Quantification of the Synthetic Phenolic Antioxidant Cyanox 1790 in Bottled Water with SPE-HPLC/MS/MS and Determination of the Impact of the Use of Recycled Packaging on Its Generation

Round 1

Reviewer 1 Report

In this manuscript, negative effect of SPAs Cyanox 1790 present in the packaged bottle is discussed specifically in Colombia. The study has the potential as these molecules are harmful for human life, aquatic life and environment. Some points need to be taken care of:

1. Plagiarism is 9% that can be acceptable

2. Grammatical mistakes are very common in the manuscript.

3. Can authors think of some possible solution for the problem as reusability is also maximizing the concentrations of Cyanox 1790.

4. Title should be more precise.

Author Response

Dear,

Very kind for reviewing this research. We have attached the responses to your comments. We have answered all of them and, as expected, made all the corrections.

1. Plagiarism is 9% that can be acceptable

R/ Thank you for reviewing this research. It has been difficult for us to bring it to 9%. We tested it previously and lowered it to a tiny percentage.

2. Grammatical mistakes are very common in the manuscript.

R/ Thank you for reviewing this research. We have made the corrections

3. Can authors think of some possible solution for the problem as reusability is also maximizing the concentrations of Cyanox 1790.

R/ Thank you for reviewing this research.Nosotros consideramos que la solución es que las empresas productoras utilicen aditivos antioxidantes que no sen agresivos para los seres humanos. Mientras estos cambios no se realicen o no se eliminen la causa raíz del problema las soluciones serán superficiales

4. Title should be more precise.

R/ Thank you for reviewing this research.Nosotros hemos modificado el titulo para tener mayor precisión.

Reviewer 2 Report

Manuscript ID: water-2220085

I reviewed your manuscript “Identification and quantification of the synthetic phenolic anti-oxidant 1,3,5-Tris (4-tert-butyl-3-hydroxy-2,6-dimethyl benzyl)- 1,3,5-triazine-2,4,6-(1H,3H,5H)-trione (Cyanox 1790) in bottled water in Colombia.” very carefully. The work carried out in the manuscript is interesting and seems logical. However, there are several errors in this work and before publication, it needs to restructure the research manuscript properly. Therefore, I would like to recommend this manuscript for "Major Revision".

1.      The novelty of this work was not specified; authors should discuss the novelty of their work in the introduction section.

2.      In abstract correct this sentence, “Cyanox 1790 is a SPA that, although it is not a food additive, but polymeric, could be present in food that is stored in containers made of some type of polymer.”

3.      There are many spelling mistakes in manuscript even in abstract too. I can’t mentioned here all of them, like, bottlesranged, Mostrado, levelis and many maore. Athors advised to revised carefuly and consult native English speaker. Also correct the formatting errors.

4.      Sequencing of abstract sentences is also not appropriate

5.      In introduction section cite these articles on bottled water and water contaminants, https://doi.org/10.1080/03067319.2020.1846732, Inorganic Chemistry Communications 145 (2022) 110008, Surfaces and Interfaces 34 (2022) 102324.

6.      Authors add many references unnecessarily like, “The relative standard deviation (RSD) and LOD for the determination of SPA by HPLC are both less than 10%.[3], [66]–[68] in matrices with low[42],  [64], [65]to complexity of [3], [66]–[68]chemical content. Differential heat scanning (DSCs) has been used to determine the melting temperature of SPAs and to examine the synergistic effects of antioxidants, including SPAs. [69].” Avoid this practice and remove all unnecessary references

7.      In conclusion add more numerical data from results

8.      The percentage purity and company of all reagents/chemicals utilized must be reported..

9.      There are so many grammatical, spelling and formatting mistakes in manuscript. I can’t mentioned here all of it. The whole manuscript must be cross-checked thoroughly for English editing, grammatical, spelling mistakes, and syntax errors.

Author Response

Dear,

Very kind for reviewing this research. We have attached the responses to your comments. We have answered all of them and, as expected, made all the corrections.

1. The novelty of this work was not specified; authors should discuss the novelty of their work in the introduction section.
2. In abstract correct this sentence, “Cyanox 1790 is a SPA that, although it is not a food additive, but polymeric, could be present in food that is stored in containers made of some type of polymer.”

R/ Thank you for reviewing this research. This was fixed.

3. There are many spelling mistakes in manuscript even in abstract too. I can’t mentioned here all of them, like, bottlesranged, Mostrado, levelis and many maore. Athors advised to revised carefuly and consult native English speaker. Also correct the formatting errors.

R/ Thank you for reviewing this research. We have made the corrections

4. Sequencing of abstract sentences is also not appropriate

R/ Thank you for reviewing this research. We have made the corrections

5. 5.In introduction section cite these articles on bottled water and water contaminants, https://doi.org/10.1080/03067319.2020.1846732,Inorganic Chemistry Communications 145 (2022) 110008, Surfaces and Interfaces 34 (2022) 102324.

R/ Thank you for reviewing this research. We have made the incluision

6. 6.Authors add many references unnecessarily like, “The relative standard deviation (RSD) and LOD for the determination of SPA by HPLC are both less than 10%.[3], [66]–[68] in matrices with low[42],  [64], [65]to complexity of [3], [66]–[68]chemical content. Differential heat scanning (DSCs) has been used to determine the melting temperature of SPAs and to examine the synergistic effects of antioxidants, including SPAs. [69].” Avoid this practice and remove all unnecessary references

R/ Thank you for reviewing this research. We have made the corrections

7. In conclusion add more numerical data from results

R/ Thank you for reviewing this research. We have made the corrections

8. The percentage purity and company of all reagents/chemicals utilized must be reported.

R/ Thank you for reviewing this research. We have made the corrections

9. There are so many grammatical, spelling and formatting mistakes in manuscript. I can’t mentioned here all of it. The whole manuscript must be cross-checked thoroughly for English editing, grammatical, spelling mistakes, and syntax errors.

R/ Thank you for reviewing this research. We have made the corrections

Reviewer 3 Report

Identification and quantification of the synthetic phenolic antioxidant 1,3,5-Tris (4-tert-butyl-3-hydroxy-2,6-dimethyl benzyl)–1,3,5-triazine-2,4,6-(1H,3H,5H)-trione (Cyanox 1790) in bottled water in Colombia

Overall comments:

CYANOX® 1790 is one of synthetic phenolic antioxidants which is used as an ingredient in plastics and can be presented in drinking water and food through direct contact. The manuscript of the article was very confusingly presented, with a lot of mistakes, many uses of Spanish perhaps. I dimly understand that this study appears to have been conducted to evaluate the analysis of Cyanox 1790 in drinking water and in plastic bottles. The analytical methods were HPLC-MS (perhaps for the analysis of Cyanox 1790 in water), DSC and FTIR (for characterization of plastic samples). Research results on the parameters of the analytical method and analysis of Cyanox 1790 in drinking water. Analysis of water samples contained in plastic bottles showed that Cyanox 1790 content increased following the time due to migration from plastic to water.

Overall, this study was designed and conducted quite simply. The number of samples is not much, including: 6 samples of plastic bottles and analyzed over time up to 90 days. The study did not use internal standards. The results are lightly argued.

Questions:

1.     Why is bottled water stored at 40 ^oC? Normally the storage temperature is at a cold temperature. Are the water samples taken on the first day of sampling as fresh from the bottle on day 0, or have been placed in storage before?

2.     Why does the study use 5 analysts? Are 5 people doing it in the same lab or in 5 different labs?

3.     Please explain why DSC was used in this study? DSC for calorimeter.

Specific comments:

1.     The abstract section should be rewritten after all manuscripts are completely revised. The sentences from lines 16-19 should not include.

2.     The introduction section also needs to be rewritten to separate into different paragraphs. In which many cited documents are used, the author considers the necessity to use cited documents. Make figure 1 smaller. The research objectives are presented in a confusing manner. Is research done on interday and intraday calibration curves? Is Interday within day?

3.     The materials and methods section does not cover sample preparation and treatment methods. Re-present the sampling section because it is not clear how to do the steps? How to transport samples from storage to laboratory? What is high resolution SPE in line 181?

4.     The results need to be rewritten. The section titles are ambiguous. Please explain how experimental average and theoretical concentration values are calculated in Figure 3. People usually use one axis as concentration and one axis as peak area. The study did not determine recovery via SPE. Is the repeatability with n=3 and the reproducibility performed with n=5? The standard and bottled charts in Figures 5 and 6 should be superimposed.

The manuscript should clarify whether this study analyzes plastic bottles or water in plastic bottles or both. It is also necessary to clarify where to analyze plastic and where to analyze water. Unit measurement values need to be standardized, for example in water use mg/L instead of mg/kg.

5.     The conclusion has been revised to be more quantitative.

6.     The manuscript has so many errors that I can't list them all, including typos, translation errors, typographical errors, and presentation errors. Many places do not understand. Why many long spaces? Many merged words.

7.     References also need to be in the same format and carefully checked.

Conclusions:

In general, the manuscript is not well presented. The manuscript must be completely revised and re-submitted.

Author Response

Dear,

Very kind for reviewing this research. We have attached the responses to your comments. We have answered all of them and, as expected, made all the corrections.

1. Why is bottled water stored at 40 ^oC? Normally the storage temperature is at a cold temperature. Are the water samples taken on the first day of sampling as fresh from the bottle on day 0, or have been placed in storage before?

R/ Thank you for reviewing this research. This city has a large storage cellar where all the water drinks are stored. After this deposit, the different employees, through their logistics, make the distributions to supermarkets, stores, etc. This warehouse does not have a cold storage system. The temperature there is 40 C. For this reason, in our research, we have worked with the typical temperature of this winery. This is a real experiment. This part will be explained in more detail in this document.

The results of the measurements of the samples known as Zero (0) were not placed in table 3. But now, these results have been explained in the body of the text. These zero (0) samples were placed in the warehouse under the same conditions as all the samples at 40 C. That same day they were sampled to determine the cyanox concentration, day zero.

2. Why does the study use 5 analysts? Are 5 people doing it in the same lab or in 5 different labs?

R/ Thank you for reviewing this research. This Five people perform the analyzes in the same laboratory. The objective is to know the variability of each of them and to be able to understand their impact on the measurements. We have explained this a bit in the methodology.

3. Please explain why DSC was used in this study? DSC for calorimeter.

R/ Thank you for reviewing this research. The DSC is a colorimetric test. We have this equipment in our facilities. We have used the equipment to determine the melting point. We wanted to confirm if this Cyanox was well separated or not. To know if we could have traces of microplastic in the SPE extract. Since the bottle that contains the water is made of plastic, we wanted to rule out the presence of these microplastics. The results showed us the melting point of Cyanox, ruling out the existence of microplastics.

Specific comments:

1. The abstract section should be rewritten after all manuscripts are completely revised. The sentences from lines 16-19 should not include.

R/ Thank you for reviewing this research. We have made the corrections

2. The introduction section also needs to be rewritten to separate into different paragraphs. We have made the corrections. In which many cited documents are used, the author considers the necessity to use cited documents. Make figure 1 smaller. We have made the corrections. The research objectives are presented in a confusing manner. Is research done on interday and intraday calibration curves? Yes. Is Interday within day? interday day was on different days and intraday the same day.

R/ Thank you for reviewing this research. We have made the corrections

3. The materials and methods section does not cover sample preparation and treatment methods (We have made the corrections). Re-present the sampling section because it is not clear how to do the steps? (We have made the corrections). How to transport samples from storage to laboratory? (We have made the corrections). What is high resolution SPE in line 181? (We have made the corrections. The word resolution was placed in the wrong way).

3. The results need to be rewritten. The section titles are ambiguous. Please explain how experimental average and theoretical concentration values are calculated in Figure 3 (Now we have explained these in the methodology section section 2.2). People usually use one axis as concentration and one axis as peak area. The study did not determine recovery via SPE.

Is the repeatability with n=3 and the reproducibility performed with n=5? No. In the repeatability, n=5, and the reproducibility, n=5. This is explained in the methodology.

The standard and bottled charts in Figures 5 and 6 should be superimposed. Done

The manuscript should clarify whether this study analyzes plastic bottles or water in plastic bottles or both (Now we have explained these in the methodology section section 2.2. Our goal is to test the water. The plastic bottle is not interesting to analyze for now). It is also necessary to clarify where to analyze plastic and where to analyze water. Unit measurement values need to be standardized, for example in water use mg/L instead of mg/kg (We have made the corrections)

4. The conclusion has been revised to be more quantitative.

R/ Thank you for reviewing this research. We have made the corrections

6. The manuscript has so many errors that I can't list them all, including typos, translation errors, typographical errors, and presentation errors. Many places do not understand. Why many long spaces? Many merged words. R/ Thank you for reviewing this research. We have made the corrections

7. References also need to be in the same format and carefully checked.

R/ Thank you for reviewing this research. We have made the corrections

Round 2

Reviewer 1 Report

Accepted in the present form.

Author Response

Dear

Thank you for reviewing this investigation.

We are very grateful

Kind Regards

Reviewer 2 Report

Accept

Author Response

Dear

Thank you for reviewing this investigation.

We are very grateful

Kind Regards

Reviewer 3 Report

This manuscript has been revised following the reviewer's comment.

I remain only one suggestion for the title of manuscript. It should delete the "1,3,5-tris[(4- 3 tert-butyl-3-hydroxy-2,6-dimethylphenyl)methyl]-1,3,5-tria4 zinane-2,4,6-trione". The title become: "Quantification of the synthetic phenolic antioxidant Cyanox 1790 in bottled water by SPE-HPLC/MS/MS and determination of the impact of the use of recycled packaging in its generation".

Author Response

Dear

Thank you for your suggestion.

We will place this new title.

Kind Regards