Pub Date : 2024-01-05DOI: 10.3390/separations11010019
Ikki Tateishi, M. Furukawa, H. Katsumata, S. Kaneco
B-doped zinc oxide/copper oxide composites prepared using a simple method showed high photocatalytic hydrogen production activity in the presence of aqueous sulfide solutions. Co-modification of the CuO composite with B-doping caused an increase in the charge separation efficiency and light absorption capacity. The sacrificial effect was thermodynamically enhanced by manipulating the composition of the sulfide solution. A maximum hydrogen production activity of 224 μmol g−1 h−1 was achieved under 450 nm light irradiation in a photocatalytic system with optimized B doping, a CuO composite, and a sulfide sacrificial agent concentration.
用简单的方法制备的掺杂了 B 的氧化锌/氧化铜复合材料在硫化物水溶液中显示出很高的光催化制氢活性。用 B 掺杂对氧化铜复合材料进行共修饰可提高电荷分离效率和光吸收能力。通过调节硫化物溶液的成分，牺牲效应在热力学上得到了增强。在优化了 B 掺杂、CuO 复合材料和硫化物牺牲剂浓度的光催化系统中，450 纳米光照射下的最大产氢活性达到了 224 μmol g-1 h-1。
{"title":"Effective Utilization of Sulfur Wastewater by Photocatalytic System Using B/CuO/ZnO","authors":"Ikki Tateishi, M. Furukawa, H. Katsumata, S. Kaneco","doi":"10.3390/separations11010019","DOIUrl":"https://doi.org/10.3390/separations11010019","url":null,"abstract":"B-doped zinc oxide/copper oxide composites prepared using a simple method showed high photocatalytic hydrogen production activity in the presence of aqueous sulfide solutions. Co-modification of the CuO composite with B-doping caused an increase in the charge separation efficiency and light absorption capacity. The sacrificial effect was thermodynamically enhanced by manipulating the composition of the sulfide solution. A maximum hydrogen production activity of 224 μmol g−1 h−1 was achieved under 450 nm light irradiation in a photocatalytic system with optimized B doping, a CuO composite, and a sulfide sacrificial agent concentration.","PeriodicalId":21833,"journal":{"name":"Separations","volume":"8 1","pages":""},"PeriodicalIF":2.6,"publicationDate":"2024-01-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139381101","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-01-05DOI: 10.3390/separations11010021
Bogusław Buszewski, Dušan Berek, Virginia Coman
The origin of the International Symposia on Separation Sciences (ISSS) can be found in the national gas chromatography scientific meetings held in Zagreb, Croatia, from 1967 and later at Plitvice Lakes until 1988 [...]
{"title":"Central European Group for Separation Sciences (CEGSS)—Brief History and Memoirs on the Creation and Activity","authors":"Bogusław Buszewski, Dušan Berek, Virginia Coman","doi":"10.3390/separations11010021","DOIUrl":"https://doi.org/10.3390/separations11010021","url":null,"abstract":"The origin of the International Symposia on Separation Sciences (ISSS) can be found in the national gas chromatography scientific meetings held in Zagreb, Croatia, from 1967 and later at Plitvice Lakes until 1988 [...]","PeriodicalId":21833,"journal":{"name":"Separations","volume":"36 18","pages":""},"PeriodicalIF":2.6,"publicationDate":"2024-01-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139382575","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-01-05DOI: 10.3390/separations11010018
Mohamed A. Abdelaziz, Neil D. Danielson
In this work, three cyanoalkyl silicone GC stationary-phase polymers, namely OV-105, OV-225, and OV-275, were investigated as potential extractants for dispersive liquid–liquid microextraction (DLLME). The OV-225 polymer (cyanopropylmethyl-phenylmethylsilicone) exhibited the cleanest chromatographic background and was extensively studied. The proposed polymer was tested through the DLLME of four non-steroidal anti-inflammatory drugs from aqueous samples, followed by HPLC separation with UV detection at 230 nm. To achieve the maximum enrichment, the experimental conditions that influence the DLLME process were optimized using one-factor-at-a-time and design-of-experiment (DoE) approaches. The extraction variables (polymer mass, dispersive solvent volume, buffer pH, and mixing time) were screened by implementing a two-level full factorial design (FFD). Significant variables were fine-tuned using response surface methodology based on a face-centered central composite design (CCD). The optimum conditions were 10 mg of polymer (extraction medium); 50 µL of tetrahydrofuran (dispersive solvent); 100 µL of phosphate buffer pH 2.75 ([PO43−] = 100 mM); and 3 min of vortex mixing. The addition of salt had a minimal effect on the enrichment factors. In the optimum conditions, enrichment factors up to 46 were achieved using 1.5 mL samples. Calibration curves exhibited correlation coefficients > 0.999 using 4-pentylbenzoic acid as an internal standard. The limits of quantitation were 5 ng/mL for naproxen, 10 ng/mL for diflunisal, 25 ng/mL for indomethacin, and 75 ng/mL for ibuprofen. The analysis of spiked tap water samples showed adequate relative recoveries and precision. In conclusion, the proposed polymer (OV-225) is a potential greener alternative to traditional organic extractants used in DLLME.
{"title":"A Cyanoalkyl Silicone GC Stationary-Phase Polymer as an Extractant for Dispersive Liquid–Liquid Microextraction","authors":"Mohamed A. Abdelaziz, Neil D. Danielson","doi":"10.3390/separations11010018","DOIUrl":"https://doi.org/10.3390/separations11010018","url":null,"abstract":"In this work, three cyanoalkyl silicone GC stationary-phase polymers, namely OV-105, OV-225, and OV-275, were investigated as potential extractants for dispersive liquid–liquid microextraction (DLLME). The OV-225 polymer (cyanopropylmethyl-phenylmethylsilicone) exhibited the cleanest chromatographic background and was extensively studied. The proposed polymer was tested through the DLLME of four non-steroidal anti-inflammatory drugs from aqueous samples, followed by HPLC separation with UV detection at 230 nm. To achieve the maximum enrichment, the experimental conditions that influence the DLLME process were optimized using one-factor-at-a-time and design-of-experiment (DoE) approaches. The extraction variables (polymer mass, dispersive solvent volume, buffer pH, and mixing time) were screened by implementing a two-level full factorial design (FFD). Significant variables were fine-tuned using response surface methodology based on a face-centered central composite design (CCD). The optimum conditions were 10 mg of polymer (extraction medium); 50 µL of tetrahydrofuran (dispersive solvent); 100 µL of phosphate buffer pH 2.75 ([PO43−] = 100 mM); and 3 min of vortex mixing. The addition of salt had a minimal effect on the enrichment factors. In the optimum conditions, enrichment factors up to 46 were achieved using 1.5 mL samples. Calibration curves exhibited correlation coefficients > 0.999 using 4-pentylbenzoic acid as an internal standard. The limits of quantitation were 5 ng/mL for naproxen, 10 ng/mL for diflunisal, 25 ng/mL for indomethacin, and 75 ng/mL for ibuprofen. The analysis of spiked tap water samples showed adequate relative recoveries and precision. In conclusion, the proposed polymer (OV-225) is a potential greener alternative to traditional organic extractants used in DLLME.","PeriodicalId":21833,"journal":{"name":"Separations","volume":"38 3","pages":""},"PeriodicalIF":2.6,"publicationDate":"2024-01-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139382337","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-01-05DOI: 10.3390/separations11010020
Wenxia Xie, Chunmin Tu, Jun Zhang, Chengwei Xu
The accumulation of uncollected fly ash from flue gas in post-combustion CO2 capture processes is a significant concern in current coal-fired power plants due to its potential impact on the performance of CO2 absorbent and absorption towers. In order to determine the effect of fly ash on the mass transfer performance of CO2 absorption into monoethanolamine (MEA) and diethanolamine (DEA) aqueous solutions, experimental studies were carried out using a small-sized packed tower equipped with θ-ring random packing. These studies were conducted under various operating parameters, including solution temperature, liquid/gas ratio (L/G), packing height, and fly ash concentration. The results show that the effect of fly ash on the outlet CO2 concentration was primarily observed during the initial stages of the experimental process. Moreover, the presence of fly ash leads to a reduction in the volumetric overall mass transfer coefficient (KGav) when using MEA and DEA solution, and increasing the fly ash concentration further exacerbates this negative impact. However, the effect of fly ash on the reduction in KGav is not significantly related to its chemical composition but rather depends on the operational parameters. With increasing solution temperature, liquid/gas ratio (L/G), and packing height, the KGav values for different solutions exhibit an upward trend. The negative effect of fly ash on KGav remains relatively stable for MEA as solution temperature and packing height increase. Compared to MEA, fly ash has a greater negative effect on DEA solution under the same experimental conditions. The analysis reveals that the detrimental effect of fly ash on KGav primarily stems from its ability to alter the distribution state of the absorption liquid within the packed tower.
在目前的燃煤发电厂中，燃烧后二氧化碳捕集过程中烟气中积累的未收集飞灰是一个重大问题，因为它可能会影响二氧化碳吸收剂和吸收塔的性能。为了确定粉煤灰对二氧化碳吸收到单乙醇胺（MEA）和二乙醇胺（DEA）水溶液中的传质性能的影响，我们使用装有θ-环无规填料的小型填料塔进行了实验研究。这些研究是在不同的操作参数下进行的，包括溶液温度、液气比 (L/G)、填料高度和粉煤灰浓度。结果表明，粉煤灰对出口二氧化碳浓度的影响主要体现在实验过程的初始阶段。此外，在使用 MEA 和 DEA 溶液时，粉煤灰的存在会导致体积总传质系数（KGav）降低，而增加粉煤灰浓度会进一步加剧这种负面影响。不过，粉煤灰对 KGav 降低的影响与其化学成分并无明显关系，而是取决于运行参数。随着溶液温度、液气比（L/G）和填料高度的增加，不同溶液的 KGav 值呈上升趋势。随着溶液温度和填料高度的增加，粉煤灰对 MEA KGav 的负面影响保持相对稳定。与 MEA 相比，在相同的实验条件下，粉煤灰对 DEA 溶液的负面影响更大。分析表明，粉煤灰对 KGav 的不利影响主要源于粉煤灰能够改变填料塔内吸收液的分布状态。
{"title":"Effect of Fly Ash on the Mass Transfer Performance of CO2 Removal Using MEA and DEA Solutions in a Packed Tower","authors":"Wenxia Xie, Chunmin Tu, Jun Zhang, Chengwei Xu","doi":"10.3390/separations11010020","DOIUrl":"https://doi.org/10.3390/separations11010020","url":null,"abstract":"The accumulation of uncollected fly ash from flue gas in post-combustion CO2 capture processes is a significant concern in current coal-fired power plants due to its potential impact on the performance of CO2 absorbent and absorption towers. In order to determine the effect of fly ash on the mass transfer performance of CO2 absorption into monoethanolamine (MEA) and diethanolamine (DEA) aqueous solutions, experimental studies were carried out using a small-sized packed tower equipped with θ-ring random packing. These studies were conducted under various operating parameters, including solution temperature, liquid/gas ratio (L/G), packing height, and fly ash concentration. The results show that the effect of fly ash on the outlet CO2 concentration was primarily observed during the initial stages of the experimental process. Moreover, the presence of fly ash leads to a reduction in the volumetric overall mass transfer coefficient (KGav) when using MEA and DEA solution, and increasing the fly ash concentration further exacerbates this negative impact. However, the effect of fly ash on the reduction in KGav is not significantly related to its chemical composition but rather depends on the operational parameters. With increasing solution temperature, liquid/gas ratio (L/G), and packing height, the KGav values for different solutions exhibit an upward trend. The negative effect of fly ash on KGav remains relatively stable for MEA as solution temperature and packing height increase. Compared to MEA, fly ash has a greater negative effect on DEA solution under the same experimental conditions. The analysis reveals that the detrimental effect of fly ash on KGav primarily stems from its ability to alter the distribution state of the absorption liquid within the packed tower.","PeriodicalId":21833,"journal":{"name":"Separations","volume":"9 4","pages":""},"PeriodicalIF":2.6,"publicationDate":"2024-01-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139383133","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-01-03DOI: 10.3390/separations11010017
Tao Bai, Yuhu Yao, Jiaxin Zhao, Laixin Tian, Luming Zhang
This study investigated the adsorption performance of hydrothermal carbon derived from banana peel and modified with different concentrations of phosphoric acid solution, then used to adsorb lead ions in an aqueous solution. The surface structure and functional groups of the modified hydrothermal carbon were analyzed using XRD, SEM, FT-IR, elemental analysis, and BET. The results showed that the adsorption capacity of modified hydrothermal carbon derived from banana peel reached 40.64 mg/g at a hydrothermal temperature of 240 °C, a phosphoric acid solution of 2 mol/L, and a solid–liquid ratio of 2 g/L, with a removal efficiency of 82.74%. The adsorption process conformed to the pseudo-second-order kinetic model and the Langmuir isotherm equation. The correlation coefficient of 0.99 for fitting the adsorption process using an artificial neural network, indicating that the artificial neural network could be used to predict adsorption. The adsorption of Pb(II) from an aqueous solution by phosphoric acid-modified hydrothermal carbon was dominated by monolayer chemical adsorption, and the adsorption mechanisms included electrostatic attraction, ion exchange, surface complexation, and physical adsorption.
{"title":"Adsorption Performance and Mechanism of H3PO4-Modified Banana Peel Hydrothermal Carbon on Pb(II)","authors":"Tao Bai, Yuhu Yao, Jiaxin Zhao, Laixin Tian, Luming Zhang","doi":"10.3390/separations11010017","DOIUrl":"https://doi.org/10.3390/separations11010017","url":null,"abstract":"This study investigated the adsorption performance of hydrothermal carbon derived from banana peel and modified with different concentrations of phosphoric acid solution, then used to adsorb lead ions in an aqueous solution. The surface structure and functional groups of the modified hydrothermal carbon were analyzed using XRD, SEM, FT-IR, elemental analysis, and BET. The results showed that the adsorption capacity of modified hydrothermal carbon derived from banana peel reached 40.64 mg/g at a hydrothermal temperature of 240 °C, a phosphoric acid solution of 2 mol/L, and a solid–liquid ratio of 2 g/L, with a removal efficiency of 82.74%. The adsorption process conformed to the pseudo-second-order kinetic model and the Langmuir isotherm equation. The correlation coefficient of 0.99 for fitting the adsorption process using an artificial neural network, indicating that the artificial neural network could be used to predict adsorption. The adsorption of Pb(II) from an aqueous solution by phosphoric acid-modified hydrothermal carbon was dominated by monolayer chemical adsorption, and the adsorption mechanisms included electrostatic attraction, ion exchange, surface complexation, and physical adsorption.","PeriodicalId":21833,"journal":{"name":"Separations","volume":"115 9","pages":""},"PeriodicalIF":2.6,"publicationDate":"2024-01-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139387792","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-01-03DOI: 10.3390/separations11010016
F. Buthmann, Sophia Volpert, J. Koop, Gerhard Schembecker
Centrifugal Partition Chromatography (CPC) utilizes a two-phase liquid–liquid system as mobile and stationary phases. During operation, the latter continuously drains out of the rotor, despite it being in fact stationary, leading to decreasing separation efficiency over time, a phenomenon still poorly understood today because neither simulations nor extensive experimental investigations have addressed this so-called bleeding. With the model presented in this study, the underlying hydrodynamics are discussed in detail. This model can simulate bleeding over 60 s and is verified experimentally for different operating points (volumetric flow rates of 5, 12, and 20 mL⋅min−1) of the Centrifugal Partition Chromatograph utilizing an aqueous–organic phase system. We simulated two interconnected chambers at the rotor inlet and analyzed the loss of the stationary phase over time. The results of the simulated second chamber are closely aligned with the experimental validation results. Thus, the prediction of bleeding utilizing the simulation of hydrodynamics was successful. Moreover, we highlighted the benefits of the two-chamber setup modeled in this study compared to single-chamber models.
{"title":"Prediction of Bleeding via Simulation of Hydrodynamics in Centrifugal Partition Chromatography","authors":"F. Buthmann, Sophia Volpert, J. Koop, Gerhard Schembecker","doi":"10.3390/separations11010016","DOIUrl":"https://doi.org/10.3390/separations11010016","url":null,"abstract":"Centrifugal Partition Chromatography (CPC) utilizes a two-phase liquid–liquid system as mobile and stationary phases. During operation, the latter continuously drains out of the rotor, despite it being in fact stationary, leading to decreasing separation efficiency over time, a phenomenon still poorly understood today because neither simulations nor extensive experimental investigations have addressed this so-called bleeding. With the model presented in this study, the underlying hydrodynamics are discussed in detail. This model can simulate bleeding over 60 s and is verified experimentally for different operating points (volumetric flow rates of 5, 12, and 20 mL⋅min−1) of the Centrifugal Partition Chromatograph utilizing an aqueous–organic phase system. We simulated two interconnected chambers at the rotor inlet and analyzed the loss of the stationary phase over time. The results of the simulated second chamber are closely aligned with the experimental validation results. Thus, the prediction of bleeding utilizing the simulation of hydrodynamics was successful. Moreover, we highlighted the benefits of the two-chamber setup modeled in this study compared to single-chamber models.","PeriodicalId":21833,"journal":{"name":"Separations","volume":"12 8","pages":""},"PeriodicalIF":2.6,"publicationDate":"2024-01-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139388610","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-12-31DOI: 10.3390/separations11010015
A. Francioso, Ignacio Antonio Jiménez Díaz, Carolina Pérez Reyes, Cristina González Montelongo, M. Pierini, Claudio Villani, I. Bazzocchi
Phyllanthus is a large genus of the Euphorbiaceae family, which has been widely used in traditional medicine. The current study reports the isolation of an unusual C-glycosyl flavonoid, named tenelloside, from Phyllanthus tenellus Roxb., a non-endemic plant present in Canary Islands. The chemical structure of this secondary metabolite was established employing combined spectrometric and spectroscopic techniques, including 1D and 2D NMR experiments and mass spectrometry. The absolute stereochemical configuration was determined via the comparison of experimental and calculated electronic circular dichroism spectra. In our previous work, another C-glycosylated bioactive product was isolated from another Phyllanthus species, suggesting that this class of compounds can be produced in a genus-specific manner in different geographic regions. This work represents another important report for direct future studies on the biological and chemotaxonomic potential of C-glycosylated products of the Phyllanthus genus.
{"title":"Isolation and Chemotaxonomic Implications of Tenelloside, a Novel Unusual C-Glycosyl Flavanone from Phyllanthus tenellus Roxb. in Tenerife Island","authors":"A. Francioso, Ignacio Antonio Jiménez Díaz, Carolina Pérez Reyes, Cristina González Montelongo, M. Pierini, Claudio Villani, I. Bazzocchi","doi":"10.3390/separations11010015","DOIUrl":"https://doi.org/10.3390/separations11010015","url":null,"abstract":"Phyllanthus is a large genus of the Euphorbiaceae family, which has been widely used in traditional medicine. The current study reports the isolation of an unusual C-glycosyl flavonoid, named tenelloside, from Phyllanthus tenellus Roxb., a non-endemic plant present in Canary Islands. The chemical structure of this secondary metabolite was established employing combined spectrometric and spectroscopic techniques, including 1D and 2D NMR experiments and mass spectrometry. The absolute stereochemical configuration was determined via the comparison of experimental and calculated electronic circular dichroism spectra. In our previous work, another C-glycosylated bioactive product was isolated from another Phyllanthus species, suggesting that this class of compounds can be produced in a genus-specific manner in different geographic regions. This work represents another important report for direct future studies on the biological and chemotaxonomic potential of C-glycosylated products of the Phyllanthus genus.","PeriodicalId":21833,"journal":{"name":"Separations","volume":"114 16","pages":""},"PeriodicalIF":2.6,"publicationDate":"2023-12-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139135380","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-12-30DOI: 10.3390/separations11010014
Ljuboš Ušjak, M. Niketić, Silvana Petrović
The aim of this work was to investigate the composition of essential oils isolated from fruits of Peucedanum longifolium, and Rhizomatophora aegopodioides (a species which was previously placed in the genus Peucedanum), as well as to compare the obtained results to those available for other previously investigated related species (including taxa which are also, according to some authors, excluded from the genus Peucedanum). Essential oils were obtained via hydrodistillation in a Clevenger-type apparatus and their composition was analyzed using GC-FID and GC-MS. To compare these data to those of previously investigated taxa, a chemometric approach was applied; the data were analyzed using multivariate statistical methods: non-metric multidimensional scaling (nMDS) and hierarchical cluster analysis. The most abundant in P. longifolium essential oil were monoterpenes (79.7%), mostly α-phellandrene (26.2%), β-phellandrene + limonene (21.0%) and myrcene (9.5%), followed by sesquiterpenes (18.3%), mostly germacrene B (9.5%). On the other hand, dominant in R. aegopodioides essential oil were non-terpenic aliphatic hydrocarbons (46.1%), mainly n-undecane (16.5%) and n-nonane (11.3%). In addition, this essential oil also contained a notable quantity of sesquiterpenes (25.1%), with (E)-sesquilavandulol being the most abundant (10.0%). The results of multivariate statistics revealed a clear separation of the essential oil composition of R. aegopodioides and P. longifolium, as well as of P. longifolium and P. officinale. The clustering of the samples of most of the taxa that do not belong to the Peucedanum in the narrow sense (sensu stricto) was also observed, which is in accordance with their recent inclusion in separate genera.
这项工作的目的是研究从 Peucedanum longifolium 和 Rhizomatophora aegopodioides（以前被归入 Peucedanum 属的一个物种）的果实中分离出来的精油成分，并将所得结果与以前研究过的其他相关物种（包括一些作者认为也被排除在 Peucedanum 属之外的类群）的结果进行比较。精油是在克莱文格尔型仪器中通过水蒸馏获得的，并使用 GC-FID 和 GC-MS 对其成分进行了分析。为了将这些数据与之前研究过的分类群的数据进行比较，采用了化学计量学方法；数据分析采用了多元统计方法：非计量多维标度（nMDS）和分层聚类分析。长叶松精油中含量最高的是单萜（79.7%），主要是α-黄柏烯（26.2%）、β-黄柏烯+柠檬烯（21.0%）和月桂烯（9.5%），其次是倍半萜（18.3%），主要是革兰氏烯 B（9.5%）。另一方面，在 R. aegopodioides 精油中占主导地位的是非萜类脂肪烃（46.1%），主要是正十一烷（16.5%）和正壬烷（11.3%）。此外，这种精油还含有大量倍半萜（25.1%），其中以 (E)-sesquilavandulol 含量最高（10.0%）。多元统计结果显示，R. aegopodioides 和 P. longifolium，以及 P. longifolium 和 P. officinale 的精油成分有明显的分离。此外，还观察到大多数不属于狭义 Peucedanum（严格意义上的 Peucedanum）的分类群样本聚集在一起，这与它们最近被列入单独的属是一致的。
{"title":"Composition of Essential Oils from Fruits of Peucedanum longifolium and Rhizomatophora aegopodioides (Apiaceae) with Regard to Other Related Taxa—A Chemometric Approach","authors":"Ljuboš Ušjak, M. Niketić, Silvana Petrović","doi":"10.3390/separations11010014","DOIUrl":"https://doi.org/10.3390/separations11010014","url":null,"abstract":"The aim of this work was to investigate the composition of essential oils isolated from fruits of Peucedanum longifolium, and Rhizomatophora aegopodioides (a species which was previously placed in the genus Peucedanum), as well as to compare the obtained results to those available for other previously investigated related species (including taxa which are also, according to some authors, excluded from the genus Peucedanum). Essential oils were obtained via hydrodistillation in a Clevenger-type apparatus and their composition was analyzed using GC-FID and GC-MS. To compare these data to those of previously investigated taxa, a chemometric approach was applied; the data were analyzed using multivariate statistical methods: non-metric multidimensional scaling (nMDS) and hierarchical cluster analysis. The most abundant in P. longifolium essential oil were monoterpenes (79.7%), mostly α-phellandrene (26.2%), β-phellandrene + limonene (21.0%) and myrcene (9.5%), followed by sesquiterpenes (18.3%), mostly germacrene B (9.5%). On the other hand, dominant in R. aegopodioides essential oil were non-terpenic aliphatic hydrocarbons (46.1%), mainly n-undecane (16.5%) and n-nonane (11.3%). In addition, this essential oil also contained a notable quantity of sesquiterpenes (25.1%), with (E)-sesquilavandulol being the most abundant (10.0%). The results of multivariate statistics revealed a clear separation of the essential oil composition of R. aegopodioides and P. longifolium, as well as of P. longifolium and P. officinale. The clustering of the samples of most of the taxa that do not belong to the Peucedanum in the narrow sense (sensu stricto) was also observed, which is in accordance with their recent inclusion in separate genera.","PeriodicalId":21833,"journal":{"name":"Separations","volume":" 10","pages":""},"PeriodicalIF":2.6,"publicationDate":"2023-12-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139139650","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-12-28DOI: 10.3390/separations11010013
Tellez-Robles Daniela, López-Cortez Ma. del Socorro, Santoyo-Tepole Fortunata, Rosales-Martínez Patricia, García-Ochoa Felipe, Hernández-Botello Mayuric Teresa, Salgdo-Cruz María de la Paz
Red wine contains polyphenols which are extracted during the winemaking process. However, winemaking is not an extraction; therefore, the resulting byproducts still have a substantial polyphenol content. The aim of this study was to compare two methods for the extraction of phenolic compounds: maceration and matrix solid-phase dispersion (MSPD). Grape pomace (Vitis vinifera var. Cabernet Sauvignon) from a winery in Querétaro, Mexico was used. The optimal conditions for both methods were identified. Phenolic compounds and antioxidant activity were the response variables. A central composite design was used (Minitab 17) for the extraction by maceration. The maceration time (1, 4, 12, 20, and 24 h) and the ratio of ethanol (50 to 80%) acidified with 1% HCl were the two factors studied. For the MSPD extraction, sea sand was used as a dispersant, and a 22 factorial design was employed for the evaluation, with the elution volume and the ratio of sample/dispersant being the two factors analyzed. The optimal extraction method was MSPD with 96 mL (acidified ethanol) as the elution volume and a 1:2 ratio of sample/dispersant. Using these conditions, 14.01 ± 0.19 mMol TEAC/100 g db (Trolox equivalent of antioxidant capacity) of grape pomace was obtained, whereas the total phenolic content was 2836.73 ± 41.90 mg GAE/100 g db. These values are greater than those obtained by maceration. These conditions are close to those predicted by the model (analysis of variance (ANOVA) with a level of significance of 5% (p < 0.05) and a Tukey comparison test for determining significant differences in the comparison of results).
{"title":"Optimization of the Extraction of Bioactive Compounds from Cabernet Sauvignon Grape Pomace from Querétaro, Mexico, Using MSPD","authors":"Tellez-Robles Daniela, López-Cortez Ma. del Socorro, Santoyo-Tepole Fortunata, Rosales-Martínez Patricia, García-Ochoa Felipe, Hernández-Botello Mayuric Teresa, Salgdo-Cruz María de la Paz","doi":"10.3390/separations11010013","DOIUrl":"https://doi.org/10.3390/separations11010013","url":null,"abstract":"Red wine contains polyphenols which are extracted during the winemaking process. However, winemaking is not an extraction; therefore, the resulting byproducts still have a substantial polyphenol content. The aim of this study was to compare two methods for the extraction of phenolic compounds: maceration and matrix solid-phase dispersion (MSPD). Grape pomace (Vitis vinifera var. Cabernet Sauvignon) from a winery in Querétaro, Mexico was used. The optimal conditions for both methods were identified. Phenolic compounds and antioxidant activity were the response variables. A central composite design was used (Minitab 17) for the extraction by maceration. The maceration time (1, 4, 12, 20, and 24 h) and the ratio of ethanol (50 to 80%) acidified with 1% HCl were the two factors studied. For the MSPD extraction, sea sand was used as a dispersant, and a 22 factorial design was employed for the evaluation, with the elution volume and the ratio of sample/dispersant being the two factors analyzed. The optimal extraction method was MSPD with 96 mL (acidified ethanol) as the elution volume and a 1:2 ratio of sample/dispersant. Using these conditions, 14.01 ± 0.19 mMol TEAC/100 g db (Trolox equivalent of antioxidant capacity) of grape pomace was obtained, whereas the total phenolic content was 2836.73 ± 41.90 mg GAE/100 g db. These values are greater than those obtained by maceration. These conditions are close to those predicted by the model (analysis of variance (ANOVA) with a level of significance of 5% (p < 0.05) and a Tukey comparison test for determining significant differences in the comparison of results).","PeriodicalId":21833,"journal":{"name":"Separations","volume":"27 36","pages":""},"PeriodicalIF":2.6,"publicationDate":"2023-12-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139148252","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-12-25DOI: 10.3390/separations11010008
Ş. Kurhan, K. Hanková, P. Klouček, M. Koudela
Straw is an important by-product of crop production. It has been widely used as a feed as well as in fruit–vegetable production due to exerting a positive impact on soil and crop health and quality in the operated areas. On the other hand, applied crop-specific herbicides throughout the production stage, like aminopyralid (AP), may lead to significant plant injuries in sensitive vegetable plantations, even in very low concentrations. This study aims to optimize a short time, minimal consumables needed, and sensitive extraction and analytical method for AP residues in straw material using LC-MS/MS. For this purpose, standard AP signal response in acetonitrile (MeCN) and 1% of formic acid (FA) in methanol (MeOH) were tested; several chromatographic separation and mass spectroscopy (MS) parameters were improved and optimized. Subsequently, two different extraction methods were performed in AP spiked straw samples, and extraction efficacies were compared. Salting-out assisted liquid–liquid extraction (SALLE) by acidified MeCN combined with final dissolution in MeOH with 1% of FA prior to the analysis was chosen as the most appropriate method for the straw matrix. This method was then used for validation and real sample test analysis. The limit of quantification (LOQ) of AP in this optimized extraction method achieved 10 ng/g straw with a recovery rate of 71% and 13% RSD. The method was also tested on field straw mulch samples and 22.54 ± 0.8 ng/g of AP was detected.
秸秆是农作物生产的重要副产品。秸秆被广泛用作饲料和蔬菜水果生产的原料，因为它对操作区的土壤和作物健康及质量有积极影响。另一方面，在整个生产阶段施用作物专用除草剂，如氨基吡啶甲酸盐（AP），即使浓度很低，也可能对敏感的蔬菜种植园造成严重的植物伤害。本研究旨在优化一种时间短、耗材少、灵敏度高的提取和分析方法，利用 LC-MS/MS 对秸秆材料中的 AP 残留进行分析。为此，测试了乙腈（MeCN）和甲醇（MeOH）中 1%甲酸（FA）的标准 AP 信号响应；改进并优化了多个色谱分离和质谱（MS）参数。随后，对添加了 AP 的秸秆样品进行了两种不同的萃取方法，并比较了萃取效果。对于秸秆基质，最合适的方法是采用酸化的 MeCN 进行盐析辅助液液萃取（SALLE），并在分析前用含 1%FA的 MeOH 进行最终溶解。该方法随后被用于验证和实际样品测试分析。在这种优化的提取方法中，AP 的定量限 (LOQ) 为 10 纳克/克秸秆，回收率为 71%，RSD 为 13%。该方法还在田间秸秆地膜样品中进行了测试，检测到了 22.54 ± 0.8 纳克/克的 AP。
{"title":"Method Development for Aminopyralid Residues Determination by Ultra-High-Performance Liquid Chromatography Coupled to Tandem Mass Spectrometry in Straw","authors":"Ş. Kurhan, K. Hanková, P. Klouček, M. Koudela","doi":"10.3390/separations11010008","DOIUrl":"https://doi.org/10.3390/separations11010008","url":null,"abstract":"Straw is an important by-product of crop production. It has been widely used as a feed as well as in fruit–vegetable production due to exerting a positive impact on soil and crop health and quality in the operated areas. On the other hand, applied crop-specific herbicides throughout the production stage, like aminopyralid (AP), may lead to significant plant injuries in sensitive vegetable plantations, even in very low concentrations. This study aims to optimize a short time, minimal consumables needed, and sensitive extraction and analytical method for AP residues in straw material using LC-MS/MS. For this purpose, standard AP signal response in acetonitrile (MeCN) and 1% of formic acid (FA) in methanol (MeOH) were tested; several chromatographic separation and mass spectroscopy (MS) parameters were improved and optimized. Subsequently, two different extraction methods were performed in AP spiked straw samples, and extraction efficacies were compared. Salting-out assisted liquid–liquid extraction (SALLE) by acidified MeCN combined with final dissolution in MeOH with 1% of FA prior to the analysis was chosen as the most appropriate method for the straw matrix. This method was then used for validation and real sample test analysis. The limit of quantification (LOQ) of AP in this optimized extraction method achieved 10 ng/g straw with a recovery rate of 71% and 13% RSD. The method was also tested on field straw mulch samples and 22.54 ± 0.8 ng/g of AP was detected.","PeriodicalId":21833,"journal":{"name":"Separations","volume":"9 1","pages":""},"PeriodicalIF":2.6,"publicationDate":"2023-12-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139159680","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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