Pub Date : 2024-02-14DOI: 10.3390/separations11020059
Zeinab Rabiei, Andrew Simons, Magdalena Folkmanova, Tereza Vesela, O. Uhlík, E. Kozliak, Alena Kubátová
Lignin, a complex and abundant biopolymer, is a major constituent of plant cell walls. Due to its chemical and structural complexity, lignin degradation is a challenging task for both natural and engineered systems. Therefore, investigation of lignin degradation using so called “model compounds” has been the focus of many research efforts in recent years. This study addresses the utility of guaiacylglycerol-β-guaiacyl ether (Gβ2) as a model compound for evaluating the β-O-4 bond cleavage under diverse thermal and aqueous medium conditions. Experimental conditions included varied pH (3–10), microbial biodegradation, subcritical water environment (150–250 °C), and mild pyrolysis (150–250 °C). A high-performance liquid chromatography with high-resolution mass spectrometry was employed for accurate detection and quantification of both Gβ2 and its degradation/modification products in an aqueous environment. Pyrolysis experiments were performed using gas chromatography-mass spectrometry analysis with a pyrolyzer. The results showed that Gβ2 remained stable under exposure to moderate pH and several bacterial strains, which were successfully used previously for biodegradation of other recalcitrant pollutants. We report, for the first time, differing Gβ2 breakdown pathways for subcritical water treatment vs. pyrolysis under an inert atmosphere. The scientific novelty lies in the presentation of differences in the degradation pathways of Gβ2 during subcritical water treatment compared to pyrolysis in an inert atmosphere, with water playing a key role. The observed differences are ascribed to the suppression of homolytic reactions by water as a solvent.
{"title":"Stability and Reactivity of Guaiacylglycerol-β-Guaiacyl Ether, a Compound Modeling β-O-4 Linkage in Lignin","authors":"Zeinab Rabiei, Andrew Simons, Magdalena Folkmanova, Tereza Vesela, O. Uhlík, E. Kozliak, Alena Kubátová","doi":"10.3390/separations11020059","DOIUrl":"https://doi.org/10.3390/separations11020059","url":null,"abstract":"Lignin, a complex and abundant biopolymer, is a major constituent of plant cell walls. Due to its chemical and structural complexity, lignin degradation is a challenging task for both natural and engineered systems. Therefore, investigation of lignin degradation using so called “model compounds” has been the focus of many research efforts in recent years. This study addresses the utility of guaiacylglycerol-β-guaiacyl ether (Gβ2) as a model compound for evaluating the β-O-4 bond cleavage under diverse thermal and aqueous medium conditions. Experimental conditions included varied pH (3–10), microbial biodegradation, subcritical water environment (150–250 °C), and mild pyrolysis (150–250 °C). A high-performance liquid chromatography with high-resolution mass spectrometry was employed for accurate detection and quantification of both Gβ2 and its degradation/modification products in an aqueous environment. Pyrolysis experiments were performed using gas chromatography-mass spectrometry analysis with a pyrolyzer. The results showed that Gβ2 remained stable under exposure to moderate pH and several bacterial strains, which were successfully used previously for biodegradation of other recalcitrant pollutants. We report, for the first time, differing Gβ2 breakdown pathways for subcritical water treatment vs. pyrolysis under an inert atmosphere. The scientific novelty lies in the presentation of differences in the degradation pathways of Gβ2 during subcritical water treatment compared to pyrolysis in an inert atmosphere, with water playing a key role. The observed differences are ascribed to the suppression of homolytic reactions by water as a solvent.","PeriodicalId":510456,"journal":{"name":"Separations","volume":"466 4","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-02-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139839073","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 : 2024-02-13DOI: 10.3390/separations11020058
Nadin Boegelsack, James Walker, Court D. Sandau, D. McMartin, Jonathan M. Withey, Gwen O'Sullivan
Producing defensible data for legal proceedings requires strict monitoring of sample integrity. In fire debris analysis, various approved packaging and storage solutions are designed to achieve this by preventing cross-contamination. This study examines the efficiency of current practices at preventing cross-contamination in the presence of a sample matrix (charred wood) via analysis by comprehensive multidimensional gas chromatography coupled with time-of-flight mass spectrometry (GC×GC-ToF MS). The transfer of ignitable liquid residue (ILR) was assessed by comparing percentages of the target ILR area relative to the total chromatogram area and applying chemometric tools developed to detect cross-contamination. All practices reduced cross-contamination in comparison to faulty packaging. Individual practices varied in their performance. Nylon-based packaging performed best, whereas commercial polyethylene-based packaging performed worst due to interfering compounds emitted from the material and sealing mechanism. Heat-sealing was the best sealing mechanism when applied correctly, followed by press-fit connections, and lastly, adhesive sealing. Refrigerated storage offered several advantages, with elevated impact for polyethylene-based packaging and adhesive sealing mechanisms. Triple-layer packaging practices did not show significant benefits over double-layers. The recommended packaging approach based on these findings is mixed-material packaging (metal quart can in a heat-sealed nylon bag), offering advanced prevention of cross-contamination and practical advantages with continued refrigeration during transport.
{"title":"Cross-Contamination of Ignitable Liquid Residues on Wildfire Debris—Effects of Packaging and Storage on Detection and Characterization","authors":"Nadin Boegelsack, James Walker, Court D. Sandau, D. McMartin, Jonathan M. Withey, Gwen O'Sullivan","doi":"10.3390/separations11020058","DOIUrl":"https://doi.org/10.3390/separations11020058","url":null,"abstract":"Producing defensible data for legal proceedings requires strict monitoring of sample integrity. In fire debris analysis, various approved packaging and storage solutions are designed to achieve this by preventing cross-contamination. This study examines the efficiency of current practices at preventing cross-contamination in the presence of a sample matrix (charred wood) via analysis by comprehensive multidimensional gas chromatography coupled with time-of-flight mass spectrometry (GC×GC-ToF MS). The transfer of ignitable liquid residue (ILR) was assessed by comparing percentages of the target ILR area relative to the total chromatogram area and applying chemometric tools developed to detect cross-contamination. All practices reduced cross-contamination in comparison to faulty packaging. Individual practices varied in their performance. Nylon-based packaging performed best, whereas commercial polyethylene-based packaging performed worst due to interfering compounds emitted from the material and sealing mechanism. Heat-sealing was the best sealing mechanism when applied correctly, followed by press-fit connections, and lastly, adhesive sealing. Refrigerated storage offered several advantages, with elevated impact for polyethylene-based packaging and adhesive sealing mechanisms. Triple-layer packaging practices did not show significant benefits over double-layers. The recommended packaging approach based on these findings is mixed-material packaging (metal quart can in a heat-sealed nylon bag), offering advanced prevention of cross-contamination and practical advantages with continued refrigeration during transport.","PeriodicalId":510456,"journal":{"name":"Separations","volume":"38 16","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-02-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139780074","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 : 2024-02-13DOI: 10.3390/separations11020058
Nadin Boegelsack, James Walker, Court D. Sandau, D. McMartin, Jonathan M. Withey, Gwen O'Sullivan
Producing defensible data for legal proceedings requires strict monitoring of sample integrity. In fire debris analysis, various approved packaging and storage solutions are designed to achieve this by preventing cross-contamination. This study examines the efficiency of current practices at preventing cross-contamination in the presence of a sample matrix (charred wood) via analysis by comprehensive multidimensional gas chromatography coupled with time-of-flight mass spectrometry (GC×GC-ToF MS). The transfer of ignitable liquid residue (ILR) was assessed by comparing percentages of the target ILR area relative to the total chromatogram area and applying chemometric tools developed to detect cross-contamination. All practices reduced cross-contamination in comparison to faulty packaging. Individual practices varied in their performance. Nylon-based packaging performed best, whereas commercial polyethylene-based packaging performed worst due to interfering compounds emitted from the material and sealing mechanism. Heat-sealing was the best sealing mechanism when applied correctly, followed by press-fit connections, and lastly, adhesive sealing. Refrigerated storage offered several advantages, with elevated impact for polyethylene-based packaging and adhesive sealing mechanisms. Triple-layer packaging practices did not show significant benefits over double-layers. The recommended packaging approach based on these findings is mixed-material packaging (metal quart can in a heat-sealed nylon bag), offering advanced prevention of cross-contamination and practical advantages with continued refrigeration during transport.
{"title":"Cross-Contamination of Ignitable Liquid Residues on Wildfire Debris—Effects of Packaging and Storage on Detection and Characterization","authors":"Nadin Boegelsack, James Walker, Court D. Sandau, D. McMartin, Jonathan M. Withey, Gwen O'Sullivan","doi":"10.3390/separations11020058","DOIUrl":"https://doi.org/10.3390/separations11020058","url":null,"abstract":"Producing defensible data for legal proceedings requires strict monitoring of sample integrity. In fire debris analysis, various approved packaging and storage solutions are designed to achieve this by preventing cross-contamination. This study examines the efficiency of current practices at preventing cross-contamination in the presence of a sample matrix (charred wood) via analysis by comprehensive multidimensional gas chromatography coupled with time-of-flight mass spectrometry (GC×GC-ToF MS). The transfer of ignitable liquid residue (ILR) was assessed by comparing percentages of the target ILR area relative to the total chromatogram area and applying chemometric tools developed to detect cross-contamination. All practices reduced cross-contamination in comparison to faulty packaging. Individual practices varied in their performance. Nylon-based packaging performed best, whereas commercial polyethylene-based packaging performed worst due to interfering compounds emitted from the material and sealing mechanism. Heat-sealing was the best sealing mechanism when applied correctly, followed by press-fit connections, and lastly, adhesive sealing. Refrigerated storage offered several advantages, with elevated impact for polyethylene-based packaging and adhesive sealing mechanisms. Triple-layer packaging practices did not show significant benefits over double-layers. The recommended packaging approach based on these findings is mixed-material packaging (metal quart can in a heat-sealed nylon bag), offering advanced prevention of cross-contamination and practical advantages with continued refrigeration during transport.","PeriodicalId":510456,"journal":{"name":"Separations","volume":"180 3","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-02-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139840006","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 : 2024-02-12DOI: 10.3390/separations11020057
Krastena Nikolova, N. Petkova, D. Mihaylova, G. Gentscheva, Georgi Gavrailov, Ivaylo Pehlivanov, V. Andonova
Phycocyanin is a pigment–protein complex from the group of phycobiliproteins obtained from Spirulina (Arthrospira platensis), with possibilities for various applications in food and pharmaceutical technologies. It is a natural colorant for food and cosmetic products. This study aimed to investigate the effect of ultrasonic and microwave extraction conditions on antioxidant activity (AOA), chlorophyll content, and the content and purity index of phycocyanin in aqueous and alcoholic extracts of Spirulina (Arthrospira platensis). For this purpose, ultrasonic extraction with water or ethanol was performed at 20 °C, 30 °C, and 40 °C for 1, 2, and 3 h at an ultrasonic frequency of 36 kHz, 40 kHz, and 45 kHz. Microwave water extraction was performed for 60 s, 120 s, and 180 s. For each of the obtained samples, three parallel measurements of antioxidant activity were made by DPPH and FRAP methods, and chlorophyll content and phycocyanin yield and purity index were determined spectrophotometrically. Ultrasonic extraction resulted in a higher yield and purity index of phycocyanin compared to microwave extraction. The highest yield of 14.88 mg g−1 with a purity index of 1.60 was achieved at a temperature of 40 °C for one hour and an ultrasonic wave frequency of 40 kHz. A relatively low yield of 4.21 mg g−1, but with a purity index of 2.67, was obtained at a temperature of 30 °C, a time of two hours, and an ultrasonic frequency of 40 kHz. Chlorophyll b content at 20 °C, for two hours and ultrasonic frequency 40 kHz was 1.400 mg g−1. The study proposes ultrasonic extraction as a green method to obtain phycocyanin of varying purity index that may be used for food, cosmetic, or biomedical purposes.
{"title":"Extraction of Phycocyanin and Chlorophyll from Spirulina by “Green Methods”","authors":"Krastena Nikolova, N. Petkova, D. Mihaylova, G. Gentscheva, Georgi Gavrailov, Ivaylo Pehlivanov, V. Andonova","doi":"10.3390/separations11020057","DOIUrl":"https://doi.org/10.3390/separations11020057","url":null,"abstract":"Phycocyanin is a pigment–protein complex from the group of phycobiliproteins obtained from Spirulina (Arthrospira platensis), with possibilities for various applications in food and pharmaceutical technologies. It is a natural colorant for food and cosmetic products. This study aimed to investigate the effect of ultrasonic and microwave extraction conditions on antioxidant activity (AOA), chlorophyll content, and the content and purity index of phycocyanin in aqueous and alcoholic extracts of Spirulina (Arthrospira platensis). For this purpose, ultrasonic extraction with water or ethanol was performed at 20 °C, 30 °C, and 40 °C for 1, 2, and 3 h at an ultrasonic frequency of 36 kHz, 40 kHz, and 45 kHz. Microwave water extraction was performed for 60 s, 120 s, and 180 s. For each of the obtained samples, three parallel measurements of antioxidant activity were made by DPPH and FRAP methods, and chlorophyll content and phycocyanin yield and purity index were determined spectrophotometrically. Ultrasonic extraction resulted in a higher yield and purity index of phycocyanin compared to microwave extraction. The highest yield of 14.88 mg g−1 with a purity index of 1.60 was achieved at a temperature of 40 °C for one hour and an ultrasonic wave frequency of 40 kHz. A relatively low yield of 4.21 mg g−1, but with a purity index of 2.67, was obtained at a temperature of 30 °C, a time of two hours, and an ultrasonic frequency of 40 kHz. Chlorophyll b content at 20 °C, for two hours and ultrasonic frequency 40 kHz was 1.400 mg g−1. The study proposes ultrasonic extraction as a green method to obtain phycocyanin of varying purity index that may be used for food, cosmetic, or biomedical purposes.","PeriodicalId":510456,"journal":{"name":"Separations","volume":"124 38","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-02-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139785032","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 : 2024-02-12DOI: 10.3390/separations11020057
Krastena Nikolova, N. Petkova, D. Mihaylova, G. Gentscheva, Georgi Gavrailov, Ivaylo Pehlivanov, V. Andonova
Phycocyanin is a pigment–protein complex from the group of phycobiliproteins obtained from Spirulina (Arthrospira platensis), with possibilities for various applications in food and pharmaceutical technologies. It is a natural colorant for food and cosmetic products. This study aimed to investigate the effect of ultrasonic and microwave extraction conditions on antioxidant activity (AOA), chlorophyll content, and the content and purity index of phycocyanin in aqueous and alcoholic extracts of Spirulina (Arthrospira platensis). For this purpose, ultrasonic extraction with water or ethanol was performed at 20 °C, 30 °C, and 40 °C for 1, 2, and 3 h at an ultrasonic frequency of 36 kHz, 40 kHz, and 45 kHz. Microwave water extraction was performed for 60 s, 120 s, and 180 s. For each of the obtained samples, three parallel measurements of antioxidant activity were made by DPPH and FRAP methods, and chlorophyll content and phycocyanin yield and purity index were determined spectrophotometrically. Ultrasonic extraction resulted in a higher yield and purity index of phycocyanin compared to microwave extraction. The highest yield of 14.88 mg g−1 with a purity index of 1.60 was achieved at a temperature of 40 °C for one hour and an ultrasonic wave frequency of 40 kHz. A relatively low yield of 4.21 mg g−1, but with a purity index of 2.67, was obtained at a temperature of 30 °C, a time of two hours, and an ultrasonic frequency of 40 kHz. Chlorophyll b content at 20 °C, for two hours and ultrasonic frequency 40 kHz was 1.400 mg g−1. The study proposes ultrasonic extraction as a green method to obtain phycocyanin of varying purity index that may be used for food, cosmetic, or biomedical purposes.
{"title":"Extraction of Phycocyanin and Chlorophyll from Spirulina by “Green Methods”","authors":"Krastena Nikolova, N. Petkova, D. Mihaylova, G. Gentscheva, Georgi Gavrailov, Ivaylo Pehlivanov, V. Andonova","doi":"10.3390/separations11020057","DOIUrl":"https://doi.org/10.3390/separations11020057","url":null,"abstract":"Phycocyanin is a pigment–protein complex from the group of phycobiliproteins obtained from Spirulina (Arthrospira platensis), with possibilities for various applications in food and pharmaceutical technologies. It is a natural colorant for food and cosmetic products. This study aimed to investigate the effect of ultrasonic and microwave extraction conditions on antioxidant activity (AOA), chlorophyll content, and the content and purity index of phycocyanin in aqueous and alcoholic extracts of Spirulina (Arthrospira platensis). For this purpose, ultrasonic extraction with water or ethanol was performed at 20 °C, 30 °C, and 40 °C for 1, 2, and 3 h at an ultrasonic frequency of 36 kHz, 40 kHz, and 45 kHz. Microwave water extraction was performed for 60 s, 120 s, and 180 s. For each of the obtained samples, three parallel measurements of antioxidant activity were made by DPPH and FRAP methods, and chlorophyll content and phycocyanin yield and purity index were determined spectrophotometrically. Ultrasonic extraction resulted in a higher yield and purity index of phycocyanin compared to microwave extraction. The highest yield of 14.88 mg g−1 with a purity index of 1.60 was achieved at a temperature of 40 °C for one hour and an ultrasonic wave frequency of 40 kHz. A relatively low yield of 4.21 mg g−1, but with a purity index of 2.67, was obtained at a temperature of 30 °C, a time of two hours, and an ultrasonic frequency of 40 kHz. Chlorophyll b content at 20 °C, for two hours and ultrasonic frequency 40 kHz was 1.400 mg g−1. The study proposes ultrasonic extraction as a green method to obtain phycocyanin of varying purity index that may be used for food, cosmetic, or biomedical purposes.","PeriodicalId":510456,"journal":{"name":"Separations","volume":"52 20","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-02-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139845052","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 : 2024-02-10DOI: 10.3390/separations11020056
F. Buthmann, Philip Laby, Djamal Hamza, J. Koop, Gerhard Schembecker
Centrifugal Partition Chromatography (CPC) is a separation technique that utilizes immiscible liquid phases to purify compounds. The selection of solvents in Liquid–Liquid Chromatography offers flexibility and optimization possibilities for specific separation tasks. Understanding the hydrodynamics inside the apparatus is crucial for optimizing a CPC process. The phase retention ratio (Sf) determines the apparatus’s operating point and separation efficiency. However, stationary phase leakage, known as bleeding, complicates the immobilization of this phase. We used a partly transparent single-disc rotor to investigate the time and space dependency of bleeding inside a CPC apparatus, enabling real-time and localized determination of the phase retention ratio. By tracking the retention values over time, we observed the bleeding phenomenon and its progression from the inlet to the rotor outlet. Depending on the phase system used, the CPC was utilizable for a separation task for only 173–500 dimensionless residence times. Systems with a higher stability parameter (as described in the literature) showed a lower bleeding rate and increased stability over time. Accordingly, our results demonstrate the importance of maintaining an optimal ratio of mobile to stationary phase for efficient separation.
{"title":"Spatially and Temporally Resolved Analysis of Bleeding in a Centrifugal Partition Chromatography Rotor","authors":"F. Buthmann, Philip Laby, Djamal Hamza, J. Koop, Gerhard Schembecker","doi":"10.3390/separations11020056","DOIUrl":"https://doi.org/10.3390/separations11020056","url":null,"abstract":"Centrifugal Partition Chromatography (CPC) is a separation technique that utilizes immiscible liquid phases to purify compounds. The selection of solvents in Liquid–Liquid Chromatography offers flexibility and optimization possibilities for specific separation tasks. Understanding the hydrodynamics inside the apparatus is crucial for optimizing a CPC process. The phase retention ratio (Sf) determines the apparatus’s operating point and separation efficiency. However, stationary phase leakage, known as bleeding, complicates the immobilization of this phase. We used a partly transparent single-disc rotor to investigate the time and space dependency of bleeding inside a CPC apparatus, enabling real-time and localized determination of the phase retention ratio. By tracking the retention values over time, we observed the bleeding phenomenon and its progression from the inlet to the rotor outlet. Depending on the phase system used, the CPC was utilizable for a separation task for only 173–500 dimensionless residence times. Systems with a higher stability parameter (as described in the literature) showed a lower bleeding rate and increased stability over time. Accordingly, our results demonstrate the importance of maintaining an optimal ratio of mobile to stationary phase for efficient separation.","PeriodicalId":510456,"journal":{"name":"Separations","volume":" 13","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-02-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139787530","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 : 2024-02-10DOI: 10.3390/separations11020056
F. Buthmann, Philip Laby, Djamal Hamza, J. Koop, Gerhard Schembecker
Centrifugal Partition Chromatography (CPC) is a separation technique that utilizes immiscible liquid phases to purify compounds. The selection of solvents in Liquid–Liquid Chromatography offers flexibility and optimization possibilities for specific separation tasks. Understanding the hydrodynamics inside the apparatus is crucial for optimizing a CPC process. The phase retention ratio (Sf) determines the apparatus’s operating point and separation efficiency. However, stationary phase leakage, known as bleeding, complicates the immobilization of this phase. We used a partly transparent single-disc rotor to investigate the time and space dependency of bleeding inside a CPC apparatus, enabling real-time and localized determination of the phase retention ratio. By tracking the retention values over time, we observed the bleeding phenomenon and its progression from the inlet to the rotor outlet. Depending on the phase system used, the CPC was utilizable for a separation task for only 173–500 dimensionless residence times. Systems with a higher stability parameter (as described in the literature) showed a lower bleeding rate and increased stability over time. Accordingly, our results demonstrate the importance of maintaining an optimal ratio of mobile to stationary phase for efficient separation.
{"title":"Spatially and Temporally Resolved Analysis of Bleeding in a Centrifugal Partition Chromatography Rotor","authors":"F. Buthmann, Philip Laby, Djamal Hamza, J. Koop, Gerhard Schembecker","doi":"10.3390/separations11020056","DOIUrl":"https://doi.org/10.3390/separations11020056","url":null,"abstract":"Centrifugal Partition Chromatography (CPC) is a separation technique that utilizes immiscible liquid phases to purify compounds. The selection of solvents in Liquid–Liquid Chromatography offers flexibility and optimization possibilities for specific separation tasks. Understanding the hydrodynamics inside the apparatus is crucial for optimizing a CPC process. The phase retention ratio (Sf) determines the apparatus’s operating point and separation efficiency. However, stationary phase leakage, known as bleeding, complicates the immobilization of this phase. We used a partly transparent single-disc rotor to investigate the time and space dependency of bleeding inside a CPC apparatus, enabling real-time and localized determination of the phase retention ratio. By tracking the retention values over time, we observed the bleeding phenomenon and its progression from the inlet to the rotor outlet. Depending on the phase system used, the CPC was utilizable for a separation task for only 173–500 dimensionless residence times. Systems with a higher stability parameter (as described in the literature) showed a lower bleeding rate and increased stability over time. Accordingly, our results demonstrate the importance of maintaining an optimal ratio of mobile to stationary phase for efficient separation.","PeriodicalId":510456,"journal":{"name":"Separations","volume":"122 1-4","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-02-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139847414","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 : 2024-02-08DOI: 10.3390/separations11020055
Ayah Nader Abu-shark, A. Shakya, Safwan M. Al-Adwan, R. Naik
Perampanel, a novel α-amino-3-hydroxy-5-methyl-4-isoxazolepropionic acid (AMPA) receptor antagonist, is registered for the adjunctive treatment of patients (aged ≥ 12 years) with refractory partial-onset seizures. A simple high-performance liquid chromatographic method fluorescence detection (HPLC-FLD) was developed to analyze perampanel in rats’ plasma and validated for bioanalytical purposes. Rats’ plasma (50 µL) was processed by microextraction packed sorbent (MEPS). The analytes were separated using a Hypersil Gold octadecyl silane column (250 × 4.6 mm internal diameter, 5 μm particle size) with isocratic elution. A mobile phase consisting of acetonitrile–methanol–water (275:275:450, v/v/v; containing 50 µL triethylamine and pH adjusted to 3.25 with orthophosphoric acid) was used in this analysis. The flow rate was 1.25 mL/min. Analytes were monitored at an excitation wavelength of 285 nm and an emission wavelength of 430 nm. The linearity range for this validated method was from 3.75 to 300 ng/mL. No endogenous peaks were found in the elution of analytes in drug-free rats’ plasma. Intra- and inter-batch reproducibility studies demonstrated accuracy and precision within the acceptance criteria. The results indicate that the present method is simple, selective, reproducible, and suitable for the analysis of perampanel in small volume samples. The robustness of the method was accessed using MODDE® design of experiments software version 12.5.
{"title":"Development and Validation of HPLC-FLD Analysis of Perampanel in MEPS-Processed Rat Plasma Sample","authors":"Ayah Nader Abu-shark, A. Shakya, Safwan M. Al-Adwan, R. Naik","doi":"10.3390/separations11020055","DOIUrl":"https://doi.org/10.3390/separations11020055","url":null,"abstract":"Perampanel, a novel α-amino-3-hydroxy-5-methyl-4-isoxazolepropionic acid (AMPA) receptor antagonist, is registered for the adjunctive treatment of patients (aged ≥ 12 years) with refractory partial-onset seizures. A simple high-performance liquid chromatographic method fluorescence detection (HPLC-FLD) was developed to analyze perampanel in rats’ plasma and validated for bioanalytical purposes. Rats’ plasma (50 µL) was processed by microextraction packed sorbent (MEPS). The analytes were separated using a Hypersil Gold octadecyl silane column (250 × 4.6 mm internal diameter, 5 μm particle size) with isocratic elution. A mobile phase consisting of acetonitrile–methanol–water (275:275:450, v/v/v; containing 50 µL triethylamine and pH adjusted to 3.25 with orthophosphoric acid) was used in this analysis. The flow rate was 1.25 mL/min. Analytes were monitored at an excitation wavelength of 285 nm and an emission wavelength of 430 nm. The linearity range for this validated method was from 3.75 to 300 ng/mL. No endogenous peaks were found in the elution of analytes in drug-free rats’ plasma. Intra- and inter-batch reproducibility studies demonstrated accuracy and precision within the acceptance criteria. The results indicate that the present method is simple, selective, reproducible, and suitable for the analysis of perampanel in small volume samples. The robustness of the method was accessed using MODDE® design of experiments software version 12.5.","PeriodicalId":510456,"journal":{"name":"Separations","volume":" 2","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-02-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139791278","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 : 2024-02-08DOI: 10.3390/separations11020055
Ayah Nader Abu-shark, A. Shakya, Safwan M. Al-Adwan, R. Naik
Perampanel, a novel α-amino-3-hydroxy-5-methyl-4-isoxazolepropionic acid (AMPA) receptor antagonist, is registered for the adjunctive treatment of patients (aged ≥ 12 years) with refractory partial-onset seizures. A simple high-performance liquid chromatographic method fluorescence detection (HPLC-FLD) was developed to analyze perampanel in rats’ plasma and validated for bioanalytical purposes. Rats’ plasma (50 µL) was processed by microextraction packed sorbent (MEPS). The analytes were separated using a Hypersil Gold octadecyl silane column (250 × 4.6 mm internal diameter, 5 μm particle size) with isocratic elution. A mobile phase consisting of acetonitrile–methanol–water (275:275:450, v/v/v; containing 50 µL triethylamine and pH adjusted to 3.25 with orthophosphoric acid) was used in this analysis. The flow rate was 1.25 mL/min. Analytes were monitored at an excitation wavelength of 285 nm and an emission wavelength of 430 nm. The linearity range for this validated method was from 3.75 to 300 ng/mL. No endogenous peaks were found in the elution of analytes in drug-free rats’ plasma. Intra- and inter-batch reproducibility studies demonstrated accuracy and precision within the acceptance criteria. The results indicate that the present method is simple, selective, reproducible, and suitable for the analysis of perampanel in small volume samples. The robustness of the method was accessed using MODDE® design of experiments software version 12.5.
{"title":"Development and Validation of HPLC-FLD Analysis of Perampanel in MEPS-Processed Rat Plasma Sample","authors":"Ayah Nader Abu-shark, A. Shakya, Safwan M. Al-Adwan, R. Naik","doi":"10.3390/separations11020055","DOIUrl":"https://doi.org/10.3390/separations11020055","url":null,"abstract":"Perampanel, a novel α-amino-3-hydroxy-5-methyl-4-isoxazolepropionic acid (AMPA) receptor antagonist, is registered for the adjunctive treatment of patients (aged ≥ 12 years) with refractory partial-onset seizures. A simple high-performance liquid chromatographic method fluorescence detection (HPLC-FLD) was developed to analyze perampanel in rats’ plasma and validated for bioanalytical purposes. Rats’ plasma (50 µL) was processed by microextraction packed sorbent (MEPS). The analytes were separated using a Hypersil Gold octadecyl silane column (250 × 4.6 mm internal diameter, 5 μm particle size) with isocratic elution. A mobile phase consisting of acetonitrile–methanol–water (275:275:450, v/v/v; containing 50 µL triethylamine and pH adjusted to 3.25 with orthophosphoric acid) was used in this analysis. The flow rate was 1.25 mL/min. Analytes were monitored at an excitation wavelength of 285 nm and an emission wavelength of 430 nm. The linearity range for this validated method was from 3.75 to 300 ng/mL. No endogenous peaks were found in the elution of analytes in drug-free rats’ plasma. Intra- and inter-batch reproducibility studies demonstrated accuracy and precision within the acceptance criteria. The results indicate that the present method is simple, selective, reproducible, and suitable for the analysis of perampanel in small volume samples. The robustness of the method was accessed using MODDE® design of experiments software version 12.5.","PeriodicalId":510456,"journal":{"name":"Separations","volume":"123 4","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-02-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139851006","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 : 2024-02-07DOI: 10.3390/separations11020052
Luz Fanny Echeverri-Giraldo, Valentina Osorio Pérez, Claudia Tabares Arboleda, Lady Juliet Vargas Gutiérrez, Luis Carlos Imbachi Quinchua
Cesar, a coffee-growing department in Colombia, has particular characteristics that favor the production of coffees differentiated by sensory profile, for which the acidity attribute stands out. The chemical composition and sensory quality of the coffee produced by 160 coffee growers during two production harvests (2021 and 2022) and processed by the wet method were evaluated to correlate the contents of the main acidic chemical compounds present in green coffee beans with the perceived acidity of the beverage. The chemical analysis of coffee samples utilized spectrophotometric methods and HPLC-DAD techniques. Lactic, 3,5-di-CQA and phosphoric acids were good discriminators of acidity classified as excellent; that is, with a score higher than 7.75 on the Specialty Coffee Association (SCA) scale, presenting the highest contents in the green coffee bean. There was a direct linear relationship between acidity and 3,5-di-CQA and 5-CQA and an inverse relationship between acidity and 3-CQA, 4-CQA and 4,5-CQA. These findings contribute to the understanding of the quality and chemistry of Colombian coffee.
{"title":"Content of Acidic Compounds in the Bean of Coffea arabica L., Produced in the Department of Cesar (Colombia), and Its Relationship with the Sensorial Attribute of Acidity","authors":"Luz Fanny Echeverri-Giraldo, Valentina Osorio Pérez, Claudia Tabares Arboleda, Lady Juliet Vargas Gutiérrez, Luis Carlos Imbachi Quinchua","doi":"10.3390/separations11020052","DOIUrl":"https://doi.org/10.3390/separations11020052","url":null,"abstract":"Cesar, a coffee-growing department in Colombia, has particular characteristics that favor the production of coffees differentiated by sensory profile, for which the acidity attribute stands out. The chemical composition and sensory quality of the coffee produced by 160 coffee growers during two production harvests (2021 and 2022) and processed by the wet method were evaluated to correlate the contents of the main acidic chemical compounds present in green coffee beans with the perceived acidity of the beverage. The chemical analysis of coffee samples utilized spectrophotometric methods and HPLC-DAD techniques. Lactic, 3,5-di-CQA and phosphoric acids were good discriminators of acidity classified as excellent; that is, with a score higher than 7.75 on the Specialty Coffee Association (SCA) scale, presenting the highest contents in the green coffee bean. There was a direct linear relationship between acidity and 3,5-di-CQA and 5-CQA and an inverse relationship between acidity and 3-CQA, 4-CQA and 4,5-CQA. These findings contribute to the understanding of the quality and chemistry of Colombian coffee.","PeriodicalId":510456,"journal":{"name":"Separations","volume":"43 1-2","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-02-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139855692","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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