Pub Date : 2023-07-03DOI: 10.1080/10826076.2023.2227893
Naella S. Valencia Pérez, A. Garrido Hernández, Francisco J. Martínez Valdez, Genaro I. Cerón Montes, Roberto García Rosales, Jorge Yáñez Fernández
Abstract In the current work, a flash chromatography method was developed to separate the main anthocyanins of blue corn; cyanidin-3-glucoside (Cy3G), peonidin-3-glucoside (Pn3G), and cyanidin-3-(6-malonylglucoside) (Cy3MG). These anthocyanins were identified by mass spectroscopy analysis. The implemented method consisted of the isocratic elution in a two-step mixture of methanol: water: acetic acid as the mobile phase (easy to remove) and C18 resin as the stationary phase. In the chromatographic method, different elution conditions were evaluated. The better condition to separate the anthocyanins with glycoside was 5% methanol and 10% acetic acid for 200 minutes of elution, followed by 200 minutes with 25% methanol and 2.5% acetic acid for the malonylglucoside forms. From the chromatograms prepared, the efficiency of the chromatographic separation was evaluated by calculating the parameters: retention factor ( ), selectivity ( ), number of theoretical plates ( ), and resolution ( ). The optimal values were determined as follows: Cy3G and Cy3MG were as follows: for Cy3G, the rretention factir (k) was dtermined to be 30.2, the selectivity (α) was 1.55, the number of theorical plates (N) was 202, and the resolution (Rs) was 1.09. For Cy3MG, the corresponding values were; k = 104.9, α =1.21, N=522, and Rs 0.093. These parameters are useful to implement separation processes of anthocyanins from other sources of pigmented corn or even others containing anthocyanins. Graphical abstract
{"title":"Study of the scale isolation of anthocyanins from blue corn by flash chromatography","authors":"Naella S. Valencia Pérez, A. Garrido Hernández, Francisco J. Martínez Valdez, Genaro I. Cerón Montes, Roberto García Rosales, Jorge Yáñez Fernández","doi":"10.1080/10826076.2023.2227893","DOIUrl":"https://doi.org/10.1080/10826076.2023.2227893","url":null,"abstract":"Abstract In the current work, a flash chromatography method was developed to separate the main anthocyanins of blue corn; cyanidin-3-glucoside (Cy3G), peonidin-3-glucoside (Pn3G), and cyanidin-3-(6-malonylglucoside) (Cy3MG). These anthocyanins were identified by mass spectroscopy analysis. The implemented method consisted of the isocratic elution in a two-step mixture of methanol: water: acetic acid as the mobile phase (easy to remove) and C18 resin as the stationary phase. In the chromatographic method, different elution conditions were evaluated. The better condition to separate the anthocyanins with glycoside was 5% methanol and 10% acetic acid for 200 minutes of elution, followed by 200 minutes with 25% methanol and 2.5% acetic acid for the malonylglucoside forms. From the chromatograms prepared, the efficiency of the chromatographic separation was evaluated by calculating the parameters: retention factor ( ), selectivity ( ), number of theoretical plates ( ), and resolution ( ). The optimal values were determined as follows: Cy3G and Cy3MG were as follows: for Cy3G, the rretention factir (k) was dtermined to be 30.2, the selectivity (α) was 1.55, the number of theorical plates (N) was 202, and the resolution (Rs) was 1.09. For Cy3MG, the corresponding values were; k = 104.9, α =1.21, N=522, and Rs 0.093. These parameters are useful to implement separation processes of anthocyanins from other sources of pigmented corn or even others containing anthocyanins. Graphical abstract","PeriodicalId":16295,"journal":{"name":"Journal of Liquid Chromatography & Related Technologies","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2023-07-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"87890846","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-07-03DOI: 10.1080/10826076.2023.2247484
Rahul Koli, V. Mannur
Abstract Aflatoxins are naturally occurring secondary metabolites generated by several molds, particularly Aspergillus flavus and Aspergillus parasiticus. They can contaminate agricultural products in the field, particularly during periods of high humidity and warmth, such as before or during harvest, or as a result of inappropriate storage, and their occurrence in the food chain is regrettably inevitable. Therefore, it is crucial to detect and measure aflatoxins. For the purpose of determining the presence of aflatoxins in various products, chromatographic methods based on high performance liquid chromatography, liquid chromatography coupled with mass spectrometry, ultra-high performance liquid chromatography coupled with mass spectrometry, high performance thin layer chromatography, and thin layer chromatography were described, along with sample preparation and risk assessment. By using several chromatographic techniques with different mobile phases and stationary phases, many analytical methods demonstrated good recovery rates of aflatoxins in a variety of products. An analysis of the existing literature indicates that from 2010 to 2022, a range of chromatographic methods have been accessible for identifying and measuring aflatoxins in food, feed, and certain herbal remedies. Although the literature shows interesting methods from an economic and environmental point of view and they can still be improved to detect aflatoxins in various products. Graphical Abstract
{"title":"Determination of aflatoxins using chromatographic methods in several foods, feed and herbal medicine products: an analytical review (from 2010 to 2022)","authors":"Rahul Koli, V. Mannur","doi":"10.1080/10826076.2023.2247484","DOIUrl":"https://doi.org/10.1080/10826076.2023.2247484","url":null,"abstract":"Abstract Aflatoxins are naturally occurring secondary metabolites generated by several molds, particularly Aspergillus flavus and Aspergillus parasiticus. They can contaminate agricultural products in the field, particularly during periods of high humidity and warmth, such as before or during harvest, or as a result of inappropriate storage, and their occurrence in the food chain is regrettably inevitable. Therefore, it is crucial to detect and measure aflatoxins. For the purpose of determining the presence of aflatoxins in various products, chromatographic methods based on high performance liquid chromatography, liquid chromatography coupled with mass spectrometry, ultra-high performance liquid chromatography coupled with mass spectrometry, high performance thin layer chromatography, and thin layer chromatography were described, along with sample preparation and risk assessment. By using several chromatographic techniques with different mobile phases and stationary phases, many analytical methods demonstrated good recovery rates of aflatoxins in a variety of products. An analysis of the existing literature indicates that from 2010 to 2022, a range of chromatographic methods have been accessible for identifying and measuring aflatoxins in food, feed, and certain herbal remedies. Although the literature shows interesting methods from an economic and environmental point of view and they can still be improved to detect aflatoxins in various products. Graphical Abstract","PeriodicalId":16295,"journal":{"name":"Journal of Liquid Chromatography & Related Technologies","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2023-07-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"45053082","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-07-03DOI: 10.1080/10826076.2023.2252495
Jake A Cravino, Richard Thomas, G. Pandey, Corey W. Manwaring, Sophie E. Parks, R. Shalliker
Abstract Blueberries are a widely consumed superfood, known for their potent phytochemical content and health benefits. Given their importance to the global food market and the current health culture, blueberries are the focal point of much inquiry into their composition, physiological benefits, and the effect of growing conditions on the quality of the final berry. Given their complex nature and the numerous factors involved in the growing and production of blueberries, there are many variables to consider when determining the chemical characteristics of blueberry samples. One important factor to control is the berry size, which, if left uncontrolled, may confound the objective information sought within the study. This communication, which utilizes HPLC and in-column derivatization for the analysis of antioxidants, shows the impact of berry size (mass/volume) on the antioxidant content and that once the size of a blueberry is controlled, sample-to-sample variations become minimized. GRAPHICAL ABSTRACT
{"title":"Exploring the relationship between blueberry size and antioxidant content","authors":"Jake A Cravino, Richard Thomas, G. Pandey, Corey W. Manwaring, Sophie E. Parks, R. Shalliker","doi":"10.1080/10826076.2023.2252495","DOIUrl":"https://doi.org/10.1080/10826076.2023.2252495","url":null,"abstract":"Abstract Blueberries are a widely consumed superfood, known for their potent phytochemical content and health benefits. Given their importance to the global food market and the current health culture, blueberries are the focal point of much inquiry into their composition, physiological benefits, and the effect of growing conditions on the quality of the final berry. Given their complex nature and the numerous factors involved in the growing and production of blueberries, there are many variables to consider when determining the chemical characteristics of blueberry samples. One important factor to control is the berry size, which, if left uncontrolled, may confound the objective information sought within the study. This communication, which utilizes HPLC and in-column derivatization for the analysis of antioxidants, shows the impact of berry size (mass/volume) on the antioxidant content and that once the size of a blueberry is controlled, sample-to-sample variations become minimized. GRAPHICAL ABSTRACT","PeriodicalId":16295,"journal":{"name":"Journal of Liquid Chromatography & Related Technologies","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2023-07-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"85427010","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-07-03DOI: 10.1080/10826076.2023.2251152
V. V. Sursyakova, V. Levdansky, A. I. Rubaylo
Abstract The influence of conditions on the separation of betulin (BT), betulinic (BIA), and betulonic (BOA) acids by reversed-phase high-performance liquid chromatography (RP-HPLC) with isocratic elution was studied. It was shown that the order of peaks in chromatograms changed with varying the acetonitrile (ACN) content in the mobile phase, and a poor separation under certain conditions was observed. The highest peak resolution with minimal retention times was at a column temperature of 20 °C, flow rate of 0.25 ml/min, and 92.5% ACN in the mobile phase. The extracts from jujube (Ziziphus jujuba) dried fruit, chaga mushroom (Inonotus obliquus), and white birch bark (Betula pendula) were studied using the obtained conditions. For extracts from the first two sources, it was found that peaks of the compound studied interfered with unknown peaks. By varying the ACN content in the mobile phase with a small step from run to run and tracking the peaks, a baseline separation was achieved. The optimal % ACN in the mobile phase was 87 and 89 for the extracts from jujube and chaga mushroom, respectively. Jujube dried fruit was found to contain, in terms of dry weight of the jujube, 0.223 ± 0.008 mg/g of BIA and 0.044 ± 0.006 mg/g of BOA. Chaga mushroom studied contains 0.022 ± 0.004 mg/g of BT and 0.062 ± 0.009 mg/g of BIA. White birch bark contains 50.9 ± 0.7 mg/g of BT, 11.2 ± 0.3 mg/g of BIA, and 2.5 ± 0.3 mg/g of BOA. GRAPHICAL ABSTRACT
{"title":"Separation of betulin and its derivatives by high-performance liquid chromatography and their determination in extracts of some plants and chaga mushroom","authors":"V. V. Sursyakova, V. Levdansky, A. I. Rubaylo","doi":"10.1080/10826076.2023.2251152","DOIUrl":"https://doi.org/10.1080/10826076.2023.2251152","url":null,"abstract":"Abstract The influence of conditions on the separation of betulin (BT), betulinic (BIA), and betulonic (BOA) acids by reversed-phase high-performance liquid chromatography (RP-HPLC) with isocratic elution was studied. It was shown that the order of peaks in chromatograms changed with varying the acetonitrile (ACN) content in the mobile phase, and a poor separation under certain conditions was observed. The highest peak resolution with minimal retention times was at a column temperature of 20 °C, flow rate of 0.25 ml/min, and 92.5% ACN in the mobile phase. The extracts from jujube (Ziziphus jujuba) dried fruit, chaga mushroom (Inonotus obliquus), and white birch bark (Betula pendula) were studied using the obtained conditions. For extracts from the first two sources, it was found that peaks of the compound studied interfered with unknown peaks. By varying the ACN content in the mobile phase with a small step from run to run and tracking the peaks, a baseline separation was achieved. The optimal % ACN in the mobile phase was 87 and 89 for the extracts from jujube and chaga mushroom, respectively. Jujube dried fruit was found to contain, in terms of dry weight of the jujube, 0.223 ± 0.008 mg/g of BIA and 0.044 ± 0.006 mg/g of BOA. Chaga mushroom studied contains 0.022 ± 0.004 mg/g of BT and 0.062 ± 0.009 mg/g of BIA. White birch bark contains 50.9 ± 0.7 mg/g of BT, 11.2 ± 0.3 mg/g of BIA, and 2.5 ± 0.3 mg/g of BOA. GRAPHICAL ABSTRACT","PeriodicalId":16295,"journal":{"name":"Journal of Liquid Chromatography & Related Technologies","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2023-07-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"91279142","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-07-03DOI: 10.1080/10826076.2023.2235402
Yulia S Sotnikova, Y. Patrushev
Abstract This paper presents examples of separation on monolithic columns prepared by two different methods: copolymerization and post-modification. In the first method, monoliths were prepared from styrene, divinylbenzene, and heterocyclic nitrogen-containing monomers. In the second, a styrene/divinylbenzene/4-vinylbenzyl chloride copolymer was obtained and in situ modified with 1-methylimidazole. It has been shown that monolithic columns are capable of separating macromolecules and low-molecular compounds. A comparison was made between a styrene/divinylbenzene/1-vinylimidazole copolymer column and a ProSwift™ RP-3U monolithic column. It has been established that a monolithic column based on 1-vinylimidazole is capable of separating proteins and low molecular weight test substances. However, the ProSwift™ RP-3U column is only capable of separating proteins. Separation examples are given: a test mixture of proteins, natural milk proteins, carbohydrates and drugs on a column with a sorbent based on styrene/divinylbenzene. A modified column was used to study the content of salicylic acid in medicinal preparations containing acetylsalicylic acid. Graphical Abstract
{"title":"Food, drug and model mix analysis by organic monolithic columns based on heterocyclic monomers","authors":"Yulia S Sotnikova, Y. Patrushev","doi":"10.1080/10826076.2023.2235402","DOIUrl":"https://doi.org/10.1080/10826076.2023.2235402","url":null,"abstract":"Abstract This paper presents examples of separation on monolithic columns prepared by two different methods: copolymerization and post-modification. In the first method, monoliths were prepared from styrene, divinylbenzene, and heterocyclic nitrogen-containing monomers. In the second, a styrene/divinylbenzene/4-vinylbenzyl chloride copolymer was obtained and in situ modified with 1-methylimidazole. It has been shown that monolithic columns are capable of separating macromolecules and low-molecular compounds. A comparison was made between a styrene/divinylbenzene/1-vinylimidazole copolymer column and a ProSwift™ RP-3U monolithic column. It has been established that a monolithic column based on 1-vinylimidazole is capable of separating proteins and low molecular weight test substances. However, the ProSwift™ RP-3U column is only capable of separating proteins. Separation examples are given: a test mixture of proteins, natural milk proteins, carbohydrates and drugs on a column with a sorbent based on styrene/divinylbenzene. A modified column was used to study the content of salicylic acid in medicinal preparations containing acetylsalicylic acid. Graphical Abstract","PeriodicalId":16295,"journal":{"name":"Journal of Liquid Chromatography & Related Technologies","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2023-07-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"85843458","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-07-03DOI: 10.1080/10826076.2023.2238824
Jiacai Hu, Xiuming Lv, Hao Zhang, B. Zhu, De-ye Liu, W. Ji
Abstract In this work, we developed a method to separate and detect inorganic antimony (iSb) in tea infusions based on liquid chromatography-inductively coupled plasma-mass spectrometry (LC-ICP-MS). Considering that iSb was present in tea infusions in trace amounts, a commercial solid-phase extraction (SPE) column was employed to enrich iSb(III) and iSb(V). In this study, we found that iSb exists in tea infusions in a bound state with an unknown substance rather than in a free state. Therefore, the enrichment step was combined with oxidation and reduction processes. Because of the enrichment process and the high sensitivity of LC-ICP-MS, the LODs of iSb(III) and iSb(V) were both as low as 0.03 μg L−1. The RSDs (n = 6) of iSb(III) and iSb(V) were all below 8.1%, and the recoveries (n = 6) were 92–96% and 90–94%, respectively. Then, a total of six tea infusion samples were inspected. The data revealed that the total Sb in the tea infusions ranged from 0.22 to 0.97 μg L−1, and we found that 50–83% of the total Sb in the tea infusion was iSb. This method is worth promoting since it has satisfying methodological performance. Graphical abstract
{"title":"Speciation and determination of inorganic antimony in tea infusion by using solid-phase extraction-based liquid chromatography-inductively coupled plasma-mass spectrometry","authors":"Jiacai Hu, Xiuming Lv, Hao Zhang, B. Zhu, De-ye Liu, W. Ji","doi":"10.1080/10826076.2023.2238824","DOIUrl":"https://doi.org/10.1080/10826076.2023.2238824","url":null,"abstract":"Abstract In this work, we developed a method to separate and detect inorganic antimony (iSb) in tea infusions based on liquid chromatography-inductively coupled plasma-mass spectrometry (LC-ICP-MS). Considering that iSb was present in tea infusions in trace amounts, a commercial solid-phase extraction (SPE) column was employed to enrich iSb(III) and iSb(V). In this study, we found that iSb exists in tea infusions in a bound state with an unknown substance rather than in a free state. Therefore, the enrichment step was combined with oxidation and reduction processes. Because of the enrichment process and the high sensitivity of LC-ICP-MS, the LODs of iSb(III) and iSb(V) were both as low as 0.03 μg L−1. The RSDs (n = 6) of iSb(III) and iSb(V) were all below 8.1%, and the recoveries (n = 6) were 92–96% and 90–94%, respectively. Then, a total of six tea infusion samples were inspected. The data revealed that the total Sb in the tea infusions ranged from 0.22 to 0.97 μg L−1, and we found that 50–83% of the total Sb in the tea infusion was iSb. This method is worth promoting since it has satisfying methodological performance. Graphical abstract","PeriodicalId":16295,"journal":{"name":"Journal of Liquid Chromatography & Related Technologies","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2023-07-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46312652","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-07-03DOI: 10.1080/10826076.2023.2240913
Jake A Cravino, Corey W. Manwaring, Jonathan G. H. Stathakis, R. Shalliker
Abstract Blueberries are widely consumed for their flavor and complex array of antioxidants and other beneficial phytochemicals. Central to studies on blueberries is the ability to extract antioxidants. For appropriate analysis, the extracted compounds must represent those contained in the blueberry without bias or loss of information. Given the complex array of phytochemicals present, extracting these chemicals from blueberries is a complex task and is the focus of much debate in the current literature. While many studies have examined the best extraction technique to maximize the concentration of extracted antioxidants, there remains no systematic study on the effect of extraction conditions and technique on the variety of antioxidants extracted from the blueberry samples. The current study fills this gap by applying High-Performance Liquid Chromatography combined with novel forms of post-column derivatization and the commonly used CUPRAC assay to examine the range and concentration of antioxidants extracted. We have found that solvent choice plays a large role in determining the variety of compounds extracted, with acidification, extraction time, and temperature having minimal effect, and acetone has been shown to provide extraction of the greatest range and highest concentration of compounds. Graphical Abstract
{"title":"Extracting antioxidants from blueberries","authors":"Jake A Cravino, Corey W. Manwaring, Jonathan G. H. Stathakis, R. Shalliker","doi":"10.1080/10826076.2023.2240913","DOIUrl":"https://doi.org/10.1080/10826076.2023.2240913","url":null,"abstract":"Abstract Blueberries are widely consumed for their flavor and complex array of antioxidants and other beneficial phytochemicals. Central to studies on blueberries is the ability to extract antioxidants. For appropriate analysis, the extracted compounds must represent those contained in the blueberry without bias or loss of information. Given the complex array of phytochemicals present, extracting these chemicals from blueberries is a complex task and is the focus of much debate in the current literature. While many studies have examined the best extraction technique to maximize the concentration of extracted antioxidants, there remains no systematic study on the effect of extraction conditions and technique on the variety of antioxidants extracted from the blueberry samples. The current study fills this gap by applying High-Performance Liquid Chromatography combined with novel forms of post-column derivatization and the commonly used CUPRAC assay to examine the range and concentration of antioxidants extracted. We have found that solvent choice plays a large role in determining the variety of compounds extracted, with acidification, extraction time, and temperature having minimal effect, and acetone has been shown to provide extraction of the greatest range and highest concentration of compounds. Graphical Abstract","PeriodicalId":16295,"journal":{"name":"Journal of Liquid Chromatography & Related Technologies","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2023-07-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49651760","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-06-29DOI: 10.1080/10826076.2023.2227792
Vanessa Morais Muniz, J. V. Chaves Júnior, C. Aragão, F. S. Souza, F. C. Sampaio
Abstract The antimicrobial chlorhexidine is considered the gold standard in dentistry. Thymol is a phenol found in the essential oils of various plant species and also stands out for its antimicrobial potential. Synergistic effects can be promoted by applying these two active pharmaceutical ingredients together in technological products, for example in controlled release microparticles. The objective of this work was to develop and validate an analytical methodology applying a Box-Behnken experimental design and using High Performance Liquid Chromatography capable of quantifying chlorhexidine and thymol simultaneously in a matrix including pharmaceutical excipients. After optimization, the mobile phase consisted of methanol and 0.03 M monobasic sodium phosphate buffer (60:40), with 0.4% triethylamine and octylsilane as the applied stationary phase. The method proved selective, even in the presence of chlorhexidine and thymol degradation products. For chlorhexidine, the method was linear from 4.8 to 19.2 µg/mL, and for thymol from 8.0 to 32.0 µg/mL. Accuracy was close to 100%, and the precision assessment yielded coefficient variation values of <5%. Being based on the Box-Behnken design, the method was robust and therefore validated for assisting in quality control processes involving these active pharmaceutical ingredients. Graphical Abstract
{"title":"A HPLC method for simultaneous quantification of chlorhexidine and thymol using Box-Behnken design for robustness of the method assessment","authors":"Vanessa Morais Muniz, J. V. Chaves Júnior, C. Aragão, F. S. Souza, F. C. Sampaio","doi":"10.1080/10826076.2023.2227792","DOIUrl":"https://doi.org/10.1080/10826076.2023.2227792","url":null,"abstract":"Abstract The antimicrobial chlorhexidine is considered the gold standard in dentistry. Thymol is a phenol found in the essential oils of various plant species and also stands out for its antimicrobial potential. Synergistic effects can be promoted by applying these two active pharmaceutical ingredients together in technological products, for example in controlled release microparticles. The objective of this work was to develop and validate an analytical methodology applying a Box-Behnken experimental design and using High Performance Liquid Chromatography capable of quantifying chlorhexidine and thymol simultaneously in a matrix including pharmaceutical excipients. After optimization, the mobile phase consisted of methanol and 0.03 M monobasic sodium phosphate buffer (60:40), with 0.4% triethylamine and octylsilane as the applied stationary phase. The method proved selective, even in the presence of chlorhexidine and thymol degradation products. For chlorhexidine, the method was linear from 4.8 to 19.2 µg/mL, and for thymol from 8.0 to 32.0 µg/mL. Accuracy was close to 100%, and the precision assessment yielded coefficient variation values of <5%. Being based on the Box-Behnken design, the method was robust and therefore validated for assisting in quality control processes involving these active pharmaceutical ingredients. Graphical Abstract","PeriodicalId":16295,"journal":{"name":"Journal of Liquid Chromatography & Related Technologies","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2023-06-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49339923","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-06-28DOI: 10.1080/10826076.2023.2227884
Negin Yazdanian, B. Akbari‐adergani, M. Kazemipour, M. Javanbakht, H. Ahmad panahi
Abstract In this work, the synthesis of thin-layer, pH-sensitive molecularly imprinted membrane using methacrylic acid and maleic acid as functional monomers, ethylene glycol dimethacrylate as cross-linker, 2,2′-azobisisobutyronitrile as initiator, poly (vinylidene fluoride) as porous membrane, and celecoxib as a target molecule have been reported. Different technique analyses characterized the membrane product. A novel molecularly imprinted membrane-solid phase extraction method was used for the extraction of celecoxib and concentrating it prior to be analyzed in the human plasma and urine matrix. High-performance liquid chromatography with ultraviolet detection was used and validated for the analysis of celecoxib which was extracted from biological fluids. The molecularly imprinted membrane showed selective performance for the template, and extraction recoveries of the drug by the membrane from human plasma and urine samples were between 96.2 and 97.3%. The obtained results showed that the detection and quantification limits of the drug were 0.12 and 0.40 ng mL−1, respectively. The adsorption capacity of 4.95 mg g−1 was obtained from the fitting by the Langmuir model. The molecularly imprinted membrane can be easily regenerated eight times with sustained efficiency. Therefore, the developed method can be a good candidate for the separation and detection of celecoxib in biological samples. GRAPHICAL ABSTRACT
摘要本文报道了以甲基丙烯酸和马来酸为功能单体，乙二醇二甲基丙烯酸酯为交联剂，2，2′-偶氮二异丁腈为引发剂，聚偏二氟乙烯为多孔膜，塞来昔布为靶分子，合成了对pH敏感的薄层分子印迹膜。不同的技术分析对膜产品进行了表征。采用一种新的分子印迹膜固相萃取方法提取塞来昔布，并在人体血浆和尿液基质中进行分析前进行浓缩。采用紫外检测的高效液相色谱法对从生物液中提取的塞来昔布进行了分析和验证。分子印迹膜对模板具有选择性，从人血浆和尿液中提取药物的回收率在96.2%至97.3%之间。结果表明，该药物的检测和定量限分别为0.12和0.40 ng mL−1。吸附容量4.95 通过Langmuir模型拟合得到mg g−1。分子印迹膜可以容易地再生八次并具有持续的效率。因此，所开发的方法可以很好地用于生物样品中塞来昔布的分离和检测。图形摘要
{"title":"Synthesis and characterization of pH-sensitive thin-layer molecularly imprinted membranes for selective solid-phase extraction of celecoxib from biological fluids followed by high-performance liquid chromatography with UV detection","authors":"Negin Yazdanian, B. Akbari‐adergani, M. Kazemipour, M. Javanbakht, H. Ahmad panahi","doi":"10.1080/10826076.2023.2227884","DOIUrl":"https://doi.org/10.1080/10826076.2023.2227884","url":null,"abstract":"Abstract In this work, the synthesis of thin-layer, pH-sensitive molecularly imprinted membrane using methacrylic acid and maleic acid as functional monomers, ethylene glycol dimethacrylate as cross-linker, 2,2′-azobisisobutyronitrile as initiator, poly (vinylidene fluoride) as porous membrane, and celecoxib as a target molecule have been reported. Different technique analyses characterized the membrane product. A novel molecularly imprinted membrane-solid phase extraction method was used for the extraction of celecoxib and concentrating it prior to be analyzed in the human plasma and urine matrix. High-performance liquid chromatography with ultraviolet detection was used and validated for the analysis of celecoxib which was extracted from biological fluids. The molecularly imprinted membrane showed selective performance for the template, and extraction recoveries of the drug by the membrane from human plasma and urine samples were between 96.2 and 97.3%. The obtained results showed that the detection and quantification limits of the drug were 0.12 and 0.40 ng mL−1, respectively. The adsorption capacity of 4.95 mg g−1 was obtained from the fitting by the Langmuir model. The molecularly imprinted membrane can be easily regenerated eight times with sustained efficiency. Therefore, the developed method can be a good candidate for the separation and detection of celecoxib in biological samples. GRAPHICAL ABSTRACT","PeriodicalId":16295,"journal":{"name":"Journal of Liquid Chromatography & Related Technologies","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2023-06-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46197983","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-06-28DOI: 10.1080/10826076.2023.2227887
Nada Seddiq, A. Asan
Abstract A simple and effective one-step pre-column derivatization method for reversed-phase HPLC-UV determination of the major organic acids (citric, malic, tartaric, and succinic acids) in fruit juices has been developed. The method is based on the coupling reaction of organic acids with 1-naphthylamine in the presence of N,N′-diisopropylcarbodiimide. The resulting organic acid amide derivatives were successfully separated on an AQ-C18 column and detected by a UV detector at 222 nm. Isocratic elution was performed using an acetonitrile-methanol-tetrahydrofuran-water (37:4:1:58; v/v) mixture as a mobile phase at a flow rate of 2.0 mL/min. Validation studies showed good recoveries ranging from 88.97 to 92.52% with RSD % between 2.95 and 4.56%. The detection limits obtained were 0.18, 0.48, 0.14, and 0.69 µg/mL for tartaric acid, malic acid, succinic acid, and citric acid, respectively. The method was successfully applied to three different commercial fruit juice and nectar samples with little or no clean-up procedures. Graphical Abstract
{"title":"One-step pre-column derivatization method for HPLC-UV determination of organic acids in fruit juices","authors":"Nada Seddiq, A. Asan","doi":"10.1080/10826076.2023.2227887","DOIUrl":"https://doi.org/10.1080/10826076.2023.2227887","url":null,"abstract":"Abstract A simple and effective one-step pre-column derivatization method for reversed-phase HPLC-UV determination of the major organic acids (citric, malic, tartaric, and succinic acids) in fruit juices has been developed. The method is based on the coupling reaction of organic acids with 1-naphthylamine in the presence of N,N′-diisopropylcarbodiimide. The resulting organic acid amide derivatives were successfully separated on an AQ-C18 column and detected by a UV detector at 222 nm. Isocratic elution was performed using an acetonitrile-methanol-tetrahydrofuran-water (37:4:1:58; v/v) mixture as a mobile phase at a flow rate of 2.0 mL/min. Validation studies showed good recoveries ranging from 88.97 to 92.52% with RSD % between 2.95 and 4.56%. The detection limits obtained were 0.18, 0.48, 0.14, and 0.69 µg/mL for tartaric acid, malic acid, succinic acid, and citric acid, respectively. The method was successfully applied to three different commercial fruit juice and nectar samples with little or no clean-up procedures. Graphical Abstract","PeriodicalId":16295,"journal":{"name":"Journal of Liquid Chromatography & Related Technologies","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2023-06-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"85345671","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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