Pub Date : 2023-05-25DOI: 10.30744/brjac.2179-3425.ar-106-2022
Gabriela Alcantara, Giovanna Spíndola, W. Melchert
Coffee contains different volatile and non-volatile compounds, which are responsible for its characteristic flavor and aroma attributes. The extraction of non-volatile compounds from high-quality and traditional coffee by different methods was evaluated to determine the chemical compounds that discriminate between coffees types. Standard methods of preparing the coffee drink by consumers were evaluated. Method A corresponded to boiling water with coffee, and method B to the strained coffee method. Extraction with different solvents did not distinguish the compounds chosen as markers for coffees. In addition to being non-toxic and low-cost, water was the most suitable solvent, conforming to the principles of green chemistry while enabling direct comparison with sensory analysis. The total dissolved solids, percentage extraction, and non-volatile compounds were quantified to select the most satisfactory extraction method. The TDS value ranged from 1.7 to 3 between methods and coffee types, and the extraction percentage ranged from 25 to 45%. Significant differences in the extracts obtained using methods A and B high-quality versus traditional coffees were detected using the Student’s t-test. Although method A extracted the chemical compounds in more substantial amounts, method B was also efficient in extracting the compounds and was easily executed given its similarity to the usual way of preparing coffee beverages used by consumers. The evaluated non-volatile compounds were identified in both high-quality and traditional coffee samples. In the chosen extraction method (method B), the average concentrations in mg 100 g-1 of the sample found for the compounds were: 5-hydroxymethylfurfural (11±0.5), 3,4-hydroxybenzoic acid (62±4), catechin (58±5), 4-hydroxybenzoic acid (58±2), caffeine (1152±44), chlorogenic acid (598±23), caffeic acid (0.7±0.1), and gallic acid (3±0.2).
{"title":"Extraction of Non-Volatile Chemical Compounds in High-Quality and Traditional Coffee","authors":"Gabriela Alcantara, Giovanna Spíndola, W. Melchert","doi":"10.30744/brjac.2179-3425.ar-106-2022","DOIUrl":"https://doi.org/10.30744/brjac.2179-3425.ar-106-2022","url":null,"abstract":"Coffee contains different volatile and non-volatile compounds, which are responsible for its characteristic flavor and aroma attributes. The extraction of non-volatile compounds from high-quality and traditional coffee by different methods was evaluated to determine the chemical compounds that discriminate between coffees types. Standard methods of preparing the coffee drink by consumers were evaluated. Method A corresponded to boiling water with coffee, and method B to the strained coffee method. Extraction with different solvents did not distinguish the compounds chosen as markers for coffees. In addition to being non-toxic and low-cost, water was the most suitable solvent, conforming to the principles of green chemistry while enabling direct comparison with sensory analysis. The total dissolved solids, percentage extraction, and non-volatile compounds were quantified to select the most satisfactory extraction method. The TDS value ranged from 1.7 to 3 between methods and coffee types, and the extraction percentage ranged from 25 to 45%. Significant differences in the extracts obtained using methods A and B high-quality versus traditional coffees were detected using the Student’s t-test. Although method A extracted the chemical compounds in more substantial amounts, method B was also efficient in extracting the compounds and was easily executed given its similarity to the usual way of preparing coffee beverages used by consumers. The evaluated non-volatile compounds were identified in both high-quality and traditional coffee samples. In the chosen extraction method (method B), the average concentrations in mg 100 g-1 of the sample found for the compounds were: 5-hydroxymethylfurfural (11±0.5), 3,4-hydroxybenzoic acid (62±4), catechin (58±5), 4-hydroxybenzoic acid (58±2), caffeine (1152±44), chlorogenic acid (598±23), caffeic acid (0.7±0.1), and gallic acid (3±0.2).","PeriodicalId":9115,"journal":{"name":"Brazilian Journal of Analytical Chemistry","volume":" ","pages":""},"PeriodicalIF":0.7,"publicationDate":"2023-05-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43809204","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-05-25DOI: 10.30744/brjac.2179-3425.tn-11-2023
Javier Silva, M. Pistón
Biorsorbents can be used to pack minicolumns for the preconcentration of trace elements and thus improve the detection limits of some techniques. A biosorbent is efficient when presents binding sites as carbonyls, amines, and carboxylic groups, among others. Thus, natural materials as the sisal fiber (Agave sisalana) may be a good candidate. Sisal fiber demonstrated good performance for Cu preconcentration when it was impregnated with alizarine fluorine blue (AFB). However, very good results were reported for the first time by our group with this column, without the use of additional reagents for both, Mn and Cu determinations in water samples by using microwave plasma atomic emission spectroscopy (MP AES). In this paper a comparison of the sisal fiber preparation with and without impregnation with AFB is presented and discussed in terms of the figures of merit, including precision, trueness, limits of detection and quantification. In addition to that, the number of determinations without the need of replacement of the solid phase was evaluated. Results demonstrated that the impregnation of sisal fiber with AFB does not leads to an improvement in the analytical performance. Analytical Greenness Metric Approach (AGREE) was used to evaluate the greenness of both methods and results obtained were similar. Despite this, the method without impregnation of the fiber has some remarkable advantages, that contributes to Green Analytical Chemistry (GAC), related to the lifetime of the sorbent, not considered in the AGREE tool.
{"title":"Evaluations of Sisal Fiber as Biosorbent for online Preconcentration and Determination of Cu and Mn coupled to MP AES using the Analytical Greenness Metric Approach","authors":"Javier Silva, M. Pistón","doi":"10.30744/brjac.2179-3425.tn-11-2023","DOIUrl":"https://doi.org/10.30744/brjac.2179-3425.tn-11-2023","url":null,"abstract":"Biorsorbents can be used to pack minicolumns for the preconcentration of trace elements and thus improve the detection limits of some techniques. A biosorbent is efficient when presents binding sites as carbonyls, amines, and carboxylic groups, among others. Thus, natural materials as the sisal fiber (Agave sisalana) may be a good candidate. Sisal fiber demonstrated good performance for Cu preconcentration when it was impregnated with alizarine fluorine blue (AFB). However, very good results were reported for the first time by our group with this column, without the use of additional reagents for both, Mn and Cu determinations in water samples by using microwave plasma atomic emission spectroscopy (MP AES). In this paper a comparison of the sisal fiber preparation with and without impregnation with AFB is presented and discussed in terms of the figures of merit, including precision, trueness, limits of detection and quantification. In addition to that, the number of determinations without the need of replacement of the solid phase was evaluated. Results demonstrated that the impregnation of sisal fiber with AFB does not leads to an improvement in the analytical performance. Analytical Greenness Metric Approach (AGREE) was used to evaluate the greenness of both methods and results obtained were similar. Despite this, the method without impregnation of the fiber has some remarkable advantages, that contributes to Green Analytical Chemistry (GAC), related to the lifetime of the sorbent, not considered in the AGREE tool.","PeriodicalId":9115,"journal":{"name":"Brazilian Journal of Analytical Chemistry","volume":" ","pages":""},"PeriodicalIF":0.7,"publicationDate":"2023-05-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"45660863","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-05-25DOI: 10.30744/brjac.2179-3425.tn-113-2022
Saphire Dias, Aline Oliveira, I. Gaubeur, C. Nomura, J. Naozuka
For physiological functions development and a healthy life maintenance, a balanced diet, containing carbohydrates, proteins, and lipids, should be practiced, and consumed. The proteins should be highlighted, since are essential macronutrients for cell growth and repair mechanisms in our body. There is an increase in the protein sources consumption, mainly by athletes, aiming an increase of muscle mass and to avoid muscle hypertrophy. Although animal proteins exhibit high digestibility, animal foods can not be accessible and widely consumed, due to high cost or lifestyle choice (vegetarians and vegans). In these sceneries, scientists and food industry are constantly searching for alternative proteins, such as plant and fungi proteins. In view of these information, extraction procedures are proposed to proteins fractionation. However, these procedures must be done to exhaustion to guarantee the acquisition of quantitative values. Therefore, the aims of this work were evaluated the protein distribution in edible mushrooms and optimized the sequential protein extraction procedure to obtain total concentration of albumin, globulin, prolamin and glutelin in edible mushrooms, evidencing the need to carry out extraction procedures until exhaustion to adequately attribute nutritional value to edible mushrooms (pink oyster, shiitake, portobello and champignon). The optimized extraction conditions (extractant, time, concentration, number of extractions) were as follows (H2O, 30 min, ---, 3); (NaCl, 15 min, 0.25 mol L-1, 1); (ethanol, 15 min, 50% (v v-1), 1); (NaOH, 60 min, 0.25 mol L-1, 8) for albumin, globulin, prolamin and glutelin extraction. The champignon mushrooms presented all protein group concentrations below LOD and LOQ. The portobello presented the lowest total proteins concentration. The pink oyster mushroom is the species with the highest concentration of albumin and glutelin as well as total protein concentration 4.7 times higher than shiitake mushroom, which is one of the most consumed mushroom species, showing that this exotic species can be promising mainly due to nutritional characteristics and protein source.
{"title":"Optimization of the Protein Sequential Extraction for Quantitative Determination of Albumins, Globulins, Prolamins and Glutelins in Edible Mushrooms","authors":"Saphire Dias, Aline Oliveira, I. Gaubeur, C. Nomura, J. Naozuka","doi":"10.30744/brjac.2179-3425.tn-113-2022","DOIUrl":"https://doi.org/10.30744/brjac.2179-3425.tn-113-2022","url":null,"abstract":"For physiological functions development and a healthy life maintenance, a balanced diet, containing carbohydrates, proteins, and lipids, should be practiced, and consumed. The proteins should be highlighted, since are essential macronutrients for cell growth and repair mechanisms in our body. There is an increase in the protein sources consumption, mainly by athletes, aiming an increase of muscle mass and to avoid muscle hypertrophy. Although animal proteins exhibit high digestibility, animal foods can not be accessible and widely consumed, due to high cost or lifestyle choice (vegetarians and vegans). In these sceneries, scientists and food industry are constantly searching for alternative proteins, such as plant and fungi proteins. In view of these information, extraction procedures are proposed to proteins fractionation. However, these procedures must be done to exhaustion to guarantee the acquisition of quantitative values. Therefore, the aims of this work were evaluated the protein distribution in edible mushrooms and optimized the sequential protein extraction procedure to obtain total concentration of albumin, globulin, prolamin and glutelin in edible mushrooms, evidencing the need to carry out extraction procedures until exhaustion to adequately attribute nutritional value to edible mushrooms (pink oyster, shiitake, portobello and champignon). The optimized extraction conditions (extractant, time, concentration, number of extractions) were as follows (H2O, 30 min, ---, 3); (NaCl, 15 min, 0.25 mol L-1, 1); (ethanol, 15 min, 50% (v v-1), 1); (NaOH, 60 min, 0.25 mol L-1, 8) for albumin, globulin, prolamin and glutelin extraction. The champignon mushrooms presented all protein group concentrations below LOD and LOQ. The portobello presented the lowest total proteins concentration. The pink oyster mushroom is the species with the highest concentration of albumin and glutelin as well as total protein concentration 4.7 times higher than shiitake mushroom, which is one of the most consumed mushroom species, showing that this exotic species can be promising mainly due to nutritional characteristics and protein source.","PeriodicalId":9115,"journal":{"name":"Brazilian Journal of Analytical Chemistry","volume":" ","pages":""},"PeriodicalIF":0.7,"publicationDate":"2023-05-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43134693","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-05-19DOI: 10.30744/brjac.2179-3425.ar-112-2022
M. Marques, P. Ferreira, Tháles A. Pereira, Alessandra Sussulini
The instrumental aspect employed in metabolomic and lipidomic strategies has been well developed as of the past two decades, allowing large-scale analysis with high sensitivity and reproducibility, while statistical analysis and bioinformatics are emerging fields for data interpretation. Conversely, sample preparation is an important element that, if not optimized, has an impact on metabolome profiling and may result in erroneous and biased biological interpretation, remaining the bottleneck of the metabolomics workflow. Therefore, this work presents an evaluation of liquid-liquid extraction protocols for blood serum samples aiming at metabolomics and lipidomics analysis using liquid chromatography coupled to mass spectrometry (LC-MS). The Bligh & Dyer, Matyash and SIMPLEX protocols were investigated and the findings demonstrate that the composition of the solvents in each approach has a considerable impact on the putatively identified lipids, as well as the average concentration of extracted proteins. The study of the aqueous fraction, however, revealed no statistically significant variations in the identified metabolites. Hence, the optimization of the sample preparation step is crucial for biomolecules profiling and must be carefully considered in accordance with the objectives of the research and the chosen biological matrices.
{"title":"The Importance of Sample Preparation for Omics Analysis: Which Extraction Method is the most Suited for my Biological Question?","authors":"M. Marques, P. Ferreira, Tháles A. Pereira, Alessandra Sussulini","doi":"10.30744/brjac.2179-3425.ar-112-2022","DOIUrl":"https://doi.org/10.30744/brjac.2179-3425.ar-112-2022","url":null,"abstract":"The instrumental aspect employed in metabolomic and lipidomic strategies has been well developed as of the past two decades, allowing large-scale analysis with high sensitivity and reproducibility, while statistical analysis and bioinformatics are emerging fields for data interpretation. Conversely, sample preparation is an important element that, if not optimized, has an impact on metabolome profiling and may result in erroneous and biased biological interpretation, remaining the bottleneck of the metabolomics workflow. Therefore, this work presents an evaluation of liquid-liquid extraction protocols for blood serum samples aiming at metabolomics and lipidomics analysis using liquid chromatography coupled to mass spectrometry (LC-MS). The Bligh & Dyer, Matyash and SIMPLEX protocols were investigated and the findings demonstrate that the composition of the solvents in each approach has a considerable impact on the putatively identified lipids, as well as the average concentration of extracted proteins. The study of the aqueous fraction, however, revealed no statistically significant variations in the identified metabolites. Hence, the optimization of the sample preparation step is crucial for biomolecules profiling and must be carefully considered in accordance with the objectives of the research and the chosen biological matrices.","PeriodicalId":9115,"journal":{"name":"Brazilian Journal of Analytical Chemistry","volume":" ","pages":""},"PeriodicalIF":0.7,"publicationDate":"2023-05-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43548632","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-05-19DOI: 10.30744/brjac.2179-3425.rv-136-2022
Hanna de Sá, E. D. dos Santos, Samara Carvalho, Rafaela Nunes, G. Canuto
Metabolomics has become a prominent area within the omics sciences and allows an understanding of complex biological systems. Among several areas of knowledge, the study of microorganisms (microbial metabolomics) has received attention. Due to the many species of microorganisms and their high metabolic complexity, many challenges are involved in metabolomics workflow. Careful experimental design and execution of the experiments will provide reliable results, allowing correct biological interpretation. This review presents the fundamentals of metabolomics and workflow, focusing on the description of the steps and analytical strategies applied to microbial sample preparation, highlighting the current challenges in sample handling. In addition, the state of the art of analytical technologies based on separation techniques hyphenated to mass spectrometry and applications in microbial metabolomics are presented.
{"title":"Fundamentals and Analytical Strategies for Metabolomics Workflow: An Overview and Microbial Applications","authors":"Hanna de Sá, E. D. dos Santos, Samara Carvalho, Rafaela Nunes, G. Canuto","doi":"10.30744/brjac.2179-3425.rv-136-2022","DOIUrl":"https://doi.org/10.30744/brjac.2179-3425.rv-136-2022","url":null,"abstract":"Metabolomics has become a prominent area within the omics sciences and allows an understanding of complex biological systems. Among several areas of knowledge, the study of microorganisms (microbial metabolomics) has received attention. Due to the many species of microorganisms and their high metabolic complexity, many challenges are involved in metabolomics workflow. Careful experimental design and execution of the experiments will provide reliable results, allowing correct biological interpretation. This review presents the fundamentals of metabolomics and workflow, focusing on the description of the steps and analytical strategies applied to microbial sample preparation, highlighting the current challenges in sample handling. In addition, the state of the art of analytical technologies based on separation techniques hyphenated to mass spectrometry and applications in microbial metabolomics are presented.","PeriodicalId":9115,"journal":{"name":"Brazilian Journal of Analytical Chemistry","volume":" ","pages":""},"PeriodicalIF":0.7,"publicationDate":"2023-05-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46837926","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-05-15DOI: 10.30744/brjac.2179-3425.ar-129-2022
P. Mello, G. Bitencourt, T. Berón, Aline Müller
Dietary supplements have been used to overcome nutritional deficiencies and the knowledge concerning essential and non-essential elements is an important issue. In this work the suitability of microwave-induced plasma optical emission spectrometry (MIP OES) for the determination of essential and non-essential elements in dietary supplements was evaluated. Twelve dietary supplement samples of several classifications (vitamins/minerals, minerals, amino acids, and botanicals) were digested in their whole form for determination of essential (Ca, Co, Cu, Fe, K, Mg, Mn, Mo, Na, and Zn) and non-essential (Ag, Al, B, Ba, Be, Cd, Cr, La, Li, Ni, Pb, Sr, and V) elements by MIP OES. Potential non-spectral interferences by common concomitants (C, S, K, Na, and Ca) were evaluated, as well as those by residual acidity of digests. The study of non-spectral interferences showed that a signal suppression effect is observed with higher concentrations of Ca, Na, and K. Relatively good robustness was observed considering the presence of C and S, as well as residual HNO3. The limits of quantification (LOQs) were dependent on the sample mass used for decomposition (from 0.6 to 1.6 g in the commercial product) and on the minimum dilution factor. From the results, there was a prevalence of essential and non-essential elements in vitamins and minerals, minerals, and botanicals-based dietary supplements, whereas lower concentrations were found in the dietary supplements based on amino acids. All elements were in a concentration below the recommended dietary allowances (RDAs), exception for those with the concentration intentionally higher. Accuracy of results by MIP OES was evaluated by using standard reference materials (SRM) NIST 1572 and NIST 1575a. In addition, results showed no statistical difference by comparison with those by ICP OES. MIP OES proved to be a suitable technique for the determination of metals in dietary supplements, being a feasible alternative for the quality control of these products.
{"title":"Determination of Essential and Non-Essential Elements in Dietary Supplements by Microwave-Induced Plasma Optical Emission Spectrometry: Method Development and Study of Non-Spectral Interferences","authors":"P. Mello, G. Bitencourt, T. Berón, Aline Müller","doi":"10.30744/brjac.2179-3425.ar-129-2022","DOIUrl":"https://doi.org/10.30744/brjac.2179-3425.ar-129-2022","url":null,"abstract":"Dietary supplements have been used to overcome nutritional deficiencies and the knowledge concerning essential and non-essential elements is an important issue. In this work the suitability of microwave-induced plasma optical emission spectrometry (MIP OES) for the determination of essential and non-essential elements in dietary supplements was evaluated. Twelve dietary supplement samples of several classifications (vitamins/minerals, minerals, amino acids, and botanicals) were digested in their whole form for determination of essential (Ca, Co, Cu, Fe, K, Mg, Mn, Mo, Na, and Zn) and non-essential (Ag, Al, B, Ba, Be, Cd, Cr, La, Li, Ni, Pb, Sr, and V) elements by MIP OES. Potential non-spectral interferences by common concomitants (C, S, K, Na, and Ca) were evaluated, as well as those by residual acidity of digests. The study of non-spectral interferences showed that a signal suppression effect is observed with higher concentrations of Ca, Na, and K. Relatively good robustness was observed considering the presence of C and S, as well as residual HNO3. The limits of quantification (LOQs) were dependent on the sample mass used for decomposition (from 0.6 to 1.6 g in the commercial product) and on the minimum dilution factor. From the results, there was a prevalence of essential and non-essential elements in vitamins and minerals, minerals, and botanicals-based dietary supplements, whereas lower concentrations were found in the dietary supplements based on amino acids. All elements were in a concentration below the recommended dietary allowances (RDAs), exception for those with the concentration intentionally higher. Accuracy of results by MIP OES was evaluated by using standard reference materials (SRM) NIST 1572 and NIST 1575a. In addition, results showed no statistical difference by comparison with those by ICP OES. MIP OES proved to be a suitable technique for the determination of metals in dietary supplements, being a feasible alternative for the quality control of these products.","PeriodicalId":9115,"journal":{"name":"Brazilian Journal of Analytical Chemistry","volume":" ","pages":""},"PeriodicalIF":0.7,"publicationDate":"2023-05-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"47297739","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-05-15DOI: 10.30744/brjac.2179-3425.rv-07-2023
L. Souza
Global plastic pollution is a serious problem that is increasing over the years since millions of tons of plastics end up in the environment. These plastics are fragmented due to sunlight radiation, biodegradation, and other environmental factors leading to small debris which can be transformed into microplastics and nanoplastics. Due to their small size and high surface area, these materials can be easily absorbed by organisms besides being able to adsorb toxic pollutants. Considering these issues, studies about their toxicity and fate in the environment are of great importance, however, the success of these studies depends on the methods of sampling, sample preparation, and also analysis, which need to be developed and improved. Thus, the current review proposes an integrated approach of methodologies of sampling, sample preparation, and analysis of solid and aqueous samples with microplastics and nanoplastics besides discussing the challenges and new methodologies for microplastics and nanoplastics analysis.
{"title":"The Emerging of Microplastic and Nanoplastic as Pollutants and their Characterization and Analysis","authors":"L. Souza","doi":"10.30744/brjac.2179-3425.rv-07-2023","DOIUrl":"https://doi.org/10.30744/brjac.2179-3425.rv-07-2023","url":null,"abstract":"Global plastic pollution is a serious problem that is increasing over the years since millions of tons of plastics end up in the environment. These plastics are fragmented due to sunlight radiation, biodegradation, and other environmental factors leading to small debris which can be transformed into microplastics and nanoplastics. Due to their small size and high surface area, these materials can be easily absorbed by organisms besides being able to adsorb toxic pollutants. Considering these issues, studies about their toxicity and fate in the environment are of great importance, however, the success of these studies depends on the methods of sampling, sample preparation, and also analysis, which need to be developed and improved. Thus, the current review proposes an integrated approach of methodologies of sampling, sample preparation, and analysis of solid and aqueous samples with microplastics and nanoplastics besides discussing the challenges and new methodologies for microplastics and nanoplastics analysis.","PeriodicalId":9115,"journal":{"name":"Brazilian Journal of Analytical Chemistry","volume":" ","pages":""},"PeriodicalIF":0.7,"publicationDate":"2023-05-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"41512141","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-05-10DOI: 10.30744/brjac.2179-3425.ar-13-2023
Ívero de Sá, C. da Silva, A. R. Nogueira
Two methods were developed for the As and Cr species determination in different kinds of seafood, exploring the LC-ICP-MS potential and chemometric approach to define the extraction conditions. Adequates separation and sensitivity data by LC-ICP-MS were obtained with 0.01 mol L-1 (NH4)2HPO4 in 1% ethanol (pH 8.0) for arsenic, and 0.015 mol L-1 Na2SO4, 0.005 mol L-1 EDTA, and 0.005 mol L-1 NaH2PO4 (pH 7.0) for chromium. The Doehlert matrix and Box-Behnken design defined the ideal extraction conditions for arsenic and chromium species. For As extraction, the optimized conditions employed 0.1 g of sample and 30 mmol L-1 HNO3 at 90°C for 45 min, and Cr, 0.1 g of sample and 0.045 mol L-1 [EDTA] at 90°C for 40 min. Recoveries from 88 to 106% of arsenobetaine (AsB), arsenite [As(III)], dimethylarsinic acid (DMA), monomethylarsonic acid (MMA), arsenate [As(V)], Cr(III) and Cr(VI) were obtained for all evaluated samples. The limits of quantification provided by the proposed methods were 5.3; 52.1; 16.4; 2.8; 83.3; 113.8; 53.9 ng g-1 for AsB, As(III), DMA, MMA, As(V), Cr(III) and Cr(VI) respectively. The trueness was evaluated using certified reference materials and addition and recovery procedures. The sum of the species agreed with the total concentration of arsenic and chromium contents.
{"title":"Chemical Speciation of Arsenic and Chromium in Seafood by LC-ICP-MS","authors":"Ívero de Sá, C. da Silva, A. R. Nogueira","doi":"10.30744/brjac.2179-3425.ar-13-2023","DOIUrl":"https://doi.org/10.30744/brjac.2179-3425.ar-13-2023","url":null,"abstract":"Two methods were developed for the As and Cr species determination in different kinds of seafood, exploring the LC-ICP-MS potential and chemometric approach to define the extraction conditions. Adequates separation and sensitivity data by LC-ICP-MS were obtained with 0.01 mol L-1 (NH4)2HPO4 in 1% ethanol (pH 8.0) for arsenic, and 0.015 mol L-1 Na2SO4, 0.005 mol L-1 EDTA, and 0.005 mol L-1 NaH2PO4 (pH 7.0) for chromium. The Doehlert matrix and Box-Behnken design defined the ideal extraction conditions for arsenic and chromium species. For As extraction, the optimized conditions employed 0.1 g of sample and 30 mmol L-1 HNO3 at 90°C for 45 min, and Cr, 0.1 g of sample and 0.045 mol L-1 [EDTA] at 90°C for 40 min. Recoveries from 88 to 106% of arsenobetaine (AsB), arsenite [As(III)], dimethylarsinic acid (DMA), monomethylarsonic acid (MMA), arsenate [As(V)], Cr(III) and Cr(VI) were obtained for all evaluated samples. The limits of quantification provided by the proposed methods were 5.3; 52.1; 16.4; 2.8; 83.3; 113.8; 53.9 ng g-1 for AsB, As(III), DMA, MMA, As(V), Cr(III) and Cr(VI) respectively. The trueness was evaluated using certified reference materials and addition and recovery procedures. The sum of the species agreed with the total concentration of arsenic and chromium contents.","PeriodicalId":9115,"journal":{"name":"Brazilian Journal of Analytical Chemistry","volume":" ","pages":""},"PeriodicalIF":0.7,"publicationDate":"2023-05-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46246051","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-05-08DOI: 10.30744/brjac.2179-3425.ar-15-2023
Shivarampura Dushyantha, C. Siddaraju, N. Rajendraprasad
Four simple, precise, and cost-effective spectrophotometric methods were designed and validated to assess Dosulepin hydrochloride (DOS) in pure and dosage form. Two of them are direct UV (Methods A and B), and the other two are indirect visible spectrophotometric methods (Methods C and D). Method A is based on the measurement of the chromophoric activity of DOS in 0.1 M acetic acid (AcOH) at 300 nm. Method B involves the measurement of absorbance due to cerium (IV) left in excess after oxidizing DOS at 320 nm. The unreacted cerium (IV) was treated with a large excess of iron (II), which results in iron (III) and cerium (III). The surplus iron (II) forms a red colored complex with o-phenanthroline at a slightly higher pH was measured at 510 nm in Method C. In Method D the iron (III) formed in the redox reaction between unreacted cerium (IV) and iron (II) was made to form a red colour complex with thiocyanate and measured at 480 nm. The methods are applicable over good linear ranges of 1.0-80.0, 0.25-10.0, 0.5-8.0 and 0.50-10.0 µg mL-1 with actual molar absorptivity values of 2.07 × 103, 3.11 × 104, 4.08 × 104 and 3.7 × 104 L mol-1cm-1 for Method A, B, C and D, respectively. The validating parameters like limit of detection (LOD), quantification (LOQ), Sandell sensitivity and others have been reported. The methods proposed were successfully applied to quantify DOS in pharmaceuticals. The Fourier Transform Infrared (FT-IR) spectra of the post degradation DOS were studied, compared with that of pure drug and reached to the possible effect of degradation to stress by stability indicating property of Method A.
设计并验证了四种简单、准确、经济高效的分光光度法来评估纯盐酸多苏列平（DOS）和剂型。其中两种是直接紫外分光光度方法（方法A和B），另两种是间接可见分光光度分析方法（方法C和D）。方法A基于DOS在0.1M乙酸（AcOH）中在300nm处的发色活性的测量。方法B包括测量由于在320nm氧化DOS后剩余过量的铈（IV）引起的吸光度。用大量过量的铁（II）处理未反应的铈（IV），得到铁（III）和铈（III）。剩余的铁（II）在略高的pH下与邻菲罗啉形成红色络合物在方法C中在510nm处测量。在方法D中，使在未反应的铈（IV）和铁（Ⅱ）之间的氧化还原反应中形成的铁（III）与硫氰酸盐形成红色络合物，并在480nm处测量。该方法适用于1.0-80.0、0.25-10.0、0.5-8.0和0.50-10.0µg mL-1的良好线性范围，方法A、B、C和D的实际摩尔吸光系数分别为2.07×103、3.11×104、4.08×104和3.7×104 L mol-1cm-1。已经报道了检测限（LOD）、定量（LOQ）、Sandell灵敏度等验证参数。所提出的方法已成功应用于药品中DOS的定量。研究了降解后DOS的傅立叶变换红外光谱（FT-IR），并与纯药物进行了比较，通过方法A的稳定性指示特性，得出了降解应力的可能效果。
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Pub Date : 2023-04-11DOI: 10.30744/brjac.2179-3425.rv-126-2022
In recent decades, green analytical chemistry has received more attention due to the growing concern over environmental conservation and the use of non-renewable resources. Among the analytical techniques, liquid chromatography is the most widely used in quality control analysis of food, drugs, and clinical analysis among others, but it is also the technique that uses the largest amount of hazardous organic solvents and generates large volumes of waste. Therefore, strategies such as the miniaturization of chromatographic systems, the use of online sample preparation systems, and the replacement of hazardous organic solvents by green solvents have been applied to develop greener chromatographic methods. In this paper, strategies for greening methods and recent developments in green chromatography are presented. In addition, metrics for the proper evaluation of these methods are discussed.
{"title":"Recent Developments in Green Chromatography","authors":"","doi":"10.30744/brjac.2179-3425.rv-126-2022","DOIUrl":"https://doi.org/10.30744/brjac.2179-3425.rv-126-2022","url":null,"abstract":"In recent decades, green analytical chemistry has received more attention due to the growing concern over environmental conservation and the use of non-renewable resources. Among the analytical techniques, liquid chromatography is the most widely used in quality control analysis of food, drugs, and clinical analysis among others, but it is also the technique that uses the largest amount of hazardous organic solvents and generates large volumes of waste. Therefore, strategies such as the miniaturization of chromatographic systems, the use of online sample preparation systems, and the replacement of hazardous organic solvents by green solvents have been applied to develop greener chromatographic methods. In this paper, strategies for greening methods and recent developments in green chromatography are presented. In addition, metrics for the proper evaluation of these methods are discussed.","PeriodicalId":9115,"journal":{"name":"Brazilian Journal of Analytical Chemistry","volume":" ","pages":""},"PeriodicalIF":0.7,"publicationDate":"2023-04-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"45230735","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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