Pub Date : 2022-09-26DOI: 10.30744/brjac.2179-3425.ar-44-2022
Tallyta Teixeira, Jorge Rodrigues Neto, Elias Silva, A. Conceição, Felix Siqueira, P. Abdelnur
Fungi can produce many bioactive metabolites, which are enhanced when challenged in co-culture competition. For a better evaluation of these metabolites, Mass Spectrometry Imaging (MSI) can be used to provide complementary information about the metabolite spatial localization. However, some adaptations are required on available methodologies in MSI for applications in microorganisms, particularly on sample preparation, due to the characteristics of each type of cell that has to be analyzed. The imprinting method has been shown to be a robust method when applied to sample preparation, but to our knowledge it has never been tested for microbial MALDI-MSI. Herein we applied both Classic and Imprinting MALDI-MSI to compare and analyze metabolites produced by Aspergillus terreus (ATCC® 20542TM) and Pleurotus pulmonarius fungi. For the classic method, the fungi were inoculated for 8 days with PDA medium in a MALDI glass slide. For the imprinting method, fungi were also inoculated for 8 days in a MALDI glass slide and then transferred to a filter paper by manual pressure using a homemade apparatus. Samples were then dehydrated and submitted to HCCA matrix application by sublimation. The chemical images were acquired by MALDI-MSI, and the metabolites were identified by UHPLC-ESI-MS/MS. Twelve ions were detected by MALDI-MSI, using classic (m/z 210.54, 276.99, 307.45, 321.04, 329.70, 346.12, 351.12, 462.41 and 484.02) and imprinting (m/z 313.64, 379.66 and 404.36) methods. Some ions presented a higher intensity in the interaction zone between fungi areas, especially the ions m/z 329.70, 351.12 and 484.02. These ions may be related to metabolites involved in communication between microorganisms, because these fungi formed a mutualistic interaction. All ions were investigated by UHPLC-ESI-MS/MS, and two were identified: adenosine monophosphate (C10H14N5O7P, m/z 346.12, [M-H]-) visualized in the Classic Method, and rubrophen (C22H20O6, m/z 379.66, [M-H]-) visualized in the Imprinting Method. The metabolites from microorganisms are rarely reported in MS/MS databases, which explains the difficulty in the identification of these compounds. Our MSI analysis using the classic method provided a higher number of detected ions. However, both classic and imprinting methods resulted in a complementary information, leading to the detection of ions that were not previously observed on the classic approach. Despite of the challenges encountered on the sample preparation and metabolite identification, using both classic and imprinting MALDI-MSI for bioprospection of fungi metabolites is a promising approach on the analytical field of mass spectrometry which can be later used in biotechnological applications.
{"title":"Mass Spectrometry Imaging for fungal interaction analysis: Classic versus Imprinting Methods","authors":"Tallyta Teixeira, Jorge Rodrigues Neto, Elias Silva, A. Conceição, Felix Siqueira, P. Abdelnur","doi":"10.30744/brjac.2179-3425.ar-44-2022","DOIUrl":"https://doi.org/10.30744/brjac.2179-3425.ar-44-2022","url":null,"abstract":"Fungi can produce many bioactive metabolites, which are enhanced when challenged in co-culture competition. For a better evaluation of these metabolites, Mass Spectrometry Imaging (MSI) can be used to provide complementary information about the metabolite spatial localization. However, some adaptations are required on available methodologies in MSI for applications in microorganisms, particularly on sample preparation, due to the characteristics of each type of cell that has to be analyzed. The imprinting method has been shown to be a robust method when applied to sample preparation, but to our knowledge it has never been tested for microbial MALDI-MSI. Herein we applied both Classic and Imprinting MALDI-MSI to compare and analyze metabolites produced by Aspergillus terreus (ATCC® 20542TM) and Pleurotus pulmonarius fungi. For the classic method, the fungi were inoculated for 8 days with PDA medium in a MALDI glass slide. For the imprinting method, fungi were also inoculated for 8 days in a MALDI glass slide and then transferred to a filter paper by manual pressure using a homemade apparatus. Samples were then dehydrated and submitted to HCCA matrix application by sublimation. The chemical images were acquired by MALDI-MSI, and the metabolites were identified by UHPLC-ESI-MS/MS. Twelve ions were detected by MALDI-MSI, using classic (m/z 210.54, 276.99, 307.45, 321.04, 329.70, 346.12, 351.12, 462.41 and 484.02) and imprinting (m/z 313.64, 379.66 and 404.36) methods. Some ions presented a higher intensity in the interaction zone between fungi areas, especially the ions m/z 329.70, 351.12 and 484.02. These ions may be related to metabolites involved in communication between microorganisms, because these fungi formed a mutualistic interaction. All ions were investigated by UHPLC-ESI-MS/MS, and two were identified: adenosine monophosphate (C10H14N5O7P, m/z 346.12, [M-H]-) visualized in the Classic Method, and rubrophen (C22H20O6, m/z 379.66, [M-H]-) visualized in the Imprinting Method. The metabolites from microorganisms are rarely reported in MS/MS databases, which explains the difficulty in the identification of these compounds. Our MSI analysis using the classic method provided a higher number of detected ions. However, both classic and imprinting methods resulted in a complementary information, leading to the detection of ions that were not previously observed on the classic approach. Despite of the challenges encountered on the sample preparation and metabolite identification, using both classic and imprinting MALDI-MSI for bioprospection of fungi metabolites is a promising approach on the analytical field of mass spectrometry which can be later used in biotechnological applications.","PeriodicalId":9115,"journal":{"name":"Brazilian Journal of Analytical Chemistry","volume":" ","pages":""},"PeriodicalIF":0.7,"publicationDate":"2022-09-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"42658632","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 : 2022-08-31DOI: 10.30744/brjac.2179-3425.ar-30-2022
A. Luna, A. Torres, Camilla L Cunha, I. Lima, Luis Nonato
This work aims to develop an auto-machine learning method using Mid-Infrared (MIR) spectroscopy data to determine the cold filter plugging point (CFPP) and kinematic viscosity at 40 ºC of biodiesel, diesel, and mixtures samples. The biodiesel was obtained by the transesterification reaction and later purified. The first dataset was composed of 108 blends (biodiesel obtained from different biomass such as soy, corn, sunflower, and canola) with binary, ternary and quaternary mixtures. The second dataset was composed of 227 blends of diesel-biodiesel and diesel-biodiesel-ethanol, respectively. The physical properties of the samples were obtained according to ABNT NBR 14747 and ABNT NBR 10441, respectively. The MIR Spectroscopy data were acquired from 7,800 to 450 cm-1, with a 4 cm-1 resolution and 20 scans. The spectra' baseline alignment was carried out using the asymmetric least squares method. A Savitzky–Golay filter was applied to a set of digital data points to smooth the data. This work used a first-order polynomial and a zero derivative function to smooth the spectra. The dataset was split into training and test sets using the function CreateDataPartition from the caret package. It was adopted 70% for training and 30% for test sets. In this work, the model training process was carried out using the open-source Python library LazyPredict. The LazyPredict returns the trained models and their performance metrics. The kinematic viscosity at 40 ºC of the biodiesel samples and their blends could be modeled using the MIR Spectroscopy dataset using different auto-machine learning algorithms. The RMSEP (Root Mean Square Error of Prediction) (≤ 0.02 mm2 s-1) was similar to the experimental error obtained after log transformation. The CFPP of the biodiesel samples and their blends could be modeled using the MIR Spectroscopy dataset by different auto-machine learning algorithms with an RMSEP (≤ 1.6 ºC) similar to the experimental error obtained by traditional methodology. Based on the lower computational time and the same performance observed by the RMSEP and R2 (coefficient of determination) values from different algorithms, it is recommended to use Ridge or Ridge Cross-Validation Regression models for both physical properties using MIR Spectroscopy data.
{"title":"Employing Auto-Machine Learning Algorithms for Predicting the Cold Filter Plugging and Kinematic Viscosity at 40 ºC in Biodiesel Blends using Vibrational Spectroscopy Data","authors":"A. Luna, A. Torres, Camilla L Cunha, I. Lima, Luis Nonato","doi":"10.30744/brjac.2179-3425.ar-30-2022","DOIUrl":"https://doi.org/10.30744/brjac.2179-3425.ar-30-2022","url":null,"abstract":"This work aims to develop an auto-machine learning method using Mid-Infrared (MIR) spectroscopy data to determine the cold filter plugging point (CFPP) and kinematic viscosity at 40 ºC of biodiesel, diesel, and mixtures samples. The biodiesel was obtained by the transesterification reaction and later purified. The first dataset was composed of 108 blends (biodiesel obtained from different biomass such as soy, corn, sunflower, and canola) with binary, ternary and quaternary mixtures. The second dataset was composed of 227 blends of diesel-biodiesel and diesel-biodiesel-ethanol, respectively. The physical properties of the samples were obtained according to ABNT NBR 14747 and ABNT NBR 10441, respectively. The MIR Spectroscopy data were acquired from 7,800 to 450 cm-1, with a 4 cm-1 resolution and 20 scans. The spectra' baseline alignment was carried out using the asymmetric least squares method. A Savitzky–Golay filter was applied to a set of digital data points to smooth the data. This work used a first-order polynomial and a zero derivative function to smooth the spectra. The dataset was split into training and test sets using the function CreateDataPartition from the caret package. It was adopted 70% for training and 30% for test sets. In this work, the model training process was carried out using the open-source Python library LazyPredict. The LazyPredict returns the trained models and their performance metrics. The kinematic viscosity at 40 ºC of the biodiesel samples and their blends could be modeled using the MIR Spectroscopy dataset using different auto-machine learning algorithms. The RMSEP (Root Mean Square Error of Prediction) (≤ 0.02 mm2 s-1) was similar to the experimental error obtained after log transformation. The CFPP of the biodiesel samples and their blends could be modeled using the MIR Spectroscopy dataset by different auto-machine learning algorithms with an RMSEP (≤ 1.6 ºC) similar to the experimental error obtained by traditional methodology. Based on the lower computational time and the same performance observed by the RMSEP and R2 (coefficient of determination) values from different algorithms, it is recommended to use Ridge or Ridge Cross-Validation Regression models for both physical properties using MIR Spectroscopy data.","PeriodicalId":9115,"journal":{"name":"Brazilian Journal of Analytical Chemistry","volume":" ","pages":""},"PeriodicalIF":0.7,"publicationDate":"2022-08-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"45706617","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 : 2022-08-31DOI: 10.30744/brjac.2179-3425.ar-35-2022
Razan Alkassab, Yumen Hilal, Amin Swed
In this study, a rapid, simple, economical and accurate spectrophotometric process was developed for the determination of sodium diclofenac in modified release tablets using ethanol 96% as an available and non-toxic solvent. Sodium diclofenac standard solution was scanned under UV (200-400 nm) in a 1 cm quartz cell to determine the maximum absorption wavelength which was 285 nm. This method was validated in accordance with the requirements of the International Conference on Harmonization (ICH), where the calibration curve showed linearity in the studied concentration range (5-30 μg mL-1) with correlation coefficient R² = 0.9993. The relative standard deviation of the accuracy studies was within the acceptable range (<2%). This method also achieved an excellent recovery ratio (Mean recovery ± S.D. = 100.44% ± 0.81) with high sensitivity (limit of detection 1.10 μg mL-1 and quantitation limit of 3.34 μg mL-1). The developed process applied successfully to determine sodium diclofenac in four commercial pharmaceuticals products (A, B, C and D) marketed locally as modified-release tablets. The product C showed the highest assay value 106% and product B showed the lowest value 98%. Hence, we recommend using this method to quantitatively determine of sodium diclofenac in pharmaceutical dosage forms.
{"title":"Development and Validation of a Simple Spectrophotometric Method for Quantitative Determination of Sodium Diclofenac in Modified-Release Tablets","authors":"Razan Alkassab, Yumen Hilal, Amin Swed","doi":"10.30744/brjac.2179-3425.ar-35-2022","DOIUrl":"https://doi.org/10.30744/brjac.2179-3425.ar-35-2022","url":null,"abstract":"In this study, a rapid, simple, economical and accurate spectrophotometric process was developed for the determination of sodium diclofenac in modified release tablets using ethanol 96% as an available and non-toxic solvent. Sodium diclofenac standard solution was scanned under UV (200-400 nm) in a 1 cm quartz cell to determine the maximum absorption wavelength which was 285 nm. This method was validated in accordance with the requirements of the International Conference on Harmonization (ICH), where the calibration curve showed linearity in the studied concentration range (5-30 μg mL-1) with correlation coefficient R² = 0.9993. The relative standard deviation of the accuracy studies was within the acceptable range (<2%). This method also achieved an excellent recovery ratio (Mean recovery ± S.D. = 100.44% ± 0.81) with high sensitivity (limit of detection 1.10 μg mL-1 and quantitation limit of 3.34 μg mL-1). The developed process applied successfully to determine sodium diclofenac in four commercial pharmaceuticals products (A, B, C and D) marketed locally as modified-release tablets. The product C showed the highest assay value 106% and product B showed the lowest value 98%. Hence, we recommend using this method to quantitatively determine of sodium diclofenac in pharmaceutical dosage forms.","PeriodicalId":9115,"journal":{"name":"Brazilian Journal of Analytical Chemistry","volume":" ","pages":""},"PeriodicalIF":0.7,"publicationDate":"2022-08-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46707693","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 : 2022-08-03DOI: 10.30744/brjac.2179-3425.rv-42-2022
Lanaia Maciel, R. Martins, D. Gondim, João V A Oliveira, Julia Pereira, Gustavo Pereira, Leonardo Ferreira, A. Chaves, B. Vaz
Parkinson's disease (PD) is globally known as the most common movement disorder and the second most common neurodegenerative disease. The disease includes the symptoms of involuntary limb tremors, stiffness, or inflexibility of limbs and joints, among others. Due to this, scientific reports on analytical methodologies to evaluate the progression of neurodegenerative diseases are extremely necessary. Traditional methods include histochemical, immunohistochemical, and ligand-based approaches, however, these approaches still suffer from selectivity limitations of association, leading to a wrong evaluation. In this context, mass spectrometry imaging methods, such as desorption electrospray ionization (DESI), are potential approaches to visualize the distribution of biomarkers that can lead to the information on the progress of PD. This review aims to bring a discussion of some DESI methodologies reported in the literature for the assessment of neurotransmitters associated with PD.
{"title":"Desorption Electrospray Ionization Imaging for Neurotransmitters Evaluation: A Potential Approach to Parkinson’s Disease Monitoring","authors":"Lanaia Maciel, R. Martins, D. Gondim, João V A Oliveira, Julia Pereira, Gustavo Pereira, Leonardo Ferreira, A. Chaves, B. Vaz","doi":"10.30744/brjac.2179-3425.rv-42-2022","DOIUrl":"https://doi.org/10.30744/brjac.2179-3425.rv-42-2022","url":null,"abstract":"Parkinson's disease (PD) is globally known as the most common movement disorder and the second most common neurodegenerative disease. The disease includes the symptoms of involuntary limb tremors, stiffness, or inflexibility of limbs and joints, among others. Due to this, scientific reports on analytical methodologies to evaluate the progression of neurodegenerative diseases are extremely necessary. Traditional methods include histochemical, immunohistochemical, and ligand-based approaches, however, these approaches still suffer from selectivity limitations of association, leading to a wrong evaluation. In this context, mass spectrometry imaging methods, such as desorption electrospray ionization (DESI), are potential approaches to visualize the distribution of biomarkers that can lead to the information on the progress of PD. This review aims to bring a discussion of some DESI methodologies reported in the literature for the assessment of neurotransmitters associated with PD.","PeriodicalId":9115,"journal":{"name":"Brazilian Journal of Analytical Chemistry","volume":" ","pages":""},"PeriodicalIF":0.7,"publicationDate":"2022-08-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"42242162","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 : 2022-08-03DOI: 10.30744/brjac.2179-3425.ar-38-2022
Fiorella Iaquinta, J. Santander, M. Pistón, I. Machado
Four methods for the efficient extraction of copper from bovine and ovine liver were optimized. Sample preparation consisted of extractions with dilute nitric acid or dilute tetramethyl ammonium hydroxide, assisted by an ultrasonic bath or an ultrasonic probe. Copper was determined by flame atomic absorption spectrometry. The experimental conditions were optimized using multivariate experiments. All methods were considered adequate for copper extraction, however, the two methods involving the probe turned out to be more efficient and faster, so they were selected for subsequent validation. Trueness was verified after the analysis of a certified reference material and the performance of a microwave-assisted extraction. Results were statistically equivalent, at the 95% significance level, to the values declared on the certificate. Precision (expressed as relative standard deviation) was better than 5% for all methods. Samples obtained from Uruguayan animals were analyzed. Obtained results agreed with previous results from sheep and cattle abroad. The proposed methods are simple alternatives for food surveillance and animal status monitoring, being straightforward and aligned with Green Chemistry principles, as it was demonstrated by performing the analytical Eco-Scale comprehensive approach. A discussion related to the particle size distribution obtained during the multivariate experiments was also included, to give some deeper insight into ultrasound effect on the biological tissue in different media. In addition, ultrasound-assisted extraction was compared to magnetic stirring to prove the effect of ultrasound.
{"title":"Comparison of Ultrasound-assisted Methods for Copper Determination in Bovine and Ovine Liver as Strategies for Food Surveillance and Animal Status Monitoring","authors":"Fiorella Iaquinta, J. Santander, M. Pistón, I. Machado","doi":"10.30744/brjac.2179-3425.ar-38-2022","DOIUrl":"https://doi.org/10.30744/brjac.2179-3425.ar-38-2022","url":null,"abstract":"Four methods for the efficient extraction of copper from bovine and ovine liver were optimized. Sample preparation consisted of extractions with dilute nitric acid or dilute tetramethyl ammonium hydroxide, assisted by an ultrasonic bath or an ultrasonic probe. Copper was determined by flame atomic absorption spectrometry. The experimental conditions were optimized using multivariate experiments. All methods were considered adequate for copper extraction, however, the two methods involving the probe turned out to be more efficient and faster, so they were selected for subsequent validation. Trueness was verified after the analysis of a certified reference material and the performance of a microwave-assisted extraction. Results were statistically equivalent, at the 95% significance level, to the values declared on the certificate. Precision (expressed as relative standard deviation) was better than 5% for all methods. Samples obtained from Uruguayan animals were analyzed. Obtained results agreed with previous results from sheep and cattle abroad. The proposed methods are simple alternatives for food surveillance and animal status monitoring, being straightforward and aligned with Green Chemistry principles, as it was demonstrated by performing the analytical Eco-Scale comprehensive approach. A discussion related to the particle size distribution obtained during the multivariate experiments was also included, to give some deeper insight into ultrasound effect on the biological tissue in different media. In addition, ultrasound-assisted extraction was compared to magnetic stirring to prove the effect of ultrasound.","PeriodicalId":9115,"journal":{"name":"Brazilian Journal of Analytical Chemistry","volume":" ","pages":""},"PeriodicalIF":0.7,"publicationDate":"2022-08-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44318803","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 : 2022-08-03DOI: 10.30744/brjac.2179-3425.ar-21-2022
Ana Karolina Costa, J. Senna, Larissa Cardoso, L. Palermo, C. Mansur
Flamboyant mirim gum is a galactomannan, extracted from Caesalpinia pulcherrima seeds, a legume family schrub. The main objective of this work was to propose a factorial experimental design to optimize the galactomannan extraction process from its seeds and evaluate its potential as a viscosifying agent for enhanced oil recovery (EOR). The galactomannan was characterized by FTIR, NMR, SEC, thermogravimetric analysis, elemental analysis, and rheology. Structural analyses confirmed the presence of the desired galactomannan content. The best yield obtained was 7.3% for initial seed mass and 24.6% for the endosperm. Rheological analysis showed that Flamboyant mirim gum is a promising alternative for EOR application in high salinity conditions. In addition, stability tests showed that glutaraldehyde can be considered a promising biocide for fluids containing galactomannan since it maintained the viscosity values of the systems for 42 days. Thus, the results confirmed the adequacy of the extraction procedure for obtaining galactomannan.
{"title":"Extraction and Evaluation of Flamboyant Mirim Gum as a Potential Viscosifying Agent for Enhanced Oil Recovery Fluids","authors":"Ana Karolina Costa, J. Senna, Larissa Cardoso, L. Palermo, C. Mansur","doi":"10.30744/brjac.2179-3425.ar-21-2022","DOIUrl":"https://doi.org/10.30744/brjac.2179-3425.ar-21-2022","url":null,"abstract":"Flamboyant mirim gum is a galactomannan, extracted from Caesalpinia pulcherrima seeds, a legume family schrub. The main objective of this work was to propose a factorial experimental design to optimize the galactomannan extraction process from its seeds and evaluate its potential as a viscosifying agent for enhanced oil recovery (EOR). The galactomannan was characterized by FTIR, NMR, SEC, thermogravimetric analysis, elemental analysis, and rheology. Structural analyses confirmed the presence of the desired galactomannan content. The best yield obtained was 7.3% for initial seed mass and 24.6% for the endosperm. Rheological analysis showed that Flamboyant mirim gum is a promising alternative for EOR application in high salinity conditions. In addition, stability tests showed that glutaraldehyde can be considered a promising biocide for fluids containing galactomannan since it maintained the viscosity values of the systems for 42 days. Thus, the results confirmed the adequacy of the extraction procedure for obtaining galactomannan.","PeriodicalId":9115,"journal":{"name":"Brazilian Journal of Analytical Chemistry","volume":" ","pages":""},"PeriodicalIF":0.7,"publicationDate":"2022-08-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43909451","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 : 2022-08-01DOI: 10.30744/brjac.2179-3425.ar-17-2022
C. Ramos, Daysnan dos Santos, Líbna Claudino, J. de Albuquerque, Marcílio Silva
A simple method was developed to obtain and fractionate essential oil simultaneously by hydrodistillation. With this method it was possible to obtain essential oils from the leaves of Piper arboreum with the cadinol content ranging from 17.7 to 57.9%. In the essential oils from the leaves of P. aduncum was identified dillapiole with content ranging from 4.6 to 96.9%; and further, essential oil from P. marginatum with the presence of phenylpropanoids as minor compounds. The essential oils of the three Piper species varied in antimicrobial activity when fractionated, with P. marginatum oil exhibiting the lowest minimum inhibitory concentration at 19.5 µg mL-1 for the Pseudomonas aeruginosa bacterium. The method was efficient for the separation and concentration of chemical constituents of essential oils from the same plant, able to distinguish the different chemical profiles, both qualitatively and quantitatively.
{"title":"Use of Hydrodistillation to Obtain and Fractionate Essential Oils Simultaneously","authors":"C. Ramos, Daysnan dos Santos, Líbna Claudino, J. de Albuquerque, Marcílio Silva","doi":"10.30744/brjac.2179-3425.ar-17-2022","DOIUrl":"https://doi.org/10.30744/brjac.2179-3425.ar-17-2022","url":null,"abstract":"A simple method was developed to obtain and fractionate essential oil simultaneously by hydrodistillation. With this method it was possible to obtain essential oils from the leaves of Piper arboreum with the cadinol content ranging from 17.7 to 57.9%. In the essential oils from the leaves of P. aduncum was identified dillapiole with content ranging from 4.6 to 96.9%; and further, essential oil from P. marginatum with the presence of phenylpropanoids as minor compounds. The essential oils of the three Piper species varied in antimicrobial activity when fractionated, with P. marginatum oil exhibiting the lowest minimum inhibitory concentration at 19.5 µg mL-1 for the Pseudomonas aeruginosa bacterium. The method was efficient for the separation and concentration of chemical constituents of essential oils from the same plant, able to distinguish the different chemical profiles, both qualitatively and quantitatively.","PeriodicalId":9115,"journal":{"name":"Brazilian Journal of Analytical Chemistry","volume":" ","pages":""},"PeriodicalIF":0.7,"publicationDate":"2022-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44575072","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 : 2022-08-01DOI: 10.30744/brjac.2179-3425.ar-47-2022
N. Agrawal, Shilpi Pathak
Evogliptin (EGT) is used in fixed-dose combination with metformin hydrochloride (MFH) for a better glycemic control in Type 2 diabetes mellitus. To date, no method is available for simultaneous estimation of these drugs. In the present study, an UV spectrophotometric method was developed in distilled water, an environment-friendly solvent using the simultaneous equation technique to simultaneously determine EGT and MFH in bulk and tablet dosage form. The developed method was validated and applied to commercial tablet dosage forms containing EGT and MFH in combination. With a great correlation value (R2>0.998), the analytes displayed good linearity in the range of 10-100 μg mL-1. The low percent relative standard deviation proved the methods' precision. The methods' accuracy was demonstrated by excellent recovery. Thus, the developed method was found to be simple, environment-friendly, fast, specific, precise, and accurate, and it may be effectively used for routine analysis of EGT and MFH in bulk and their combined tablet dosage form.
{"title":"Eco-Friendly UV Spectrophotometric Method for Simultaneous Estimation of Evogliptin and Metformin Hydrochloride in Bulk and Combined Tablet Dosage Form","authors":"N. Agrawal, Shilpi Pathak","doi":"10.30744/brjac.2179-3425.ar-47-2022","DOIUrl":"https://doi.org/10.30744/brjac.2179-3425.ar-47-2022","url":null,"abstract":"Evogliptin (EGT) is used in fixed-dose combination with metformin hydrochloride (MFH) for a better glycemic control in Type 2 diabetes mellitus. To date, no method is available for simultaneous estimation of these drugs. In the present study, an UV spectrophotometric method was developed in distilled water, an environment-friendly solvent using the simultaneous equation technique to simultaneously determine EGT and MFH in bulk and tablet dosage form. The developed method was validated and applied to commercial tablet dosage forms containing EGT and MFH in combination. With a great correlation value (R2>0.998), the analytes displayed good linearity in the range of 10-100 μg mL-1. The low percent relative standard deviation proved the methods' precision. The methods' accuracy was demonstrated by excellent recovery. Thus, the developed method was found to be simple, environment-friendly, fast, specific, precise, and accurate, and it may be effectively used for routine analysis of EGT and MFH in bulk and their combined tablet dosage form.","PeriodicalId":9115,"journal":{"name":"Brazilian Journal of Analytical Chemistry","volume":" ","pages":""},"PeriodicalIF":0.7,"publicationDate":"2022-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"48044527","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 : 2022-07-11DOI: 10.30744/brjac.2179-3425.ar-16-2022
Danielle Francischini, R. Amais, N. Stríkis, M. Arruda
The laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) technique is considered versatile for multi-elemental analysis and imaging because it is easy to handle, compatible with different types of solid samples, requires minimal sample preparation, and provides high spatial resolution and sensitivity. One of the challenges of imaging analysis is to obtain accurate and precise spatial information of elements distribution in the sample, so the optimization of the laser ablation (LA) parameters is essential. In this context, this study aimed to optimize the LA parameters for direct analysis of speleothem samples. Laser intensity, frequency, and spot diameter were evaluated through multivariate experimental design and multi-response data, the influence of ablation scan speed and the use of 44Ca as an internal standard (IS) for the qualitative image of 66Zn, 137Ba, 55Mn, 57Fe, 88Sr, 60Ni, and 26Mg distribution in the sample were also evaluated. The multivariate optimization revealed positive interactions between the parameters evaluated, i.e., the greater the laser intensity, LA frequency, and spot diameter, the greater the analyte signal and, thus the sensitivity. Therefore, 90% laser ablation intensity, 20 Hz repetition rate, and 100 µm spot diameter were selected. In the scan speed evaluation, the images obtained with 40 and 20 µm s-1 were very similar for all isotopes. The use of 44Ca as IS did not impact the resolution of the images. The use of 44Ca can provide important information about the speleothem formation and paleoclimate changes.
{"title":"Qualitative imaging of elemental spatial distribution in stalagmites through laser ablation inductively coupled plasma mass spectrometry analysis","authors":"Danielle Francischini, R. Amais, N. Stríkis, M. Arruda","doi":"10.30744/brjac.2179-3425.ar-16-2022","DOIUrl":"https://doi.org/10.30744/brjac.2179-3425.ar-16-2022","url":null,"abstract":"The laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) technique is considered versatile for multi-elemental analysis and imaging because it is easy to handle, compatible with different types of solid samples, requires minimal sample preparation, and provides high spatial resolution and sensitivity. One of the challenges of imaging analysis is to obtain accurate and precise spatial information of elements distribution in the sample, so the optimization of the laser ablation (LA) parameters is essential. In this context, this study aimed to optimize the LA parameters for direct analysis of speleothem samples. Laser intensity, frequency, and spot diameter were evaluated through multivariate experimental design and multi-response data, the influence of ablation scan speed and the use of 44Ca as an internal standard (IS) for the qualitative image of 66Zn, 137Ba, 55Mn, 57Fe, 88Sr, 60Ni, and 26Mg distribution in the sample were also evaluated. The multivariate optimization revealed positive interactions between the parameters evaluated, i.e., the greater the laser intensity, LA frequency, and spot diameter, the greater the analyte signal and, thus the sensitivity. Therefore, 90% laser ablation intensity, 20 Hz repetition rate, and 100 µm spot diameter were selected. In the scan speed evaluation, the images obtained with 40 and 20 µm s-1 were very similar for all isotopes. The use of 44Ca as IS did not impact the resolution of the images. The use of 44Ca can provide important information about the speleothem formation and paleoclimate changes.","PeriodicalId":9115,"journal":{"name":"Brazilian Journal of Analytical Chemistry","volume":" ","pages":""},"PeriodicalIF":0.7,"publicationDate":"2022-07-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46730642","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 : 2022-06-27DOI: 10.30744/brjac.2179-3425.ar-14-2022
Letícia Leonardelli, S. Leonardelli, J. Schwambach
The Brazilian blueberry (Vaccinium spp.) production has made remarkable progress in developing quality and quantity. The price of the fruit for fresh and processing purposes is linked to its quality and origin. An effective method for authenticity control and traceability is the stable isotopes method. Carbon (13C) and oxygen (18O) of Brazilian blueberries have never been extensively explored. In this work, the results of 13C and 18O (performed by IRMS) of thirty blueberry samples were presented and discussed, being eleven different cultivars produced in the Southern Brazilian region from mountain and high-altitude. The blueberry showed the typical range of carbon isotopes for C3 plants, with significant differences between Rabbiteye and Southern Highbush. The δ13C and δ18O values showed a significant difference between a mountain and a high-altitude region. This study represents the first isotopic database for Brazilian blueberries, and it can be incorporated into a traceability system. In addition, these results can be used to verify the authenticity of the fruit composition declared on the label and as an effective tool for identifying the geographical origin.
{"title":"Carbon and Oxygen Isotope Profile in Brazilian Blueberries (Vaccinium spp.)","authors":"Letícia Leonardelli, S. Leonardelli, J. Schwambach","doi":"10.30744/brjac.2179-3425.ar-14-2022","DOIUrl":"https://doi.org/10.30744/brjac.2179-3425.ar-14-2022","url":null,"abstract":"The Brazilian blueberry (Vaccinium spp.) production has made remarkable progress in developing quality and quantity. The price of the fruit for fresh and processing purposes is linked to its quality and origin. An effective method for authenticity control and traceability is the stable isotopes method. Carbon (13C) and oxygen (18O) of Brazilian blueberries have never been extensively explored. In this work, the results of 13C and 18O (performed by IRMS) of thirty blueberry samples were presented and discussed, being eleven different cultivars produced in the Southern Brazilian region from mountain and high-altitude. The blueberry showed the typical range of carbon isotopes for C3 plants, with significant differences between Rabbiteye and Southern Highbush. The δ13C and δ18O values showed a significant difference between a mountain and a high-altitude region. This study represents the first isotopic database for Brazilian blueberries, and it can be incorporated into a traceability system. In addition, these results can be used to verify the authenticity of the fruit composition declared on the label and as an effective tool for identifying the geographical origin.","PeriodicalId":9115,"journal":{"name":"Brazilian Journal of Analytical Chemistry","volume":" ","pages":""},"PeriodicalIF":0.7,"publicationDate":"2022-06-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46140667","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}
京公网安备 11010802042870号
京ICP备2023020795号-1
扫码关注我们
求助内容：
应助结果提醒方式：