Pub Date : 2024-04-13DOI: 10.3390/analytica5020011
D. Castejón, J. Segura, Karen Paola Cruz-Díaz, Víctor Remiro, M. E. Fernández-Valle, M. D. Romero de Ávila, Palmira Villa, M. I. Cambero
For the first time, High-Resolution Magic Angle Nuclear Magnetic Resonance spectroscopy (NMR-HRMAS) was applied to directly identify specific metabolites from a Spanish raw ewe’s milk and enzymatic coagulation pressed-curd cheese (Protected Geographical Indication: Castellano) manufactured by two procedures (traditional/artisanal vs. industrial) and including the ewe’s raw milk. The NMR parameters were optimized to study the complex matrixes of this type of cheese. In addition, conventional overcrowded 1H-NMR-HRMAS spectra were selectively simplified by a Carr–Purcell–Meiboom–Gill (CPMG) sequence or a stimulated echo pulse sequence by bipolar gradients (DIFF), thus modulating spin–spin relaxation times and diffusion of molecular components, respectively. 1H-NMR-HRMAS spectroscopy displayed important information about cheese metabolites, which can be associated with different manufacturing processes (industrial vs. traditional) and ripening times (from 2 to 90 days). These results support that this spectroscopy is a useful technique to monitor the ripening process, from raw milk to commercial ripened cheese, using a minimum intact sample, implying the absence of time-consuming sample pretreatments.
{"title":"A Metabolomics Study by 1H HRMAS NMR: From Sheep Milk to a Pressed-Curd Cheese: A Proof of Concept","authors":"D. Castejón, J. Segura, Karen Paola Cruz-Díaz, Víctor Remiro, M. E. Fernández-Valle, M. D. Romero de Ávila, Palmira Villa, M. I. Cambero","doi":"10.3390/analytica5020011","DOIUrl":"https://doi.org/10.3390/analytica5020011","url":null,"abstract":"For the first time, High-Resolution Magic Angle Nuclear Magnetic Resonance spectroscopy (NMR-HRMAS) was applied to directly identify specific metabolites from a Spanish raw ewe’s milk and enzymatic coagulation pressed-curd cheese (Protected Geographical Indication: Castellano) manufactured by two procedures (traditional/artisanal vs. industrial) and including the ewe’s raw milk. The NMR parameters were optimized to study the complex matrixes of this type of cheese. In addition, conventional overcrowded 1H-NMR-HRMAS spectra were selectively simplified by a Carr–Purcell–Meiboom–Gill (CPMG) sequence or a stimulated echo pulse sequence by bipolar gradients (DIFF), thus modulating spin–spin relaxation times and diffusion of molecular components, respectively. 1H-NMR-HRMAS spectroscopy displayed important information about cheese metabolites, which can be associated with different manufacturing processes (industrial vs. traditional) and ripening times (from 2 to 90 days). These results support that this spectroscopy is a useful technique to monitor the ripening process, from raw milk to commercial ripened cheese, using a minimum intact sample, implying the absence of time-consuming sample pretreatments.","PeriodicalId":7829,"journal":{"name":"Analytica","volume":"63 3","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-04-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140707097","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 : 2024-04-02DOI: 10.3390/analytica5020010
M. Perkins, Colin J. Hastie, V. Langford
Personal care products (PCPs) are intended for regular application by consumers and therefore assuring the safety of these products is very important. Recently, benzene contamination has been highlighted in certain PCPs. The present study applies selected ion flow tube mass spectrometry (SIFT-MS) to a simultaneous headspace analysis of benzene, 1,4-dioxane, and formaldehyde—all known or suspected carcinogens—in nine haircare products with supporting qualitative analysis by gas chromatography–mass spectrometry (GC-MS). Headspace-SIFT-MS method development is compatible with the method of standard additions, which is necessary for the quantitation of volatile impurities in these complex emulsions. Benzene was quantified above the low-ng g−1 limit of quantitation (LOQ) in three products, dioxane above the sub-μg g−1 LOQ in all products, and formaldehyde above the low-μg g−1 LOQ in two products, providing a quantitative analysis at concentrations relevant to consumer safety. This study facilitated the development of generic workflows for SIFT-MS method development and application in routine analysis of PCPs. The assessment of workflows for SIFT-MS compared to a conventional GC-MS analysis suggests that 8- to 30-fold throughput enhancements may be possible for quantitative and screening analysis using SIFT-MS.
{"title":"Headspace-Selected Ion Flow Tube Mass Spectrometry Workflows for Rapid Screening and Quantitation of Hazardous Volatile Impurities in Personal Care Products","authors":"M. Perkins, Colin J. Hastie, V. Langford","doi":"10.3390/analytica5020010","DOIUrl":"https://doi.org/10.3390/analytica5020010","url":null,"abstract":"Personal care products (PCPs) are intended for regular application by consumers and therefore assuring the safety of these products is very important. Recently, benzene contamination has been highlighted in certain PCPs. The present study applies selected ion flow tube mass spectrometry (SIFT-MS) to a simultaneous headspace analysis of benzene, 1,4-dioxane, and formaldehyde—all known or suspected carcinogens—in nine haircare products with supporting qualitative analysis by gas chromatography–mass spectrometry (GC-MS). Headspace-SIFT-MS method development is compatible with the method of standard additions, which is necessary for the quantitation of volatile impurities in these complex emulsions. Benzene was quantified above the low-ng g−1 limit of quantitation (LOQ) in three products, dioxane above the sub-μg g−1 LOQ in all products, and formaldehyde above the low-μg g−1 LOQ in two products, providing a quantitative analysis at concentrations relevant to consumer safety. This study facilitated the development of generic workflows for SIFT-MS method development and application in routine analysis of PCPs. The assessment of workflows for SIFT-MS compared to a conventional GC-MS analysis suggests that 8- to 30-fold throughput enhancements may be possible for quantitative and screening analysis using SIFT-MS.","PeriodicalId":7829,"journal":{"name":"Analytica","volume":"23 19","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-04-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140753321","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 : 2024-03-15DOI: 10.3390/analytica5010009
Gabriela Knippelberg Bifano Manea, Vanusa Bueno Freire, Rainério Escalfoni Junior, E. C. de Oliveira
Petroleum-produced water is the primary effluent generated during the oil extraction process, presenting high flow rates, and containing a series of chemical components that are harmful to the environment, such as dissolved manganese. The proof of metrological compatibility between laboratories and different test methods or techniques is an analytical challenge when complying with environmental laws and regulations, which is the aim of this study. The first step of this study was to compare the results of manganese content in real test samples of produced water between some laboratories that used different test methods, that is, flame atomic absorption spectrophotometry, inductively coupled plasma optical emission spectroscopy, and inductively coupled plasma mass spectrometry. Based on one-way analysis of variance, systematic errors were found. The following step was to visit a specific lab, where one could confirm the relevance of the wavelength parameters, operating conditions for the view configuration, and effects of the saline matrices. Finally, a compatibility assessment between the reference laboratory and a new laboratory, which implemented and validated its analytical methodology based on these analytical adjustments, and the experiences and lessons learned in the previous step, was undertaken by a paired t-test.
石油生产用水是石油开采过程中产生的主要废水，流量大，含有一系列对环境有害的化学成分，如溶解锰。在遵守环境法律法规时，如何证明实验室和不同测试方法或技术之间的计量兼容性是一项分析挑战，这也是本研究的目的所在。本研究的第一步是比较使用不同测试方法（即火焰原子吸收分光光度法、电感耦合等离子体光发射光谱法和电感耦合等离子体质谱法）的一些实验室对真实产水测试样本中锰含量的测试结果。根据单因子方差分析，发现了系统误差。接下来的步骤是访问特定实验室，在那里可以确认波长参数的相关性、视图配置的操作条件以及盐水基质的影响。最后，通过配对 t 检验，对参考实验室和新实验室之间的兼容性进行了评估，新实验室根据这些分析调整以及上一步的经验和教训，实施并验证了其分析方法。
{"title":"Analytical Compatibility between Various Techniques for Determining Dissolved Manganese in Produced Water","authors":"Gabriela Knippelberg Bifano Manea, Vanusa Bueno Freire, Rainério Escalfoni Junior, E. C. de Oliveira","doi":"10.3390/analytica5010009","DOIUrl":"https://doi.org/10.3390/analytica5010009","url":null,"abstract":"Petroleum-produced water is the primary effluent generated during the oil extraction process, presenting high flow rates, and containing a series of chemical components that are harmful to the environment, such as dissolved manganese. The proof of metrological compatibility between laboratories and different test methods or techniques is an analytical challenge when complying with environmental laws and regulations, which is the aim of this study. The first step of this study was to compare the results of manganese content in real test samples of produced water between some laboratories that used different test methods, that is, flame atomic absorption spectrophotometry, inductively coupled plasma optical emission spectroscopy, and inductively coupled plasma mass spectrometry. Based on one-way analysis of variance, systematic errors were found. The following step was to visit a specific lab, where one could confirm the relevance of the wavelength parameters, operating conditions for the view configuration, and effects of the saline matrices. Finally, a compatibility assessment between the reference laboratory and a new laboratory, which implemented and validated its analytical methodology based on these analytical adjustments, and the experiences and lessons learned in the previous step, was undertaken by a paired t-test.","PeriodicalId":7829,"journal":{"name":"Analytica","volume":" 14","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-03-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140391613","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 : 2024-03-05DOI: 10.3390/analytica5010008
Jamila Gagour, Otmane Hallouch, Abderrahim Asbbane, A. Laknifli, E. Sakar, Khalid Majourhat, S. Gharby
This study focuses on evaluating the characteristics of olive oil produced in the Taroudant province (southern Morocco), making this the first comprehensive study focusing on olive oil from the ‘Moroccan Picholine’ cultivar. Our objective was to elucidate the distinctive qualities of olive oil from this region, providing valuable insights into its potential contributions to the country’s olive oil sector. For this purpose, several quality criteria (free fatty acids, moisture content, saponification value, and iodine value), oxidation indices (peroxide value, specific UV extinction coefficients, and oxidizability value), and purity indices (fatty acids and sterol composition) were evaluated. Our results reveal minor-to-significant variations (p < 0.05) in the quality and oxidation parameters. Specifically, our results indicate diverse ranges for free fatty acids (0.33–3.62 g/100 g), peroxide values (0.85–4.01 mEq O2/kg oil), K232 (1.68 to 2.73), and K270 (0.09–0.34). Furthermore, consistently high levels of oleic acid (55.8 to 73.1%) and β-sitosterol (94.2 to 97%) were observed in the studied samples. These outcomes were confirmed through the use principal component analysis and hierarchical cluster analysis. Likewise, important correlations were outlined among the studied parameters. Multidimensional analyses not only highlight inherent variations, but also facilitate the classification of the analyzed olive oils into distinct categories. The results suggest that the Taroudant province exhibits favorable conditions for producing high-quality olive oil.
{"title":"Physicochemical Characterization of ‘Moroccan Picholine’ Olive (Olea europaea L.) Oil Produced in Southern Morocco Using Multivariate Statistical Analysis","authors":"Jamila Gagour, Otmane Hallouch, Abderrahim Asbbane, A. Laknifli, E. Sakar, Khalid Majourhat, S. Gharby","doi":"10.3390/analytica5010008","DOIUrl":"https://doi.org/10.3390/analytica5010008","url":null,"abstract":"This study focuses on evaluating the characteristics of olive oil produced in the Taroudant province (southern Morocco), making this the first comprehensive study focusing on olive oil from the ‘Moroccan Picholine’ cultivar. Our objective was to elucidate the distinctive qualities of olive oil from this region, providing valuable insights into its potential contributions to the country’s olive oil sector. For this purpose, several quality criteria (free fatty acids, moisture content, saponification value, and iodine value), oxidation indices (peroxide value, specific UV extinction coefficients, and oxidizability value), and purity indices (fatty acids and sterol composition) were evaluated. Our results reveal minor-to-significant variations (p < 0.05) in the quality and oxidation parameters. Specifically, our results indicate diverse ranges for free fatty acids (0.33–3.62 g/100 g), peroxide values (0.85–4.01 mEq O2/kg oil), K232 (1.68 to 2.73), and K270 (0.09–0.34). Furthermore, consistently high levels of oleic acid (55.8 to 73.1%) and β-sitosterol (94.2 to 97%) were observed in the studied samples. These outcomes were confirmed through the use principal component analysis and hierarchical cluster analysis. Likewise, important correlations were outlined among the studied parameters. Multidimensional analyses not only highlight inherent variations, but also facilitate the classification of the analyzed olive oils into distinct categories. The results suggest that the Taroudant province exhibits favorable conditions for producing high-quality olive oil.","PeriodicalId":7829,"journal":{"name":"Analytica","volume":"20 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-03-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140263616","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 : 2024-03-03DOI: 10.3390/analytica5010007
Danielle Tapia Bueno, Amanda Fonseca Leitzke, R. L. Crizel, Cristina Jansen-Alves, Emanuel Gomes Bertizzolo, Juliana Porciuncula da Silva, Gabrielly Quartieri Sejanes, K. Mariotti, Claudio Martin Pereira de Pereira
Fingerprints are essential for human identification and are valuable tools in criminal investigations. The pursuit of new materials for digital printing is expanding, with increasing interest in natural compounds such as bixin, sourced from annatto seeds. Despite its traditional use as a natural dye with medicinal properties, the potential of bixin in papilloscopy remains largely untapped. In this study, we meticulously extracted bixin from annatto seeds and meticulously developed composites incorporating zinc carbonate (bixin/ZnCO3) and kaolinite (bixin/kaolinite). UV-visible spectroscopy was used for characterization, and the extracted bixin showed absorption peaks at 429, 453, and 481 nm, which were very similar to standard peaks at 429, 457, and 487 nm. The two samples also had the same retention times (7.07 min) according to further liquid chromatography analysis. Sweat pores were easier to detect thanks to the effectiveness of the bixin/ZnCO3 and bixin/kaolinite composites in creating high contrast sebaceous and natural latent fingerprints. These results highlight the composites’ potential as novel and fascinating instruments for papilloscopy applications, which might also improve forensic investigations.
{"title":"Characterization of Bixin by UV-Visible Spectroscopy and HPLC, and Its Application as Latent Fingermark Developer","authors":"Danielle Tapia Bueno, Amanda Fonseca Leitzke, R. L. Crizel, Cristina Jansen-Alves, Emanuel Gomes Bertizzolo, Juliana Porciuncula da Silva, Gabrielly Quartieri Sejanes, K. Mariotti, Claudio Martin Pereira de Pereira","doi":"10.3390/analytica5010007","DOIUrl":"https://doi.org/10.3390/analytica5010007","url":null,"abstract":"Fingerprints are essential for human identification and are valuable tools in criminal investigations. The pursuit of new materials for digital printing is expanding, with increasing interest in natural compounds such as bixin, sourced from annatto seeds. Despite its traditional use as a natural dye with medicinal properties, the potential of bixin in papilloscopy remains largely untapped. In this study, we meticulously extracted bixin from annatto seeds and meticulously developed composites incorporating zinc carbonate (bixin/ZnCO3) and kaolinite (bixin/kaolinite). UV-visible spectroscopy was used for characterization, and the extracted bixin showed absorption peaks at 429, 453, and 481 nm, which were very similar to standard peaks at 429, 457, and 487 nm. The two samples also had the same retention times (7.07 min) according to further liquid chromatography analysis. Sweat pores were easier to detect thanks to the effectiveness of the bixin/ZnCO3 and bixin/kaolinite composites in creating high contrast sebaceous and natural latent fingerprints. These results highlight the composites’ potential as novel and fascinating instruments for papilloscopy applications, which might also improve forensic investigations.","PeriodicalId":7829,"journal":{"name":"Analytica","volume":"62 0_1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-03-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140267476","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 : 2024-02-04DOI: 10.3390/analytica5010006
Dimitrios Mpakos, Theodoros G. Chatzimitakos, V. Athanasiadis, Martha Mantiniotou, Eleni Bozinou, S. Lalas
The current investigation examines the application of pulsed electric fields (PEFs) for isolating polyphenols from Cannabis sativa var. Futura 75 leaves. Firstly, the solvent composition, which included ethanol, water, and various mixtures of the two, was explored, along with the liquid-to-solid ratio. Subsequently, the primary parameters associated with PEFs (namely, pulse duration, pulse period, electric field intensity, and treatment duration) were optimized. The extracted samples were analyzed to determine their total polyphenol content (TPC), and individual polyphenols were also evaluated through high-performance liquid chromatography. In addition, the antioxidant activity of the extracts was assessed through ferric-reducing antioxidant power (FRAP) and DPPH assays. The extracts prepared utilizing PEFs were compared to the extracts obtained without PEFs in terms of their TPC, FRAP values, and DPPH activity. The results indicate that the most effective extraction parameters were a pulse duration of 10 μs, a pulse period of 1000 μs, and an electric field strength of 0.9 kV/cm after 25 min of extraction. The most efficient solvent was determined to be a 50% (v/v) mixture of ethanol and water in a 20:1 liquid-to-solid ratio. The extract obtained under the optimal conditions exhibited a ~75% increase in TPC compared to the extract obtained without any application of PEFs, while some individual polyphenols exhibited an increase of up to ~300%. Furthermore, significant increases of ~74% and ~71% were observed in FRAP and DPPH assays. From the information provided, it was observed that the tested variables had an impact on the recovery of polyphenols from C. sativa leaves.
{"title":"Optimization of Pulsed Electric Field-Based Extraction of Bioactive Compounds from Cannabis sativa Leaves","authors":"Dimitrios Mpakos, Theodoros G. Chatzimitakos, V. Athanasiadis, Martha Mantiniotou, Eleni Bozinou, S. Lalas","doi":"10.3390/analytica5010006","DOIUrl":"https://doi.org/10.3390/analytica5010006","url":null,"abstract":"The current investigation examines the application of pulsed electric fields (PEFs) for isolating polyphenols from Cannabis sativa var. Futura 75 leaves. Firstly, the solvent composition, which included ethanol, water, and various mixtures of the two, was explored, along with the liquid-to-solid ratio. Subsequently, the primary parameters associated with PEFs (namely, pulse duration, pulse period, electric field intensity, and treatment duration) were optimized. The extracted samples were analyzed to determine their total polyphenol content (TPC), and individual polyphenols were also evaluated through high-performance liquid chromatography. In addition, the antioxidant activity of the extracts was assessed through ferric-reducing antioxidant power (FRAP) and DPPH assays. The extracts prepared utilizing PEFs were compared to the extracts obtained without PEFs in terms of their TPC, FRAP values, and DPPH activity. The results indicate that the most effective extraction parameters were a pulse duration of 10 μs, a pulse period of 1000 μs, and an electric field strength of 0.9 kV/cm after 25 min of extraction. The most efficient solvent was determined to be a 50% (v/v) mixture of ethanol and water in a 20:1 liquid-to-solid ratio. The extract obtained under the optimal conditions exhibited a ~75% increase in TPC compared to the extract obtained without any application of PEFs, while some individual polyphenols exhibited an increase of up to ~300%. Furthermore, significant increases of ~74% and ~71% were observed in FRAP and DPPH assays. From the information provided, it was observed that the tested variables had an impact on the recovery of polyphenols from C. sativa leaves.","PeriodicalId":7829,"journal":{"name":"Analytica","volume":"10 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-02-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139867383","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 : 2024-02-04DOI: 10.3390/analytica5010006
Dimitrios Mpakos, Theodoros G. Chatzimitakos, V. Athanasiadis, Martha Mantiniotou, Eleni Bozinou, S. Lalas
The current investigation examines the application of pulsed electric fields (PEFs) for isolating polyphenols from Cannabis sativa var. Futura 75 leaves. Firstly, the solvent composition, which included ethanol, water, and various mixtures of the two, was explored, along with the liquid-to-solid ratio. Subsequently, the primary parameters associated with PEFs (namely, pulse duration, pulse period, electric field intensity, and treatment duration) were optimized. The extracted samples were analyzed to determine their total polyphenol content (TPC), and individual polyphenols were also evaluated through high-performance liquid chromatography. In addition, the antioxidant activity of the extracts was assessed through ferric-reducing antioxidant power (FRAP) and DPPH assays. The extracts prepared utilizing PEFs were compared to the extracts obtained without PEFs in terms of their TPC, FRAP values, and DPPH activity. The results indicate that the most effective extraction parameters were a pulse duration of 10 μs, a pulse period of 1000 μs, and an electric field strength of 0.9 kV/cm after 25 min of extraction. The most efficient solvent was determined to be a 50% (v/v) mixture of ethanol and water in a 20:1 liquid-to-solid ratio. The extract obtained under the optimal conditions exhibited a ~75% increase in TPC compared to the extract obtained without any application of PEFs, while some individual polyphenols exhibited an increase of up to ~300%. Furthermore, significant increases of ~74% and ~71% were observed in FRAP and DPPH assays. From the information provided, it was observed that the tested variables had an impact on the recovery of polyphenols from C. sativa leaves.
{"title":"Optimization of Pulsed Electric Field-Based Extraction of Bioactive Compounds from Cannabis sativa Leaves","authors":"Dimitrios Mpakos, Theodoros G. Chatzimitakos, V. Athanasiadis, Martha Mantiniotou, Eleni Bozinou, S. Lalas","doi":"10.3390/analytica5010006","DOIUrl":"https://doi.org/10.3390/analytica5010006","url":null,"abstract":"The current investigation examines the application of pulsed electric fields (PEFs) for isolating polyphenols from Cannabis sativa var. Futura 75 leaves. Firstly, the solvent composition, which included ethanol, water, and various mixtures of the two, was explored, along with the liquid-to-solid ratio. Subsequently, the primary parameters associated with PEFs (namely, pulse duration, pulse period, electric field intensity, and treatment duration) were optimized. The extracted samples were analyzed to determine their total polyphenol content (TPC), and individual polyphenols were also evaluated through high-performance liquid chromatography. In addition, the antioxidant activity of the extracts was assessed through ferric-reducing antioxidant power (FRAP) and DPPH assays. The extracts prepared utilizing PEFs were compared to the extracts obtained without PEFs in terms of their TPC, FRAP values, and DPPH activity. The results indicate that the most effective extraction parameters were a pulse duration of 10 μs, a pulse period of 1000 μs, and an electric field strength of 0.9 kV/cm after 25 min of extraction. The most efficient solvent was determined to be a 50% (v/v) mixture of ethanol and water in a 20:1 liquid-to-solid ratio. The extract obtained under the optimal conditions exhibited a ~75% increase in TPC compared to the extract obtained without any application of PEFs, while some individual polyphenols exhibited an increase of up to ~300%. Furthermore, significant increases of ~74% and ~71% were observed in FRAP and DPPH assays. From the information provided, it was observed that the tested variables had an impact on the recovery of polyphenols from C. sativa leaves.","PeriodicalId":7829,"journal":{"name":"Analytica","volume":"2001 14","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-02-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139807232","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 : 2024-02-02DOI: 10.3390/analytica5010005
A. E. F. Oliveira, Arnaldo César Pereira, Mayra A. C. Resende, L. F. Ferreira
A disposable voltammetric immunosensor was developed to measure breast cancer biomarker 15-3 (CA 15-3) in human saliva and serum samples. Screen-printed paper-based electrodes (f-SPE) previously fabricated by our research group using homemade conductive inks were used as transducers, which were later modified only with gold nanoparticles to immobilize anti-CA 15-3 antibodies. The sensor was operated using antigen–antibody interactions in conjunction with a redox species (ferrocyanide potassium) for the indirect determination of the CA 15-3 antigen. The device characterization involved atomic force microscopy (AFM) and electrochemical analysis. Optimization of the construction and response of the immunosensor was achieved at incubation times of 6 h for anti-CA 15-3, 1 h for bovine serum albumin, and 1 h for interaction with CA 15-3. The sensor displays a linear range between 2 and 16 U/mL, with a sensitivity of 0.012 μA/U mL−1, a limit of detection (LOD) of 0.56 U/mL, and a limit of quantification (LOQ) of 1.88 U/mL. The interfering substances minimally affected the signal, with 4.94% response variation, and the reproducibility of the immunosensor demonstrated a relative standard deviation (RSD) of 5.65%. The sensor successfully determined the CA 15-3 concentration in human serum and saliva, demonstrating its potential for clinical analysis.
我们开发了一种一次性伏安免疫传感器，用于测量人体唾液和血清样本中的乳腺癌生物标记物 15-3 (CA15-3)。我们的研究小组以前用自制导电油墨制作的丝网印刷纸基电极（f-SPE）被用作传感器，后来仅用金纳米粒子对其进行了修饰，以固定抗 CA 15-3 抗体。该传感器利用抗原-抗体之间的相互作用以及氧化还原物质（亚铁氰化钾）来间接测定 CA 15-3 抗原。该装置的表征包括原子力显微镜（AFM）和电化学分析。抗 CA 15-3 的孵育时间为 6 小时，牛血清白蛋白的孵育时间为 1 小时，与 CA 15-3 相互作用的孵育时间为 1 小时，在这些条件下对免疫传感器的构造和响应进行了优化。该传感器的线性范围为 2 至 16 U/mL，灵敏度为 0.012 μA/U mL-1，检出限（LOD）为 0.56 U/mL，定量限（LOQ）为 1.88 U/mL。干扰物质对信号的影响很小，反应变异率为 4.94%，免疫传感器的重现性相对标准偏差（RSD）为 5.65%。该传感器成功测定了人体血清和唾液中的 CA 15-3 浓度，证明了其在临床分析中的应用潜力。
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Pub Date : 2024-02-02DOI: 10.3390/analytica5010004
Y. Shastak, Wolf Pelletier, Andrea Kuntz
The accurate assessment of vitamin A in animal feed and tissues is vital for safeguarding animal well-being and ensuring high-quality nutritional feed. However, challenges in achieving precise results persist, necessitating a comprehensive understanding of the influencing factors. This review delves into the historical progression of analytical techniques, from colorimetric assays and spectrophotometry to advanced chromatographic methods and non-destructive spectroscopic approaches. Factors influencing analytical precision are scrutinized, encompassing sample preparation, storage conditions, interfering substances, and human errors. The crucial role of quality control and standardized protocols in ensuring the reproducibility and reliability of results is emphasized. Moreover, this review highlights the need for tailored analytical approaches to account for the complexities of sample matrices and the significance of cutting-edge technologies, including on-site analysis and data science integration, in enhancing analytical precision. By acknowledging the challenges and prospects in vitamin A analysis, this paper provides insights for optimizing analytical methodologies and promoting animal welfare and product safety.
准确评估动物饲料和组织中的维生素 A 对保障动物健康和确保优质营养饲料至关重要。然而，要获得精确的结果仍面临挑战，因此有必要全面了解影响因素。本综述深入探讨了分析技术的历史进程，从比色法和分光光度法到先进的色谱法和无损光谱法。影响分析精度的因素包括样品制备、储存条件、干扰物质和人为错误。本综述强调了质量控制和标准化方案在确保结果的可重复性和可靠性方面的关键作用。此外，本综述还强调了定制分析方法的必要性，以考虑到样品基质的复杂性，以及尖端技术（包括现场分析和数据科学集成）在提高分析精度方面的重要性。通过认识维生素 A 分析的挑战和前景，本文为优化分析方法、促进动物福利和产品安全提供了真知灼见。
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Pub Date : 2024-02-02DOI: 10.3390/analytica5010004
Y. Shastak, Wolf Pelletier, Andrea Kuntz
The accurate assessment of vitamin A in animal feed and tissues is vital for safeguarding animal well-being and ensuring high-quality nutritional feed. However, challenges in achieving precise results persist, necessitating a comprehensive understanding of the influencing factors. This review delves into the historical progression of analytical techniques, from colorimetric assays and spectrophotometry to advanced chromatographic methods and non-destructive spectroscopic approaches. Factors influencing analytical precision are scrutinized, encompassing sample preparation, storage conditions, interfering substances, and human errors. The crucial role of quality control and standardized protocols in ensuring the reproducibility and reliability of results is emphasized. Moreover, this review highlights the need for tailored analytical approaches to account for the complexities of sample matrices and the significance of cutting-edge technologies, including on-site analysis and data science integration, in enhancing analytical precision. By acknowledging the challenges and prospects in vitamin A analysis, this paper provides insights for optimizing analytical methodologies and promoting animal welfare and product safety.
准确评估动物饲料和组织中的维生素 A 对保障动物健康和确保优质营养饲料至关重要。然而，要获得精确的结果仍面临挑战，因此有必要全面了解影响因素。本综述深入探讨了分析技术的历史进程，从比色法和分光光度法到先进的色谱法和无损光谱法。影响分析精度的因素包括样品制备、储存条件、干扰物质和人为错误。本综述强调了质量控制和标准化方案在确保结果的可重复性和可靠性方面的关键作用。此外，本综述还强调了定制分析方法的必要性，以考虑到样品基质的复杂性，以及尖端技术（包括现场分析和数据科学集成）在提高分析精度方面的重要意义。通过认识维生素 A 分析的挑战和前景，本文为优化分析方法、促进动物福利和产品安全提供了真知灼见。
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