Pub Date : 2023-07-21DOI: 10.30744/brjac.2179-3425.ar-38-2023
Natália Viola, Brian Ferreira, L. Souza, M. Veiga
This study proposes a matrix separation procedure based on micellar-mediated extraction (cloud point extraction - CPE) for determining As, Cd, Pb, and Se (potential contaminants) in nickel alloy and steel samples. Structural characterization and qualitative analysis of Ni alloy were conducted on the nickel alloy using scanning electron microscopy–energy-dispersive X-ray spectroscopy (SEM-EDS). After sample decomposition, ammonium o,o-diethyl dithiophosphate (DDTP) was used to complex the analytes and Triton X-114 as a non-ionic surfactant in CPE for matrix separation and extraction. Methanol acidified with 0.1 mol L-1 HNO3 was added to the surfactant-rich phase before the analytes determination by graphite furnace atomic absorption spectrometry (GF AAS). Parameters such as pH, complexing agent and surfactant concentrations, acid medium, complexation time, and type of diluent were evaluated. The obtained results indicated that the ratio DDTP:As was 3:1, DDTP:Cd and DDTP:Pb was 2:1, and DDTP:Se was 1:1. The enrichment factors were 6, 8, 14, and 13, and limits of detection were 1.5, 0.06, 0.31 and 0.27 µg g-1 for As, Cd, Pb, and Se, respectively. The method was applied for As, Cd, Pb, and Se determination in Inconel 625 nickel alloy and standard reference materials (AISI 4340 Steel - SRM® 361, AISI 94B17 Steel - SRM® 362, Chromium-Vanadium Steel - SRM® 363, and Nickel Alloy UNS - SRM® 864). Analyte recoveries lay above 88%, and relative standard deviations were lower than 5%. Application of cloud point extraction for matrix separation allowed the determination of low concentrations of As, Cd, Pb, and Se, constituting an environmentally friendly method.
{"title":"Systematic Study for Determining As, Pb, Cd, and Se in Steel and Nickel Alloy Samples by GF AAS: Circumventing Matrix Interference with Extraction Based on Micellar Separation","authors":"Natália Viola, Brian Ferreira, L. Souza, M. Veiga","doi":"10.30744/brjac.2179-3425.ar-38-2023","DOIUrl":"https://doi.org/10.30744/brjac.2179-3425.ar-38-2023","url":null,"abstract":"This study proposes a matrix separation procedure based on micellar-mediated extraction (cloud point extraction - CPE) for determining As, Cd, Pb, and Se (potential contaminants) in nickel alloy and steel samples. Structural characterization and qualitative analysis of Ni alloy were conducted on the nickel alloy using scanning electron microscopy–energy-dispersive X-ray spectroscopy (SEM-EDS). After sample decomposition, ammonium o,o-diethyl dithiophosphate (DDTP) was used to complex the analytes and Triton X-114 as a non-ionic surfactant in CPE for matrix separation and extraction. Methanol acidified with 0.1 mol L-1 HNO3 was added to the surfactant-rich phase before the analytes determination by graphite furnace atomic absorption spectrometry (GF AAS). Parameters such as pH, complexing agent and surfactant concentrations, acid medium, complexation time, and type of diluent were evaluated. The obtained results indicated that the ratio DDTP:As was 3:1, DDTP:Cd and DDTP:Pb was 2:1, and DDTP:Se was 1:1. The enrichment factors were 6, 8, 14, and 13, and limits of detection were 1.5, 0.06, 0.31 and 0.27 µg g-1 for As, Cd, Pb, and Se, respectively. The method was applied for As, Cd, Pb, and Se determination in Inconel 625 nickel alloy and standard reference materials (AISI 4340 Steel - SRM® 361, AISI 94B17 Steel - SRM® 362, Chromium-Vanadium Steel - SRM® 363, and Nickel Alloy UNS - SRM® 864). Analyte recoveries lay above 88%, and relative standard deviations were lower than 5%. Application of cloud point extraction for matrix separation allowed the determination of low concentrations of As, Cd, Pb, and Se, constituting an environmentally friendly method.","PeriodicalId":9115,"journal":{"name":"Brazilian Journal of Analytical Chemistry","volume":" ","pages":""},"PeriodicalIF":0.7,"publicationDate":"2023-07-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"45407081","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 : 2023-07-10DOI: 10.30744/brjac.2179-3425.interview.jszpunar
J. Szpunar
Joanna Szpunar graduated from the Warsaw University of Technology in 1986 and obtained her Ph.D. (1992) and D.Sc. (Habilitation) (2000) from the University of Warsaw. Since 1997, she works at the National Research Council of France (CNRS). In 2007, she obtained in Poland the title of professor of chemistry. She has broad experience in the field of mass spectrometry-based bio-inorganic speciation analysis and metallomics with a focus on the identification and quantification of trace element species in biological systems and in the chemistry of metal-biomolecule interactions. She is the co-author of a book and approximately 250 scientific publications in peer-reviewed international journals. Joanna Szpunar is a fellow of the Royal Society of Chemistry (UK) and has been, for many years, a member of the boards of Journal of Analytical Atomic Spectrometry' and Metallomics. She regularly gives invited lectures at international analytical chemistry meetings and was the chairperson of the European Winter Conference on Plasma Spectrochemistry (Kraków, Poland) in 2013. The investigations carried out under her supervision and/or with her active participation resulted in the identification of a number of molecular targets of metals in biological systems, as well as contribute to selenometabolomics and selenoproteomics studies in bacteria and plants. In recent years, her interests were broadened to the environmental fate of metal-containing nanoparticles and nanoplastics. She has supervised 12 Ph.D. theses and several post-doctoral fellows. Joanna Szpunar is the laureate of the 2013 Jerzy Fijalkowski Award of the Committee of Analytical Chemistry of the Polish Academy of Sciences and the 2017 European Award for Plasma Spectrochemistry. In recent years, Joanna Szpunar has been involved in collaboration with analytical chemists in Brazil, hosting graduate students from the University of Campinas and the Federal University of Pelotas in the laboratory at the Institute of Analytical Sciences (IPREM) in Pau afiliated with the CNRS, lecturing at the Federal University of Santa Maria and co-supervising a Ph.D. student with work carried out at the University of Pau and the Federal University of Pelotas.
{"title":"Joanna Szpunar, a great chemical researcher internationally recognized, kindly spoke to BrJAC","authors":"J. Szpunar","doi":"10.30744/brjac.2179-3425.interview.jszpunar","DOIUrl":"https://doi.org/10.30744/brjac.2179-3425.interview.jszpunar","url":null,"abstract":"Joanna Szpunar graduated from the Warsaw University of Technology in 1986 and obtained her Ph.D. (1992) and D.Sc. (Habilitation) (2000) from the University of Warsaw. Since 1997, she works at the National Research Council of France (CNRS). In 2007, she obtained in Poland the title of professor of chemistry. She has broad experience in the field of mass spectrometry-based bio-inorganic speciation analysis and metallomics with a focus on the identification and quantification of trace element species in biological systems and in the chemistry of metal-biomolecule interactions. She is the co-author of a book and approximately 250 scientific publications in peer-reviewed international journals. Joanna Szpunar is a fellow of the Royal Society of Chemistry (UK) and has been, for many years, a member of the boards of Journal of Analytical Atomic Spectrometry' and Metallomics. She regularly gives invited lectures at international analytical chemistry meetings and was the chairperson of the European Winter Conference on Plasma Spectrochemistry (Kraków, Poland) in 2013. The investigations carried out under her supervision and/or with her active participation resulted in the identification of a number of molecular targets of metals in biological systems, as well as contribute to selenometabolomics and selenoproteomics studies in bacteria and plants. In recent years, her interests were broadened to the environmental fate of metal-containing nanoparticles and nanoplastics. She has supervised 12 Ph.D. theses and several post-doctoral fellows. Joanna Szpunar is the laureate of the 2013 Jerzy Fijalkowski Award of the Committee of Analytical Chemistry of the Polish Academy of Sciences and the 2017 European Award for Plasma Spectrochemistry. In recent years, Joanna Szpunar has been involved in collaboration with analytical chemists in Brazil, hosting graduate students from the University of Campinas and the Federal University of Pelotas in the laboratory at the Institute of Analytical Sciences (IPREM) in Pau afiliated with the CNRS, lecturing at the Federal University of Santa Maria and co-supervising a Ph.D. student with work carried out at the University of Pau and the Federal University of Pelotas.","PeriodicalId":9115,"journal":{"name":"Brazilian Journal of Analytical Chemistry","volume":" ","pages":""},"PeriodicalIF":0.7,"publicationDate":"2023-07-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"41611986","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 : 2023-07-10DOI: 10.30744/brjac.2179-3425.editorial.women.chem.n40
M. D. da Veiga, M. D. G. Korn
Women's participation in science has been an increasingly relevant and discussed topic in recent decades. Throughout history, women have faced numerous barriers and challenges to enter and stand out in this field of knowledge. However, despite the difficulties, women have contributed significantly to scientific advancement in all areas. In Brazil, the discussion about the participation of women in science has been highlighted in national events around analytical chemistry and academia. Thus, some changes have been implemented to minimize the differences discussed herein. Today we see more and more women engaged in science, holding prominent positions as researchers, professors, and leaders in their fields. They exist in many scientific disciplines, including physics, chemistry, biology, mathematics, engineering, and technology. In addition, women have also been involved in emerging and interdisciplinary areas such as computer science, artificial intelligence, and biotechnology. It is crucial to promote gender equality in chemistry by providing an inclusive environment and encouraging the active participation of women. This can be achieved by implementing policies that promote equal opportunities, encouraging female role models and mentors, supporting women chemists' training and professional development, and valuing and recognizing their contributions. Women's participation in chemistry is essential to scientific advancement in this field. We bring unique perspectives, creativity, and skills to address chemical challenges and contribute to a more comprehensive understanding of chemical processes and their practical applications. Gender diversity in chemistry drives innovation and promotes a more prosperous and inclusive scientific environment. It is essential to provide equal opportunities, support, and encouragement for women to enter and thrive in academic careers in the exact sciences, thus strengthening female representation in this field and boosting scientific excellence. In this context, the BrJAC journal worked on organizing an issue dedicated to women researchers in the field of (bio)analytical chemistry. The central idea is to celebrate those female researchers who have worked hard and dedicatedly in analytical chemistry. The interview was with Dr. Joanna Szpunar from the National Research Council of France (CNRS). She talked about her career and experience as a prominent researcher in the spectroanalytical chemistry field. The point of view was with Dr. Maria Valnice Boldrin Zanoni from UNESP, who excels in electroanalytical chemistry and shares a new perspective on artificial photosynthesis technology. The Letter written by Dr. Quezia Cass from UFSCar presented us with text on separation techniques highlighting affinity selection mass spectrometry. The issue will also feature three reviews, eight articles, and three technical notes, all led by women in (bio)analytical chemistry. It is imperative to thank all the reviewers who particip
{"title":"Women in (Bio)Analytical Chemistry: Moving Towards Equity and Inclusion","authors":"M. D. da Veiga, M. D. G. Korn","doi":"10.30744/brjac.2179-3425.editorial.women.chem.n40","DOIUrl":"https://doi.org/10.30744/brjac.2179-3425.editorial.women.chem.n40","url":null,"abstract":"Women's participation in science has been an increasingly relevant and discussed topic in recent decades. Throughout history, women have faced numerous barriers and challenges to enter and stand out in this field of knowledge. However, despite the difficulties, women have contributed significantly to scientific advancement in all areas. In Brazil, the discussion about the participation of women in science has been highlighted in national events around analytical chemistry and academia. Thus, some changes have been implemented to minimize the differences discussed herein. Today we see more and more women engaged in science, holding prominent positions as researchers, professors, and leaders in their fields. They exist in many scientific disciplines, including physics, chemistry, biology, mathematics, engineering, and technology. In addition, women have also been involved in emerging and interdisciplinary areas such as computer science, artificial intelligence, and biotechnology. It is crucial to promote gender equality in chemistry by providing an inclusive environment and encouraging the active participation of women. This can be achieved by implementing policies that promote equal opportunities, encouraging female role models and mentors, supporting women chemists' training and professional development, and valuing and recognizing their contributions. Women's participation in chemistry is essential to scientific advancement in this field. We bring unique perspectives, creativity, and skills to address chemical challenges and contribute to a more comprehensive understanding of chemical processes and their practical applications. Gender diversity in chemistry drives innovation and promotes a more prosperous and inclusive scientific environment. It is essential to provide equal opportunities, support, and encouragement for women to enter and thrive in academic careers in the exact sciences, thus strengthening female representation in this field and boosting scientific excellence. In this context, the BrJAC journal worked on organizing an issue dedicated to women researchers in the field of (bio)analytical chemistry. The central idea is to celebrate those female researchers who have worked hard and dedicatedly in analytical chemistry. The interview was with Dr. Joanna Szpunar from the National Research Council of France (CNRS). She talked about her career and experience as a prominent researcher in the spectroanalytical chemistry field. The point of view was with Dr. Maria Valnice Boldrin Zanoni from UNESP, who excels in electroanalytical chemistry and shares a new perspective on artificial photosynthesis technology. The Letter written by Dr. Quezia Cass from UFSCar presented us with text on separation techniques highlighting affinity selection mass spectrometry. The issue will also feature three reviews, eight articles, and three technical notes, all led by women in (bio)analytical chemistry. It is imperative to thank all the reviewers who particip","PeriodicalId":9115,"journal":{"name":"Brazilian Journal of Analytical Chemistry","volume":" ","pages":""},"PeriodicalIF":0.7,"publicationDate":"2023-07-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46597649","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 : 2023-07-03DOI: 10.30744/brjac.2179-3425.tn-31-2023
Maria Alice Amaral, M. Fusinato, Michele da Cunha, Jean Paulo Coll, João Henrique Lacerda, P. S. Sanches Filho
Emerging contaminants (EC) can be harmful to human health and the environment, as many of these compounds are persistent, bioaccumulative, toxic and are not regulated. Drugs are part of this group, including hormones (estrone, β-estradiol) and sunscreens (oxybenzone and octocrylene) used in this study. The adsorption capacity of biochar generated from the pyrolysis of rice husks from the region of Pelotas-RS-Brazil was evaluated in this study. The objective was to characterize the biochar and evaluate its adsorbent potential in the removal of hormones and sunscreens. The characterization of biochar was carried out through surface area (BET), Zero charge point (ZPC), X-ray diffraction (XFR), fixed carbon, volatile, and ash. The effectiveness in removing ECs was evaluated by stirring rice husk pyrolysis biochar (RHPB) (0.2 g and 0.5 g) in synthetic aqueous solutions fortified with 10.0 µg L-1 of the analytes at 25 °C for 1 hour at 150 rpm. The RHPB was filtered off and the analytes were desorbed with acetone and dichloromethane (DCM) under ultrasound for 30 min. The extract was concentrated, derivatized by silylation, and analyzed by gas chromatography coupled to mass spectrometry (GC-MS). Biochar showed promising removal results, reaching values of 60.1% removal for β-estradiol, 59.4% for estrone, 44.6% for octocrylene and 37.4% for oxybenzone.
新出现的污染物(EC)可能对人类健康和环境有害，因为其中许多化合物具有持久性、生物蓄积性、毒性且不受管制。药物是这一组的一部分，包括激素(雌酮，β-雌二醇)和防晒霜(氧苯酮和八烯)在这项研究中使用。本研究对Pelotas-RS-Brazil地区稻壳热解产生的生物炭的吸附能力进行了评价。目的是表征生物炭并评估其在去除激素和防晒霜方面的吸附潜力。通过比表面积(BET)、零电荷点(ZPC)、x射线衍射(XFR)、固定碳、挥发分和灰分等指标对生物炭进行表征。稻壳热解生物炭(RHPB) (0.2 g和0.5 g)在添加10.0 μ g L-1分析物的合成水溶液中搅拌，在25°C、150 rpm下搅拌1小时，以评估其去除ECs的效果。过滤掉RHPB，超声下丙酮和二氯甲烷(DCM)解吸30 min，提取液浓缩，硅基化衍生，气相色谱-质谱联用(GC-MS)分析。生物炭对β-雌二醇的去除率为60.1%，对雌酮的去除率为59.4%，对八烯的去除率为44.6%，对氧苯酮的去除率为37.4%。
{"title":"Evaluation of the Adsorbent Potential of Biochar obtained by Pyrolysis to Remove Emerging Contaminants","authors":"Maria Alice Amaral, M. Fusinato, Michele da Cunha, Jean Paulo Coll, João Henrique Lacerda, P. S. Sanches Filho","doi":"10.30744/brjac.2179-3425.tn-31-2023","DOIUrl":"https://doi.org/10.30744/brjac.2179-3425.tn-31-2023","url":null,"abstract":"Emerging contaminants (EC) can be harmful to human health and the environment, as many of these compounds are persistent, bioaccumulative, toxic and are not regulated. Drugs are part of this group, including hormones (estrone, β-estradiol) and sunscreens (oxybenzone and octocrylene) used in this study. The adsorption capacity of biochar generated from the pyrolysis of rice husks from the region of Pelotas-RS-Brazil was evaluated in this study. The objective was to characterize the biochar and evaluate its adsorbent potential in the removal of hormones and sunscreens. The characterization of biochar was carried out through surface area (BET), Zero charge point (ZPC), X-ray diffraction (XFR), fixed carbon, volatile, and ash. The effectiveness in removing ECs was evaluated by stirring rice husk pyrolysis biochar (RHPB) (0.2 g and 0.5 g) in synthetic aqueous solutions fortified with 10.0 µg L-1 of the analytes at 25 °C for 1 hour at 150 rpm. The RHPB was filtered off and the analytes were desorbed with acetone and dichloromethane (DCM) under ultrasound for 30 min. The extract was concentrated, derivatized by silylation, and analyzed by gas chromatography coupled to mass spectrometry (GC-MS). Biochar showed promising removal results, reaching values of 60.1% removal for β-estradiol, 59.4% for estrone, 44.6% for octocrylene and 37.4% for oxybenzone.","PeriodicalId":9115,"journal":{"name":"Brazilian Journal of Analytical Chemistry","volume":" ","pages":""},"PeriodicalIF":0.7,"publicationDate":"2023-07-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"42267295","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 : 2023-07-03DOI: 10.30744/brjac.2179-3425.ar-16-2023
Úrsula Méndez-Mejía, M. Tenorio, M. Jiménez-Reyes, Rosa Rodríguez-Tomp
This study focused on the examination of six rock pictorial panels and a solitary figure from four archaeological sites in the Sierra de las Cacachilas (Sector A) in the Region del Cabo, Baja California Sur, Mexico. Scanning Electron Microscopy-energy dispersive X-ray spectroscopy was utilized to analyze tiny samples of the pictorial layers, patina, rocky supports, and natural pigments. The concentrations of C, Mg, Al, Si, P, S, K, Ca, Cr, Ti, Mn, and Fe were subjected to statistical methods and the samples were divided into various clusters. Iron and calcium compounds appear to be the primary constituents of the pictorial layers. The red pigment spectra obtained through Fourier-transform infrared spectroscopy revealed the presence of inorganic compounds and the likelihood of a flora-based composite as the binding agent. The minerals identified through X-ray diffraction in the rocky supports were determined to be intrusive igneous rocks. These findings are significant for the conservation and preservation of the artwork in the Sierra de las Cacachilas.
{"title":"Ancient Rock Paintings at Region del Cabo-BCS, Mexico: An Analytical Study","authors":"Úrsula Méndez-Mejía, M. Tenorio, M. Jiménez-Reyes, Rosa Rodríguez-Tomp","doi":"10.30744/brjac.2179-3425.ar-16-2023","DOIUrl":"https://doi.org/10.30744/brjac.2179-3425.ar-16-2023","url":null,"abstract":"This study focused on the examination of six rock pictorial panels and a solitary figure from four archaeological sites in the Sierra de las Cacachilas (Sector A) in the Region del Cabo, Baja California Sur, Mexico. Scanning Electron Microscopy-energy dispersive X-ray spectroscopy was utilized to analyze tiny samples of the pictorial layers, patina, rocky supports, and natural pigments. The concentrations of C, Mg, Al, Si, P, S, K, Ca, Cr, Ti, Mn, and Fe were subjected to statistical methods and the samples were divided into various clusters. Iron and calcium compounds appear to be the primary constituents of the pictorial layers. The red pigment spectra obtained through Fourier-transform infrared spectroscopy revealed the presence of inorganic compounds and the likelihood of a flora-based composite as the binding agent. The minerals identified through X-ray diffraction in the rocky supports were determined to be intrusive igneous rocks. These findings are significant for the conservation and preservation of the artwork in the Sierra de las Cacachilas.","PeriodicalId":9115,"journal":{"name":"Brazilian Journal of Analytical Chemistry","volume":" ","pages":""},"PeriodicalIF":0.7,"publicationDate":"2023-07-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49095932","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 : 2023-06-19DOI: 10.30744/brjac.2179-3425.ar-122-2022
Lana Pereira, Robson Brito, Kelly Dantas
The objective of this study was to determine and evaluate the bioaccessibility of Ca, Fe, Mg, and Mn in Apis mellifera and Melipona propolis samples. Flame atomic absorption spectrometry was used for the determination of total Ca, Fe, Mg, and Mn in digested propolis, and of the bioaccessible fractions. The levels of Ca, Fe, Mg, and Mn obtained after digestion ranged from 423.43 – 4368.42, 3.85 – 814.92, 139.02 – 1170.68, and 14.28 – 67.29 mg kg–1, respectively. The bioaccessible contents after simulated gastric digestion of Ca, Fe, Mg, and Mn ranged from 17.62 – 63.35, 0.12 – 1.64, 26.06 – 86.34, and 12.08 – 83.05%, respectively. In the simulation of the gastrointestinal tract, the concentrations ranged from 3.05 – 73.08% for Ca, 0.63 – 2.45% for Fe, 0.16 – 43.26% for Mg, and 1.47 – 8.45% for Mn. In general, the simulation showed higher bioaccessible contents after gastric, compared to gastrointestinal digestion.
{"title":"Bioaccessibility of Ca, Fe, Mg, and Mn in Brazilian Propolis","authors":"Lana Pereira, Robson Brito, Kelly Dantas","doi":"10.30744/brjac.2179-3425.ar-122-2022","DOIUrl":"https://doi.org/10.30744/brjac.2179-3425.ar-122-2022","url":null,"abstract":"The objective of this study was to determine and evaluate the bioaccessibility of Ca, Fe, Mg, and Mn in Apis mellifera and Melipona propolis samples. Flame atomic absorption spectrometry was used for the determination of total Ca, Fe, Mg, and Mn in digested propolis, and of the bioaccessible fractions. The levels of Ca, Fe, Mg, and Mn obtained after digestion ranged from 423.43 – 4368.42, 3.85 – 814.92, 139.02 – 1170.68, and 14.28 – 67.29 mg kg–1, respectively. The bioaccessible contents after simulated gastric digestion of Ca, Fe, Mg, and Mn ranged from 17.62 – 63.35, 0.12 – 1.64, 26.06 – 86.34, and 12.08 – 83.05%, respectively. In the simulation of the gastrointestinal tract, the concentrations ranged from 3.05 – 73.08% for Ca, 0.63 – 2.45% for Fe, 0.16 – 43.26% for Mg, and 1.47 – 8.45% for Mn. In general, the simulation showed higher bioaccessible contents after gastric, compared to gastrointestinal digestion.","PeriodicalId":9115,"journal":{"name":"Brazilian Journal of Analytical Chemistry","volume":" ","pages":""},"PeriodicalIF":0.7,"publicationDate":"2023-06-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"48716704","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 : 2023-06-19DOI: 10.30744/brjac.2179-3425.ar-18-2023
Ma.Helen P. Seco, Eliana Larruscain, Jader Silveira, R. Picoloto, F. Duarte
In this work, a new method for Fe extraction and preconcentration from beer by using dispersive liquid-liquid microextraction (DLLME) and determination by flame atomic absorption spectrometry (F AAS) was developed. Although in DLLME the use of an extraction solvent is mandatory (at least in theory), which is combined with a disperser solvent, in this work only the extraction solvent was used. For Fe extraction by DLLME, the type and volume of extraction solvent, sample volume, type of complexing agent, sample pH, salting out effect, and the number of washing cycles after extraction were evaluated. Thus, after optimization, 10 mL of beer, 75 µL of 1,2-dichlorobenzene of extraction solvent, 500 µL of 0.5% (w/v) pyrrolidine ammonium dithiocarbamate (APDC) as complexing agent were used. It is important to mention that pH adjustment, salt addition or washing cycles were no required. For Fe determination after DLLME, an external calibration curve was performed (R2 > 0.99) by direct extracts (reference solutions through DLLME) introduction in the conventional nebulization system of F AAS instrument. The accuracy evaluation was performed by results comparison with those obtained after microwave-assisted digestion (MAD) and Fe determination by inductively coupled plasma optical emission spectrometry (ICP-OES). The Fe concentration in the studied samples ranged from 59.7 to 68.2 µg L-1 and the limit of quantification for DLLME/F AAS method was 9.0 µg L-1. Finally, the proposed method DLLME/F AAS was applied for Fe determination in several beer samples showing simplicity, low operational costs, suitable accuracy (104 to 119%) and precision (better than 13%), opening the possibility for its use in routine analysis for Fe determination in beer.
{"title":"A Simple Approach for Fe Determination in Beer by using Dispersive Liquid-Liquid Microextraction and Flame Atomic Absorption Spectrometry","authors":"Ma.Helen P. Seco, Eliana Larruscain, Jader Silveira, R. Picoloto, F. Duarte","doi":"10.30744/brjac.2179-3425.ar-18-2023","DOIUrl":"https://doi.org/10.30744/brjac.2179-3425.ar-18-2023","url":null,"abstract":"In this work, a new method for Fe extraction and preconcentration from beer by using dispersive liquid-liquid microextraction (DLLME) and determination by flame atomic absorption spectrometry (F AAS) was developed. Although in DLLME the use of an extraction solvent is mandatory (at least in theory), which is combined with a disperser solvent, in this work only the extraction solvent was used. For Fe extraction by DLLME, the type and volume of extraction solvent, sample volume, type of complexing agent, sample pH, salting out effect, and the number of washing cycles after extraction were evaluated. Thus, after optimization, 10 mL of beer, 75 µL of 1,2-dichlorobenzene of extraction solvent, 500 µL of 0.5% (w/v) pyrrolidine ammonium dithiocarbamate (APDC) as complexing agent were used. It is important to mention that pH adjustment, salt addition or washing cycles were no required. For Fe determination after DLLME, an external calibration curve was performed (R2 > 0.99) by direct extracts (reference solutions through DLLME) introduction in the conventional nebulization system of F AAS instrument. The accuracy evaluation was performed by results comparison with those obtained after microwave-assisted digestion (MAD) and Fe determination by inductively coupled plasma optical emission spectrometry (ICP-OES). The Fe concentration in the studied samples ranged from 59.7 to 68.2 µg L-1 and the limit of quantification for DLLME/F AAS method was 9.0 µg L-1. Finally, the proposed method DLLME/F AAS was applied for Fe determination in several beer samples showing simplicity, low operational costs, suitable accuracy (104 to 119%) and precision (better than 13%), opening the possibility for its use in routine analysis for Fe determination in beer.","PeriodicalId":9115,"journal":{"name":"Brazilian Journal of Analytical Chemistry","volume":" ","pages":""},"PeriodicalIF":0.7,"publicationDate":"2023-06-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"41806955","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 : 2023-06-02DOI: 10.30744/brjac.2179-3425.ar-21-2023
L. Falchi, M. Pistón, Gabriela Casarotto, S. Carro, C. Cajarville, Fiorella Iaquinta
A simple and fast method for the simultaneous determination of chloride and lactic acid in artisanal Danbo cheese was developed and validated. The proposed methodology combined a sample treatment using only ultrapure water as an extracting agent and ion chromatography with suppressed conductivity for the detection of the analytes. One gram of sample exactly weighted is added to 40.0 mL of ultrapure water at 55 ºC. The suspension was stirred for 5 minutes and after centrifugation the supernatant obtained is ready to be used for the determination of both analytes. The performance of this method was evaluated by comparing the results obtained with those acquired after the analysis of the cheese samples using the AOAC reference methods using a t-student test of mean concentration values. At a 95% significance level, the means obtained by the different methods were comparable. Analytical precision expressed as relative standard deviation (RSD %) was less than 6. Artisanal cheese samples were analyzed (n=12) using the validated methodology, obtaining chloride levels between 0.6 and 1.1% w w-1 expressed in sodium chloride and levels of lactic acid between 1.1 and 2.1% w w-1. Additionally, a greenness analysis was presented, using three different metric tools, concluding that the developed method is significantly in better agreement with the principles of Green Analytical Chemistry than the official methods.
{"title":"Development of a Green Methodology for the Determination of Artisanal Danbo Cheese Quality Parameters","authors":"L. Falchi, M. Pistón, Gabriela Casarotto, S. Carro, C. Cajarville, Fiorella Iaquinta","doi":"10.30744/brjac.2179-3425.ar-21-2023","DOIUrl":"https://doi.org/10.30744/brjac.2179-3425.ar-21-2023","url":null,"abstract":"A simple and fast method for the simultaneous determination of chloride and lactic acid in artisanal Danbo cheese was developed and validated. The proposed methodology combined a sample treatment using only ultrapure water as an extracting agent and ion chromatography with suppressed conductivity for the detection of the analytes. One gram of sample exactly weighted is added to 40.0 mL of ultrapure water at 55 ºC. The suspension was stirred for 5 minutes and after centrifugation the supernatant obtained is ready to be used for the determination of both analytes. The performance of this method was evaluated by comparing the results obtained with those acquired after the analysis of the cheese samples using the AOAC reference methods using a t-student test of mean concentration values. At a 95% significance level, the means obtained by the different methods were comparable. Analytical precision expressed as relative standard deviation (RSD %) was less than 6. Artisanal cheese samples were analyzed (n=12) using the validated methodology, obtaining chloride levels between 0.6 and 1.1% w w-1 expressed in sodium chloride and levels of lactic acid between 1.1 and 2.1% w w-1. Additionally, a greenness analysis was presented, using three different metric tools, concluding that the developed method is significantly in better agreement with the principles of Green Analytical Chemistry than the official methods.","PeriodicalId":9115,"journal":{"name":"Brazilian Journal of Analytical Chemistry","volume":" ","pages":""},"PeriodicalIF":0.7,"publicationDate":"2023-06-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"45596583","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 : 2023-06-02DOI: 10.30744/brjac.2179-3425.ar-4-2023
Rayane Costa, J. V. Santiago, E. Ferreira, A. Virgilio, J. G. Gomes Neto
The closed-vessel conductively heated digestion system (CHDS) was evaluated to digest dry dog foods for further determination of K, Na, Cu, Fe, Mn, and Zn by high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS). The CHDS method was optimized using a fractional factorial design with five variables (HNO3 concentration, H2O2 volume, temperature, holding time, and pre-digestion time) at two levels. The accuracy of the CHDS procedure was checked by the analysis of reference materials from the National Institute of Standards and Technology (NIST SRM 1577b Bovine Liver and 2976 Mussel Tissue) and Brazilian Agricultural Research Corporation (Embrapa MR-E1002A Fish Food). Also, the digestion efficiencies were calculated from residual carbon contents (RCCs). The RCC and blank values in the CHDS digested samples were consistently low, which is suitable for determinations using ICP OES and ICP-MS techniques. For comparison, all samples were also digested by microwave-assisted digestion in closed vessels (MW-AD). Results for Na, K, Cu, Fe, Mn, and Zn determined in sample digests obtained by CHDS were not statistically different at a 95% confidence level from those observed for MW-AD. Limits of quantification (LOQ) calculated from digests in CHDS and MW-AD were comparable, and the values provided adequate limits for elemental determinations in dog foods. Data from mineral composition and moisture were employed in a clustering analysis (HCA) and the discrimination of the samples among different manufacturers and food for dogs at different life stages was possible.
{"title":"Closed-Vessel Conductively Heated Digestion of Dry Dog Food for Spectrometric Determination of Essential Nutrients","authors":"Rayane Costa, J. V. Santiago, E. Ferreira, A. Virgilio, J. G. Gomes Neto","doi":"10.30744/brjac.2179-3425.ar-4-2023","DOIUrl":"https://doi.org/10.30744/brjac.2179-3425.ar-4-2023","url":null,"abstract":"The closed-vessel conductively heated digestion system (CHDS) was evaluated to digest dry dog foods for further determination of K, Na, Cu, Fe, Mn, and Zn by high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS). The CHDS method was optimized using a fractional factorial design with five variables (HNO3 concentration, H2O2 volume, temperature, holding time, and pre-digestion time) at two levels. The accuracy of the CHDS procedure was checked by the analysis of reference materials from the National Institute of Standards and Technology (NIST SRM 1577b Bovine Liver and 2976 Mussel Tissue) and Brazilian Agricultural Research Corporation (Embrapa MR-E1002A Fish Food). Also, the digestion efficiencies were calculated from residual carbon contents (RCCs). The RCC and blank values in the CHDS digested samples were consistently low, which is suitable for determinations using ICP OES and ICP-MS techniques. For comparison, all samples were also digested by microwave-assisted digestion in closed vessels (MW-AD). Results for Na, K, Cu, Fe, Mn, and Zn determined in sample digests obtained by CHDS were not statistically different at a 95% confidence level from those observed for MW-AD. Limits of quantification (LOQ) calculated from digests in CHDS and MW-AD were comparable, and the values provided adequate limits for elemental determinations in dog foods. Data from mineral composition and moisture were employed in a clustering analysis (HCA) and the discrimination of the samples among different manufacturers and food for dogs at different life stages was possible.","PeriodicalId":9115,"journal":{"name":"Brazilian Journal of Analytical Chemistry","volume":" ","pages":""},"PeriodicalIF":0.7,"publicationDate":"2023-06-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"41650589","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 : 2023-06-02DOI: 10.30744/brjac.2179-3425.ar-130-2022
Sofia Martins, Giselle de Sousa, Vânia Teles, L. Costa
Cadmium is a toxic element which can be accumulated in the edible parts of plants compromising an entire food chain with serious damage to the living organisms, presenting synergistic and antagonistic effects with the elemental bioaccessibility. In this work, a simulated gastrointestinal digestion was performed to assess the in vitro bioaccessibility of Cd, Cu, Fe and Zn in basil samples after Cd intoxication. The hydroponic cultivation was made in a Hoagland solution at different concentrations (0, 1.5 and 3.0 µmol L-1). Elemental concentration was achieved using a microwave-assisted acid digestion after the growing up of the plants in vermiculite pots by 15 days. The in vitro gastrointestinal procedure was applied in fresh and lyophilized leaves followed by a clean-up step in a sonoreactor cup horn using 1 mL of the extract, 100 µL of HNO3 and 500 µL of H2O2 by 5 minutes. The results showed that Cd bioaccessibility was statistically different at 95% confidence level (p < 0.05) for the lyophilized and fresh leaves samples. The in vitro bioaccessibility increased with concentration in the contamination treatment. Moreover, a high positive correlation was observed between Cd-Fe and Cu-Zn, and a negative correlation between Cd-Zn and Fe-Zn in lyophilized and fresh leaves, respectively, suggesting that the absorption of essential elements was affected by Cd.
{"title":"In vitro bioaccessibility of Cd, Cu, Fe and Zn in basil (Ocimum Basilicum L. Grecco a palla) after cadmium intoxication","authors":"Sofia Martins, Giselle de Sousa, Vânia Teles, L. Costa","doi":"10.30744/brjac.2179-3425.ar-130-2022","DOIUrl":"https://doi.org/10.30744/brjac.2179-3425.ar-130-2022","url":null,"abstract":"Cadmium is a toxic element which can be accumulated in the edible parts of plants compromising an entire food chain with serious damage to the living organisms, presenting synergistic and antagonistic effects with the elemental bioaccessibility. In this work, a simulated gastrointestinal digestion was performed to assess the in vitro bioaccessibility of Cd, Cu, Fe and Zn in basil samples after Cd intoxication. The hydroponic cultivation was made in a Hoagland solution at different concentrations (0, 1.5 and 3.0 µmol L-1). Elemental concentration was achieved using a microwave-assisted acid digestion after the growing up of the plants in vermiculite pots by 15 days. The in vitro gastrointestinal procedure was applied in fresh and lyophilized leaves followed by a clean-up step in a sonoreactor cup horn using 1 mL of the extract, 100 µL of HNO3 and 500 µL of H2O2 by 5 minutes. The results showed that Cd bioaccessibility was statistically different at 95% confidence level (p < 0.05) for the lyophilized and fresh leaves samples. The in vitro bioaccessibility increased with concentration in the contamination treatment. Moreover, a high positive correlation was observed between Cd-Fe and Cu-Zn, and a negative correlation between Cd-Zn and Fe-Zn in lyophilized and fresh leaves, respectively, suggesting that the absorption of essential elements was affected by Cd.","PeriodicalId":9115,"journal":{"name":"Brazilian Journal of Analytical Chemistry","volume":" ","pages":""},"PeriodicalIF":0.7,"publicationDate":"2023-06-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49536447","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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