021 / Published: 9 October 2021
(This article belongs to the Special Issue HPLC: A Key Tool for Analytical Chemistry)

Round 1

Reviewer 1 Report

The manuscript presents the study of various compounds' stability investigation. The manuscript was corrected in comparison with the previous version.

However, there are still significant drawbacks, that need to be corrected. 

Firs problem with the work like before is the style. There are a lot of paragraphs that contain one sentence. It is difficult to read. In the introduction, there are 7 one-sentence paragraphs!!!

The most important scientific drawbacks are listed below:

Is there a binary and quaternary pump in one UPLC?

I can see Figure 1 that repeats data from Table 3, but the figure caption is removed. Ti may be a problem of track changes function. 

There are some typological mistakes in corrected sentences that have to be corrected.

Author Response

The authors thank you the very much reviewers for their helpful  improvement advice. The replies to the comments are given below..

 

Reviewer 1

The manuscript presents the study of various compounds' stability investigation. The manuscript was corrected in comparison with the previous version.

 

However, there are still significant drawbacks, that need to be corrected.

 

Firs problem with the work like before is the style. There are a lot of paragraphs that contain one sentence. It is difficult to read. In the introduction, there are 7 one-sentence paragraphs!!!

  1. Introduction was emproved.

 

The most important scientific drawbacks are listed below:

 

Is there a binary and quaternary pump in one UPLC?

  1. I'm so sorry. Quaternary pump was refer to a previusly paper concerning a validation method for SPE-ONLINE

 

I can see Figure 1 that repeats data from Table 3, but the figure caption is removed. Ti may be a problem of track changes function.

  1. Figure 1 war removed

 

There are some typological mistakes in corrected sentences that have to be corrected.

R: Some corrections were made.

 

 

Reviewer 2

Nevertheless, few small additional comments should be addressed for Authors. First of them is trivial name of one of compounds of interest, which is still named as “ciproflo-xacina”.  The reviewer has checked this name in Internet and the result was “ciproflo-xacin” (not “ciprofloxacine”). Please correct it anywhere in the text.


  1. Ciprofoxacine were corrected in ciprofoxacin

 

Secondly, concerning the data presented in Table 4, namely “Precision, RSD, %” and “Accuracy”. It seems not necessary to indicate two decimal digits in all of them. All values should be rounded up to only one decimal digit. 

  1. Accuracy and precision in table 4 were reported bu one decimal. 

The mentioned comments seem to be not principal, so that after their corrections the manuscript cam be recommended for publication.

he work hereby presented is a study on the stability of antibiotics, pesticides and drugs in water using high performance liquid chromatography-mass spectrometry for the determination of the analytes. Despite being not particularly significant in terms of novelty, the study deserves some interest from scholars working in the field residues analysis. I therefore recommend publication after some corrections.

 

Reviewer 3

-Title: I suggest changing the word “detection” to “determination” since quantitative results are also reported in the study.

 

  1. Detection were changed in determination

 

-Abstract: Please provide the abbreviations (e.g., ACN)

  1. ACN abbreviatons was added

 

-Introduction: This part needs re-organization. The authors could make paragraphs and not present each sentence as a paragraph (lines-44-67).

  1. Introduction was emproved

 

-Section 2.1: Information about the purity of the analytes should be also included.

  1. Line 89 report the sequent information: The purity grade of all standards was always above 94%.

 

-Section 2.1.: When abbreviations are provided, they must be used in the manuscript instead of the full word (e.g., line 86: acetonitrile). Please check this throughout the manuscript.

  1. ACN was used as abreviation

 

-Table 2: Check the spaces between the analytes and the “-1 or -2”.

  1. space were checked

 

-Table 3 and line 117: Please replace “formiate” with “formate”

  1. Formiate was replace with formate

 

-Table 4: The title needs to be changed

  1. Title was changed

 

-Line 171: Please provide the appropriate references.

  1. Reference was added

 

-References: They are not in accordance with Separations guidelines.

  1. References were reported in accordance with separations guidelines.

Reviewer 2 Report

See the file attached

Comments for author File: Comments.docx

Author Response

The authors thank you the very much reviewers for their helpful  improvement advice. The replies to the comments are given below..

 

Reviewer 1

The manuscript presents the study of various compounds' stability investigation. The manuscript was corrected in comparison with the previous version.

 

However, there are still significant drawbacks, that need to be corrected.

 

Firs problem with the work like before is the style. There are a lot of paragraphs that contain one sentence. It is difficult to read. In the introduction, there are 7 one-sentence paragraphs!!!

  1. Introduction was emproved.

 

The most important scientific drawbacks are listed below:

 

Is there a binary and quaternary pump in one UPLC?

  1. I'm so sorry. Quaternary pump was refer to a previusly paper concerning a validation method for SPE-ONLINE

 

I can see Figure 1 that repeats data from Table 3, but the figure caption is removed. Ti may be a problem of track changes function.

  1. Figure 1 war removed

 

There are some typological mistakes in corrected sentences that have to be corrected.

R: Some corrections were made.

 

 

Reviewer 2

Nevertheless, few small additional comments should be addressed for Authors. First of them is trivial name of one of compounds of interest, which is still named as “ciproflo-xacina”.  The reviewer has checked this name in Internet and the result was “ciproflo-xacin” (not “ciprofloxacine”). Please correct it anywhere in the text.


  1. Ciprofoxacine were corrected in ciprofoxacin

 

Secondly, concerning the data presented in Table 4, namely “Precision, RSD, %” and “Accuracy”. It seems not necessary to indicate two decimal digits in all of them. All values should be rounded up to only one decimal digit. 

  1. Accuracy and precision in table 4 were reported bu one decimal. 

The mentioned comments seem to be not principal, so that after their corrections the manuscript cam be recommended for publication.

he work hereby presented is a study on the stability of antibiotics, pesticides and drugs in water using high performance liquid chromatography-mass spectrometry for the determination of the analytes. Despite being not particularly significant in terms of novelty, the study deserves some interest from scholars working in the field residues analysis. I therefore recommend publication after some corrections.

 

Reviewer 3

-Title: I suggest changing the word “detection” to “determination” since quantitative results are also reported in the study.

 

  1. Detection were changed in determination

 

-Abstract: Please provide the abbreviations (e.g., ACN)

  1. ACN abbreviatons was added

 

-Introduction: This part needs re-organization. The authors could make paragraphs and not present each sentence as a paragraph (lines-44-67).

  1. Introduction was emproved

 

-Section 2.1: Information about the purity of the analytes should be also included.

  1. Line 89 report the sequent information: The purity grade of all standards was always above 94%.

 

-Section 2.1.: When abbreviations are provided, they must be used in the manuscript instead of the full word (e.g., line 86: acetonitrile). Please check this throughout the manuscript.

  1. ACN was used as abreviation

 

-Table 2: Check the spaces between the analytes and the “-1 or -2”.

  1. space were checked

 

-Table 3 and line 117: Please replace “formiate” with “formate”

  1. Formiate was replace with formate

 

-Table 4: The title needs to be changed

  1. Title was changed

 

-Line 171: Please provide the appropriate references.

  1. Reference was added

 

-References: They are not in accordance with Separations guidelines.

  1. References were reported in accordance with separations guidelines.

Reviewer 3 Report

The work hereby presented is a study on the stability of antibiotics, pesticides and drugs in water using high performance liquid chromatography-mass spectrometry for the determination of the analytes. Despite being not particularly significant in terms of novelty, the study deserves some interest from scholars working in the field residues analysis. I therefore recommend publication after some corrections.

 

-Title: I suggest changing the word “detection” to “determination” since quantitative results are also reported in the study.

-Abstract: Please provide the abbreviations (e.g., ACN)

-Introduction: This part needs re-organization. The authors could make paragraphs and not present each sentence as a paragraph (lines-44-67).

-Section 2.1: Information about the purity of the analytes should be also included.

-Section 2.1.: When abbreviations are provided, they must be used in the manuscript instead of the full word (e.g., line 86: acetonitrile). Please check this throughout the manuscript.

-Table 2: Check the spaces between the analytes and the “-1 or -2”.

-Table 3 and line 117: Please replace “formiate” with “formate”

-Table 4: The title needs to be changed

-Line 171: Please provide the appropriate references.

-References: They are not in accordance with Separations guidelines.

Author Response

The authors thank you the very much reviewers for their helpful  improvement advice. The replies to the comments are given below..

 

Reviewer 1

The manuscript presents the study of various compounds' stability investigation. The manuscript was corrected in comparison with the previous version.

 

However, there are still significant drawbacks, that need to be corrected.

 

Firs problem with the work like before is the style. There are a lot of paragraphs that contain one sentence. It is difficult to read. In the introduction, there are 7 one-sentence paragraphs!!!

  1. Introduction was emproved.

 

The most important scientific drawbacks are listed below:

 

Is there a binary and quaternary pump in one UPLC?

  1. I'm so sorry. Quaternary pump was refer to a previusly paper concerning a validation method for SPE-ONLINE

 

I can see Figure 1 that repeats data from Table 3, but the figure caption is removed. Ti may be a problem of track changes function.

  1. Figure 1 war removed

 

There are some typological mistakes in corrected sentences that have to be corrected.

R: Some corrections were made.

 

 

Reviewer 2

Nevertheless, few small additional comments should be addressed for Authors. First of them is trivial name of one of compounds of interest, which is still named as “ciproflo-xacina”.  The reviewer has checked this name in Internet and the result was “ciproflo-xacin” (not “ciprofloxacine”). Please correct it anywhere in the text.


  1. Ciprofoxacine were corrected in ciprofoxacin

 

Secondly, concerning the data presented in Table 4, namely “Precision, RSD, %” and “Accuracy”. It seems not necessary to indicate two decimal digits in all of them. All values should be rounded up to only one decimal digit. 

  1. Accuracy and precision in table 4 were reported bu one decimal. 

The mentioned comments seem to be not principal, so that after their corrections the manuscript cam be recommended for publication.

he work hereby presented is a study on the stability of antibiotics, pesticides and drugs in water using high performance liquid chromatography-mass spectrometry for the determination of the analytes. Despite being not particularly significant in terms of novelty, the study deserves some interest from scholars working in the field residues analysis. I therefore recommend publication after some corrections.

 

Reviewer 3

-Title: I suggest changing the word “detection” to “determination” since quantitative results are also reported in the study.

 

  1. Detection were changed in determination

 

-Abstract: Please provide the abbreviations (e.g., ACN)

  1. ACN abbreviatons was added

 

-Introduction: This part needs re-organization. The authors could make paragraphs and not present each sentence as a paragraph (lines-44-67).

  1. Introduction was emproved

 

-Section 2.1: Information about the purity of the analytes should be also included.

  1. Line 89 report the sequent information: The purity grade of all standards was always above 94%.

 

-Section 2.1.: When abbreviations are provided, they must be used in the manuscript instead of the full word (e.g., line 86: acetonitrile). Please check this throughout the manuscript.

  1. ACN was used as abreviation

 

-Table 2: Check the spaces between the analytes and the “-1 or -2”.

  1. space were checked

 

-Table 3 and line 117: Please replace “formiate” with “formate”

  1. Formiate was replace with formate

 

-Table 4: The title needs to be changed

  1. Title was changed

 

-Line 171: Please provide the appropriate references.

  1. Reference was added

 

-References: They are not in accordance with Separations guidelines.

  1. References were reported in accordance with separations guidelines.

This manuscript is a resubmission of an earlier submission. The following is a list of the peer review reports and author responses from that submission.


Round 1

Reviewer 1 Report

The manuscript presents the results of experimentally simple, but in any extent useful work on characterizing the stability of some drugs and pesticides in dilute water solutions. It is important as the first step of such characterization, and this approach obviously can be improved in future. However, principally there are no serious limitations of the publication of this manuscript in “Separations”, but only after correcting (or explaining) the following moments:

Page 2, line 49: “neonEcotinoids” Misprinting should be corrected as “neonIcotinoids”.

Page 3: What is the sense to present two tables of different content as Table 1A and Table 1B. Following to the same logics, all other tables may be enumerated as Table 1C, Table 1D, etc.;

The titles of first columns in Tables 1B, 3, 4, 4 again, and 6: “Analyta” is Italian word; in English should be “Analyte”. Please correct;

Page 3-4; Table 1B: The sense of duplication of the data for all analytes (e.g., Trimethoprim-1 and Trimethoprim-2) should be clearly explained despite of their understandability;

Page 4, the last compound in Table 1B: “Ciprofloxacina” is Italian word; in English should be “Ciprofloxacine”;

Page 4, line 126 (twice) and titles of columns 3 and 4 in Table 4: instead “formiate” in English should be “formate”;

Page 5: Titles of the columns 2 and 3 in Table 3 are absolutely identical (it is senseless). The single difference is “Surface water” in the column 3 and “Surface Water” in the column 4. What is the heuristically aim to write “Water” with capital letter? Please correct this nonsense;

Page 6: Figure 1 duplicates the content of Table 3. Is it permitted by rules of “Separations”? According to reviewer’s point of view, such figure should be deleted;

Page 8: Figure 2 duplicated the content of Table 4; the same comment;

The same page: Surprising reader founds the second Table 4. If it is not enough; let us add few Tables with the same number in the text. If seriously, the sense of this Table (Percentage differences) seems to be not important, hence this Table can be deleted;

Page 10: Figure 3 duplicated the content of Table 6; the same comment as above;

No page (general): The data included in Tables 3, 4, and 4’ are presented without standard deviations. Thus, all of them seem like results of single measurements. Please provide standard deviations or explain using the results of singly-point measurements.

No page (general): The manuscript contains no possible explanations the reasons of low stability of selected analytes in water solutions. Without such explanations it looks like so-called natural philosophy (registration of any facts without their interpretation). Any hypotheses on low stability of analytes are highly desirable.

All comments mentioned above mean the necessity of the revision of the manuscript. Nevertheless, the “level” of such revision is not “major” and can be classified as “moderate” (not minor).

Reviewer 2 Report

The manuscript presents the study of various compounds' stability investigation. Because of significant drawbacks, I cannot recommend this work for publication. 

Firs problem with the work is the style. There are a lot of paragraphs that contain one sentence. It is difficult to read.

The scientific drawbacks are listed below:

The problem is that there is no validation data for the method.

Fig 1 seems to repeat data from Table 3

Two columns in table 3 have the same caption but values are different.

There are no standard deviations values in Table 3, Fig. 1. Table 4. Fig. 2 etc. IT causes that it is not possible to trust the results. 

In my opinion recovery and stability, the investigation is not the same.

Obtained results in its form can not conclude about stability.

Stability investigation should contain some kinetics evaluation. 

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