S. Katna, Arvind Kumar, T. Banshtu, N. Devi, Shubhra Singh, Hema Prasad
The study was carried out to determine the dissipation kinetics, persistence, and dietary risk assessment of tetraniliprole. Three applications of tetraniliprole were given at 50.00 g a.i./hac (X) and 62.50 g a.i/hac (1.25X) on chilli and brinjal at the fruiting stage. The recoveries in all the matrices were within the acceptable range of 70%–120%. The initial residues of tetraniliprole on chilli fruits were 0.379 and 0.593 μg/g and on brinjal fruits, the residues were 0.559 and 0.916 μg/g at 50.00 and 62.50 g a.i./ha, respectively. In red chilli, chilli field soil, and brinjal field soil the residues were below the limit of quantitation. The tetraniliprole follows first‐order dissipation kinetics with the half‐life (RL50) 1.58 and 1.99 days in chilli and 1.42 and 1.79 days in brinjal at X and 1.25X doses. In chilli, 9.89 and 12.11 days whereas, in brinjal, 10.75 and 13.25 days were recommended for harvesting the crops after the last application of tetraniliprole at X and 1.25 X doses, respectively. The hazard quotient values in chilli and brinjal for both males and females were below 1 indicating that the use of tetraniliprole does not cause any health risk to the consumers.
{"title":"Dissipation kinetics, persistence, and dietary risk assessment of tetraniliprole in two solanaceous vegetables, chilli and brinjal","authors":"S. Katna, Arvind Kumar, T. Banshtu, N. Devi, Shubhra Singh, Hema Prasad","doi":"10.1002/sscp.202300121","DOIUrl":"https://doi.org/10.1002/sscp.202300121","url":null,"abstract":"The study was carried out to determine the dissipation kinetics, persistence, and dietary risk assessment of tetraniliprole. Three applications of tetraniliprole were given at 50.00 g a.i./hac (X) and 62.50 g a.i/hac (1.25X) on chilli and brinjal at the fruiting stage. The recoveries in all the matrices were within the acceptable range of 70%–120%. The initial residues of tetraniliprole on chilli fruits were 0.379 and 0.593 μg/g and on brinjal fruits, the residues were 0.559 and 0.916 μg/g at 50.00 and 62.50 g a.i./ha, respectively. In red chilli, chilli field soil, and brinjal field soil the residues were below the limit of quantitation. The tetraniliprole follows first‐order dissipation kinetics with the half‐life (RL50) 1.58 and 1.99 days in chilli and 1.42 and 1.79 days in brinjal at X and 1.25X doses. In chilli, 9.89 and 12.11 days whereas, in brinjal, 10.75 and 13.25 days were recommended for harvesting the crops after the last application of tetraniliprole at X and 1.25 X doses, respectively. The hazard quotient values in chilli and brinjal for both males and females were below 1 indicating that the use of tetraniliprole does not cause any health risk to the consumers.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":1.1,"publicationDate":"2024-02-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139810305","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}
Sergio Bessa‐Jambrina, Anna Marlés‐Torres, Cristóbal Galán-Rodríguez
A reversed‐phase ultra‐high‐performance liquid chromatography‐tandem mass spectrometry method is presented for the quantification of the mutagenic impurity 7‐nitroso‐3‐(trifluoromethyl)‐5,6,7,8‐tetrahydro‐[1,2,4]triazolo[4,3‐a]pyrazine found in three sitagliptin drug substances (sitagliptin base [SG], sitagliptin hydrochloride monohydrate [SG HCl{H}] salt, and sitagliptin phosphate monohydrate [SG P{H}] salt). A simple and highly sensitive method was developed for SG, SG HCl(H) salt, and SG P(H) salt. Sample preparation was adapted to each product considering solubility, sensitivity, and accuracy issues. Chromatographic separation was achieved using an Acquity HSS T3 column (3.0 × 100 mm, 1.8 μm) and a mobile phase consisting of formic acid 0.1% in water combined with methanol. Detection and quantification of the impurity were carried out using triple quadrupole mass spectrometry detection with electrospray ionization in the multiple reaction monitoring mode. The limit of detection and limit of quantification was found to be 0.1–0.3 and 10 ppb, respectively. The accuracy and precision of the method were satisfactorily determined with recovery values between 74.1% and 119.4%. Linearity is demonstrated in the range of 10 and 2000 ppb with regression coefficients (R) within the range of 0.9918–0.9972. The method is currently used for the analysis of the mutagenic impurity in the three‐drug substances in the Moehs Group.
{"title":"Ultra‐high‐performance liquid chromatography‐tandem mass spectrometry analytical method for the determination of nitrosamine drug substance‐related impurity in sitagliptin base and salts","authors":"Sergio Bessa‐Jambrina, Anna Marlés‐Torres, Cristóbal Galán-Rodríguez","doi":"10.1002/sscp.202400003","DOIUrl":"https://doi.org/10.1002/sscp.202400003","url":null,"abstract":"A reversed‐phase ultra‐high‐performance liquid chromatography‐tandem mass spectrometry method is presented for the quantification of the mutagenic impurity 7‐nitroso‐3‐(trifluoromethyl)‐5,6,7,8‐tetrahydro‐[1,2,4]triazolo[4,3‐a]pyrazine found in three sitagliptin drug substances (sitagliptin base [SG], sitagliptin hydrochloride monohydrate [SG HCl{H}] salt, and sitagliptin phosphate monohydrate [SG P{H}] salt). A simple and highly sensitive method was developed for SG, SG HCl(H) salt, and SG P(H) salt. Sample preparation was adapted to each product considering solubility, sensitivity, and accuracy issues. Chromatographic separation was achieved using an Acquity HSS T3 column (3.0 × 100 mm, 1.8 μm) and a mobile phase consisting of formic acid 0.1% in water combined with methanol. Detection and quantification of the impurity were carried out using triple quadrupole mass spectrometry detection with electrospray ionization in the multiple reaction monitoring mode. The limit of detection and limit of quantification was found to be 0.1–0.3 and 10 ppb, respectively. The accuracy and precision of the method were satisfactorily determined with recovery values between 74.1% and 119.4%. Linearity is demonstrated in the range of 10 and 2000 ppb with regression coefficients (R) within the range of 0.9918–0.9972. The method is currently used for the analysis of the mutagenic impurity in the three‐drug substances in the Moehs Group.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":1.1,"publicationDate":"2024-02-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139810803","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}
Sergio Bessa‐Jambrina, Anna Marlés‐Torres, Cristóbal Galán-Rodríguez
A reversed‐phase ultra‐high‐performance liquid chromatography‐tandem mass spectrometry method is presented for the quantification of the mutagenic impurity 7‐nitroso‐3‐(trifluoromethyl)‐5,6,7,8‐tetrahydro‐[1,2,4]triazolo[4,3‐a]pyrazine found in three sitagliptin drug substances (sitagliptin base [SG], sitagliptin hydrochloride monohydrate [SG HCl{H}] salt, and sitagliptin phosphate monohydrate [SG P{H}] salt). A simple and highly sensitive method was developed for SG, SG HCl(H) salt, and SG P(H) salt. Sample preparation was adapted to each product considering solubility, sensitivity, and accuracy issues. Chromatographic separation was achieved using an Acquity HSS T3 column (3.0 × 100 mm, 1.8 μm) and a mobile phase consisting of formic acid 0.1% in water combined with methanol. Detection and quantification of the impurity were carried out using triple quadrupole mass spectrometry detection with electrospray ionization in the multiple reaction monitoring mode. The limit of detection and limit of quantification was found to be 0.1–0.3 and 10 ppb, respectively. The accuracy and precision of the method were satisfactorily determined with recovery values between 74.1% and 119.4%. Linearity is demonstrated in the range of 10 and 2000 ppb with regression coefficients (R) within the range of 0.9918–0.9972. The method is currently used for the analysis of the mutagenic impurity in the three‐drug substances in the Moehs Group.
{"title":"Ultra‐high‐performance liquid chromatography‐tandem mass spectrometry analytical method for the determination of nitrosamine drug substance‐related impurity in sitagliptin base and salts","authors":"Sergio Bessa‐Jambrina, Anna Marlés‐Torres, Cristóbal Galán-Rodríguez","doi":"10.1002/sscp.202400003","DOIUrl":"https://doi.org/10.1002/sscp.202400003","url":null,"abstract":"A reversed‐phase ultra‐high‐performance liquid chromatography‐tandem mass spectrometry method is presented for the quantification of the mutagenic impurity 7‐nitroso‐3‐(trifluoromethyl)‐5,6,7,8‐tetrahydro‐[1,2,4]triazolo[4,3‐a]pyrazine found in three sitagliptin drug substances (sitagliptin base [SG], sitagliptin hydrochloride monohydrate [SG HCl{H}] salt, and sitagliptin phosphate monohydrate [SG P{H}] salt). A simple and highly sensitive method was developed for SG, SG HCl(H) salt, and SG P(H) salt. Sample preparation was adapted to each product considering solubility, sensitivity, and accuracy issues. Chromatographic separation was achieved using an Acquity HSS T3 column (3.0 × 100 mm, 1.8 μm) and a mobile phase consisting of formic acid 0.1% in water combined with methanol. Detection and quantification of the impurity were carried out using triple quadrupole mass spectrometry detection with electrospray ionization in the multiple reaction monitoring mode. The limit of detection and limit of quantification was found to be 0.1–0.3 and 10 ppb, respectively. The accuracy and precision of the method were satisfactorily determined with recovery values between 74.1% and 119.4%. Linearity is demonstrated in the range of 10 and 2000 ppb with regression coefficients (R) within the range of 0.9918–0.9972. The method is currently used for the analysis of the mutagenic impurity in the three‐drug substances in the Moehs Group.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":1.1,"publicationDate":"2024-02-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139870683","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}
Molnupiravir, a promising antiviral agent, has gained significant attention for its potential in treating viral infections, particularly in the context of the coronavirus disease 2019 pandemic. This study aimed to develop and validate an ultra‐high‐performance liquid chromatography (UHPLC) method for the quantification of Molnupiravir and its associated impurities (Imp‐I, Imp‐II, Imp‐III, and Imp‐IV). The method involved a systematic investigation of critical method parameters and their optimization using Quality by Design principles. The percentage of organic modifiers, column temperature, and flow rate were systematically optimized using the Box‐Behnken design. The developed method was assessed for specificity, system suitability, accuracy, precision, linearity, and detection limits. The results demonstrate strong specificity, with the analysis remaining accurate even in the presence of impurities. The developed method exhibits excellent precision, with repeatability and intermediate precision showing relative standard deviation values ranging from 0.78% to 1.14% for impurities and 0.82% to 1.91% for Molnupiravir. Furthermore, the method displays exceptional linearity, covering a wide range of concentrations. The linear regression analysis yields high coefficients of determination (r2, 9993–0.9997), confirming the linearity. The developed UHPLC method is well‐suited for the accurate and reliable analysis of Molnupiravir and its impurities, making it a valuable tool for quality control and pharmaceutical research applications.
{"title":"Ultra‐high‐performance liquid chromatography method development for the quantification of Molnupiravir and its process‐related impurities using Box‐Behnken experimental design","authors":"Mohana Vamsi Nuli, Darna Bhikshapathi, Anil Kumar Garige, Vijitha Chandupatla, Surya Lakshmi Sunkara, P. Grover","doi":"10.1002/sscp.202300213","DOIUrl":"https://doi.org/10.1002/sscp.202300213","url":null,"abstract":"Molnupiravir, a promising antiviral agent, has gained significant attention for its potential in treating viral infections, particularly in the context of the coronavirus disease 2019 pandemic. This study aimed to develop and validate an ultra‐high‐performance liquid chromatography (UHPLC) method for the quantification of Molnupiravir and its associated impurities (Imp‐I, Imp‐II, Imp‐III, and Imp‐IV). The method involved a systematic investigation of critical method parameters and their optimization using Quality by Design principles. The percentage of organic modifiers, column temperature, and flow rate were systematically optimized using the Box‐Behnken design. The developed method was assessed for specificity, system suitability, accuracy, precision, linearity, and detection limits. The results demonstrate strong specificity, with the analysis remaining accurate even in the presence of impurities. The developed method exhibits excellent precision, with repeatability and intermediate precision showing relative standard deviation values ranging from 0.78% to 1.14% for impurities and 0.82% to 1.91% for Molnupiravir. Furthermore, the method displays exceptional linearity, covering a wide range of concentrations. The linear regression analysis yields high coefficients of determination (r2, 9993–0.9997), confirming the linearity. The developed UHPLC method is well‐suited for the accurate and reliable analysis of Molnupiravir and its impurities, making it a valuable tool for quality control and pharmaceutical research applications.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":1.1,"publicationDate":"2024-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139813930","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}
Molnupiravir, a promising antiviral agent, has gained significant attention for its potential in treating viral infections, particularly in the context of the coronavirus disease 2019 pandemic. This study aimed to develop and validate an ultra‐high‐performance liquid chromatography (UHPLC) method for the quantification of Molnupiravir and its associated impurities (Imp‐I, Imp‐II, Imp‐III, and Imp‐IV). The method involved a systematic investigation of critical method parameters and their optimization using Quality by Design principles. The percentage of organic modifiers, column temperature, and flow rate were systematically optimized using the Box‐Behnken design. The developed method was assessed for specificity, system suitability, accuracy, precision, linearity, and detection limits. The results demonstrate strong specificity, with the analysis remaining accurate even in the presence of impurities. The developed method exhibits excellent precision, with repeatability and intermediate precision showing relative standard deviation values ranging from 0.78% to 1.14% for impurities and 0.82% to 1.91% for Molnupiravir. Furthermore, the method displays exceptional linearity, covering a wide range of concentrations. The linear regression analysis yields high coefficients of determination (r2, 9993–0.9997), confirming the linearity. The developed UHPLC method is well‐suited for the accurate and reliable analysis of Molnupiravir and its impurities, making it a valuable tool for quality control and pharmaceutical research applications.
{"title":"Ultra‐high‐performance liquid chromatography method development for the quantification of Molnupiravir and its process‐related impurities using Box‐Behnken experimental design","authors":"Mohana Vamsi Nuli, Darna Bhikshapathi, Anil Kumar Garige, Vijitha Chandupatla, Surya Lakshmi Sunkara, P. Grover","doi":"10.1002/sscp.202300213","DOIUrl":"https://doi.org/10.1002/sscp.202300213","url":null,"abstract":"Molnupiravir, a promising antiviral agent, has gained significant attention for its potential in treating viral infections, particularly in the context of the coronavirus disease 2019 pandemic. This study aimed to develop and validate an ultra‐high‐performance liquid chromatography (UHPLC) method for the quantification of Molnupiravir and its associated impurities (Imp‐I, Imp‐II, Imp‐III, and Imp‐IV). The method involved a systematic investigation of critical method parameters and their optimization using Quality by Design principles. The percentage of organic modifiers, column temperature, and flow rate were systematically optimized using the Box‐Behnken design. The developed method was assessed for specificity, system suitability, accuracy, precision, linearity, and detection limits. The results demonstrate strong specificity, with the analysis remaining accurate even in the presence of impurities. The developed method exhibits excellent precision, with repeatability and intermediate precision showing relative standard deviation values ranging from 0.78% to 1.14% for impurities and 0.82% to 1.91% for Molnupiravir. Furthermore, the method displays exceptional linearity, covering a wide range of concentrations. The linear regression analysis yields high coefficients of determination (r2, 9993–0.9997), confirming the linearity. The developed UHPLC method is well‐suited for the accurate and reliable analysis of Molnupiravir and its impurities, making it a valuable tool for quality control and pharmaceutical research applications.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":1.1,"publicationDate":"2024-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139873532","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}
The primary goals of green analytical chemistry (GAC) involve the development of novel analytical technologies or the modification of existing methods to incorporate procedures with reduced reliance on hazardous chemicals. Several approaches can be employed to achieve these objectives, including the utilization of environmentally friendly solvents and reagents, shortening chromatographic separation times, and the miniaturization of analytical devices. The review summarizes the evolution of GAC with its specific principles and with special emphasis on recent applications in modern era. A detailed exploration of the choice of green solvents and their practical utilization in green liquid chromatography (LC) techniques for environmentally friendly analysis of pharmaceuticals has been discussed. An ordinary description with a tabular illustration of various modern green analytical techniques like micellar LC, superheated water chromatography, high‐speed LC, enhanced fluidity LC, two‐dimensional LC, and aspects of gas chromatography has been thoroughly provided for concepts with their mechanism and limitations. GAC provides potential applications for food analysis, environmental analysis of pharmaceutically active compounds in the aquatic environment with special emphasis on strategies for greening LC and impurity profiling, and so on. Numerous benefits, limitations, and challenges that are linked to the field of GAC are highlighted in this review. We pay special attention to new green approaches, such as automation, miniaturization, direct analysis techniques, and some initiatives like the National Environmental Methods Index Label for Analytical Eco‐Scale assessment. In spite of many promising advancements, the understanding is still limited and challenging.
{"title":"A comprehensive exploration of diverse green analytical techniques and their influence in different analytical fields","authors":"Bibhu Prasad Nanda, Arshdeep Chopra, Yogindra Kumari, R. Narang, Rohit Bhatia","doi":"10.1002/sscp.202400004","DOIUrl":"https://doi.org/10.1002/sscp.202400004","url":null,"abstract":"The primary goals of green analytical chemistry (GAC) involve the development of novel analytical technologies or the modification of existing methods to incorporate procedures with reduced reliance on hazardous chemicals. Several approaches can be employed to achieve these objectives, including the utilization of environmentally friendly solvents and reagents, shortening chromatographic separation times, and the miniaturization of analytical devices. The review summarizes the evolution of GAC with its specific principles and with special emphasis on recent applications in modern era. A detailed exploration of the choice of green solvents and their practical utilization in green liquid chromatography (LC) techniques for environmentally friendly analysis of pharmaceuticals has been discussed. An ordinary description with a tabular illustration of various modern green analytical techniques like micellar LC, superheated water chromatography, high‐speed LC, enhanced fluidity LC, two‐dimensional LC, and aspects of gas chromatography has been thoroughly provided for concepts with their mechanism and limitations. GAC provides potential applications for food analysis, environmental analysis of pharmaceutically active compounds in the aquatic environment with special emphasis on strategies for greening LC and impurity profiling, and so on. Numerous benefits, limitations, and challenges that are linked to the field of GAC are highlighted in this review. We pay special attention to new green approaches, such as automation, miniaturization, direct analysis techniques, and some initiatives like the National Environmental Methods Index Label for Analytical Eco‐Scale assessment. In spite of many promising advancements, the understanding is still limited and challenging.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":1.1,"publicationDate":"2024-01-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139532248","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}
A method was established for the simultaneous determination of furosine, furanone, and four furfural compounds (5‐hydroxymethylfurfural, furfural, furyl methyl ketone, and methyl furfural) in complementary rice, flour, and noodles for infants and young children by high performance liquid chromatography with a diode array detector. The sample was extracted using oxalic acid aqueous solution as a solvent, and the protein was removed using trichloroacetic acid. Then the six Maillard reaction products were separated by an Eclipse XDB‐C18 column with a gradient elution at a flow rate of 0.6 mL/min using acetonitrile‐0.1% trifluoroacetic acid solution as the mobile phase, detected by a diode array detector and quantified by external standard method. The linear ranges of the six Maillard reaction products were 250–20000 μg/100 g with the correlation coefficients greater than 0.999, and the limits of quantification ranged from 250 to 1000 μg/100 g (S/N ≥ 10). The recoveries of the six Maillard reaction products ranged from 71.2% to 100% with a relative standard deviation of 0.9%–4.9%. The real sample analysis results showed that 5‐hydroxymethylfurfural was detected in two cookie samples, the contents of which were 335 μg/100 g and 436 μg/100 g, respectively. There are no studies on the detection of the six Maillard reaction products in rice, flour, and noodles in the previous reports. The established method provided reference for the quantification of expiration date in complementary rice, flour, and noodles for infants and young children.
{"title":"Determination of the Maillard reaction products in complementary rice, flour, and noodles by high performance liquid chromatography with a diode array detector","authors":"Jian‐bo Hou, Wen-Hua Zhang, Ya-Qin Zhang, Ren‐yi Mao, Ze‐long Zhu, Xiaoli Hu, Xin Xu, Hui Qiu, Ying Liang","doi":"10.1002/sscp.202300204","DOIUrl":"https://doi.org/10.1002/sscp.202300204","url":null,"abstract":"A method was established for the simultaneous determination of furosine, furanone, and four furfural compounds (5‐hydroxymethylfurfural, furfural, furyl methyl ketone, and methyl furfural) in complementary rice, flour, and noodles for infants and young children by high performance liquid chromatography with a diode array detector. The sample was extracted using oxalic acid aqueous solution as a solvent, and the protein was removed using trichloroacetic acid. Then the six Maillard reaction products were separated by an Eclipse XDB‐C18 column with a gradient elution at a flow rate of 0.6 mL/min using acetonitrile‐0.1% trifluoroacetic acid solution as the mobile phase, detected by a diode array detector and quantified by external standard method. The linear ranges of the six Maillard reaction products were 250–20000 μg/100 g with the correlation coefficients greater than 0.999, and the limits of quantification ranged from 250 to 1000 μg/100 g (S/N ≥ 10). The recoveries of the six Maillard reaction products ranged from 71.2% to 100% with a relative standard deviation of 0.9%–4.9%. The real sample analysis results showed that 5‐hydroxymethylfurfural was detected in two cookie samples, the contents of which were 335 μg/100 g and 436 μg/100 g, respectively. There are no studies on the detection of the six Maillard reaction products in rice, flour, and noodles in the previous reports. The established method provided reference for the quantification of expiration date in complementary rice, flour, and noodles for infants and young children.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":1.1,"publicationDate":"2024-01-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139532193","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}
Mohsen Nikdel, Alireza Nezami, Y. Yamini, Behnam Ghorbani Nezhad, A. Nazaripour, Matin Baghani, Milad Rahimzadegan
In the present manuscript, an automated three‐phase hollow fiber liquid‐phase microextraction followed by high‐performance liquid chromatography‐diode array detection is applied for the extraction and determination of three pyrethroids, deltamethrin, fenpropathrin, and permethrin in water and fruit samples. N‐dodecane was selected as a supported liquid membrane (SLM) and its polarity was adjusted by trioctylphosphine oxide one‐variable‐at‐a‐time method was used in order to achieve optimal hollow fiber liquid‐phase microextraction parameters such as type of organic acceptor phase, the composition of SLM, ionic strength of sample solution, extraction time, length of hollow fibers and stirring speed. Under the optimal conditions, the calibration curves for the three pyrethroids were plotted, and figures of merit of the proposed method were calculated. The linear dynamic ranges were in the range of 0.9–200, 0.75–200, and 1.5–200 μg/L for deltamethrin, fenpropathrin, and permethrin, with the coefficient of determination better than 0.998. The limits of detection were in the range of 0.3, 0.25, and 0.5 and the limits of quantification were in the range of 0.9, 0.75, and 1.5 μg/L for deltamethrin, fenpropathrin, and permethrin, respectively. The precision of the method was evaluated in terms of relative standard deviation at two different concentration levels 10 and 50 μg/L. The results of real sample analysis in cucumber exhibited high sensitivity, excellent sample clean‐up, favorable repeatability, and suitable accuracy.
{"title":"Optimized three‐phase hollow fiber liquid‐phase automated microextraction and its application in ultra‐trace analysis of three pyrethroids in water and fruit samples using high‐performance liquid chromatography‐diode array detection","authors":"Mohsen Nikdel, Alireza Nezami, Y. Yamini, Behnam Ghorbani Nezhad, A. Nazaripour, Matin Baghani, Milad Rahimzadegan","doi":"10.1002/sscp.202300143","DOIUrl":"https://doi.org/10.1002/sscp.202300143","url":null,"abstract":"In the present manuscript, an automated three‐phase hollow fiber liquid‐phase microextraction followed by high‐performance liquid chromatography‐diode array detection is applied for the extraction and determination of three pyrethroids, deltamethrin, fenpropathrin, and permethrin in water and fruit samples. N‐dodecane was selected as a supported liquid membrane (SLM) and its polarity was adjusted by trioctylphosphine oxide one‐variable‐at‐a‐time method was used in order to achieve optimal hollow fiber liquid‐phase microextraction parameters such as type of organic acceptor phase, the composition of SLM, ionic strength of sample solution, extraction time, length of hollow fibers and stirring speed. Under the optimal conditions, the calibration curves for the three pyrethroids were plotted, and figures of merit of the proposed method were calculated. The linear dynamic ranges were in the range of 0.9–200, 0.75–200, and 1.5–200 μg/L for deltamethrin, fenpropathrin, and permethrin, with the coefficient of determination better than 0.998. The limits of detection were in the range of 0.3, 0.25, and 0.5 and the limits of quantification were in the range of 0.9, 0.75, and 1.5 μg/L for deltamethrin, fenpropathrin, and permethrin, respectively. The precision of the method was evaluated in terms of relative standard deviation at two different concentration levels 10 and 50 μg/L. The results of real sample analysis in cucumber exhibited high sensitivity, excellent sample clean‐up, favorable repeatability, and suitable accuracy.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":1.1,"publicationDate":"2024-01-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139534784","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}
Shaileshkumar K. Koradia, Madhavi Patel, A. Sen, D. Sen, Prasanna Pradhan
The current study aims to develop and validate an analytical quality by design approach‐based high‐performance thin‐layer chromatographic (HPTLC) method for the analysis of Axitinib tablet samples. The chromatographic conditions in the TLC method were optimized using a three‐level full factorial design. The mobile phase composition and chamber saturation time served as the independent variables for optimization. The mobile phase used for TLC separation on pre‐coated aluminum plates with silica gel 60 F254 consisted of a mixture of ethyl acetate and isopropyl alcohol in a ratio of 9:1 (v/v). Axitinib was quantified at 330 nm using the densitometric method. Axitinib peak from tablet formulation was verified against the reference standard by comparing its single band at Rf 0.44 ± 0.02. Linearity was found to exist between 100 and 600 ng/band, with a correlation coefficient (r2) of 0.9978. The percentage recovery was obtained as 98.21%–99.05%. The system was validated by determining the parameters according to the guidelines of the International Council for Harmonization of Technical Conditions for Medical Products for Human Use. The proposed TLC method can be effectively applied to routine quality control of a pharmaceutical product.
{"title":"Analytical quality by design‐based thin‐layer chromatography method development and validation for assay and content uniformity testing of the anti‐neoplastic drug Axitinib in tablet formulation","authors":"Shaileshkumar K. Koradia, Madhavi Patel, A. Sen, D. Sen, Prasanna Pradhan","doi":"10.1002/sscp.202300176","DOIUrl":"https://doi.org/10.1002/sscp.202300176","url":null,"abstract":"The current study aims to develop and validate an analytical quality by design approach‐based high‐performance thin‐layer chromatographic (HPTLC) method for the analysis of Axitinib tablet samples. The chromatographic conditions in the TLC method were optimized using a three‐level full factorial design. The mobile phase composition and chamber saturation time served as the independent variables for optimization. The mobile phase used for TLC separation on pre‐coated aluminum plates with silica gel 60 F254 consisted of a mixture of ethyl acetate and isopropyl alcohol in a ratio of 9:1 (v/v). Axitinib was quantified at 330 nm using the densitometric method. Axitinib peak from tablet formulation was verified against the reference standard by comparing its single band at Rf 0.44 ± 0.02. Linearity was found to exist between 100 and 600 ng/band, with a correlation coefficient (r2) of 0.9978. The percentage recovery was obtained as 98.21%–99.05%. The system was validated by determining the parameters according to the guidelines of the International Council for Harmonization of Technical Conditions for Medical Products for Human Use. The proposed TLC method can be effectively applied to routine quality control of a pharmaceutical product.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":1.1,"publicationDate":"2023-12-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139005643","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}
Bereket Tesfaye, A. Gure, Tsegaye Girma Asere, Toleshi Teshome, Yerosan Buzayo
An efficient analytical method has been developed based on dispersive solid‐phase extraction followed by gas chromatography‐mass spectrometry for the determinations of 13 organochlorine pesticides in fruit juice samples. In this method, dispersive solid phase extraction was used for the extraction of target analye using iron‐doped zinc oxide nanoparticles supported with silica as a sorbent. Different experimental parameters affecting the extraction efficiencies the proposed method were carefully optimized. Under the optimum conditions, the calibration graphs were linear in the concentration range of 0.6–100 ng/mL with coefficients of determinations in the range of 0.9927–0.9991. The limits of detection and quantification determined as 3 and 10 times the signal‐to‐noise ratio were in the range of 0.01–0.03 and 0.6–1.0 ng/mL, respectively. Intra‐ and inter‐day precision studies of the proposed method, expressed as relative standard deviations, were in the range of 2.1%–9.2% and 2.2%–9.7%, respectively. The recoveries of the spiked fruit juices samples were in the range of 81.4%–105.1% with the corresponding relative standard deviations ranging from 1.0%–8.8%. In general, the proposed method demonstrated satisfactory analytical performance. Thus,it could be used as simple and attracive alternative method for the extraction of organochlorine pesticides from fruit juice sample and other related matrices.
{"title":"Dispersive solid‐phase extraction for the determination of organochlorine pesticides in fruit juice samples using iron‐doped zinc oxide nanoparticles supported with silica as a sorbent","authors":"Bereket Tesfaye, A. Gure, Tsegaye Girma Asere, Toleshi Teshome, Yerosan Buzayo","doi":"10.1002/sscp.202300161","DOIUrl":"https://doi.org/10.1002/sscp.202300161","url":null,"abstract":"An efficient analytical method has been developed based on dispersive solid‐phase extraction followed by gas chromatography‐mass spectrometry for the determinations of 13 organochlorine pesticides in fruit juice samples. In this method, dispersive solid phase extraction was used for the extraction of target analye using iron‐doped zinc oxide nanoparticles supported with silica as a sorbent. Different experimental parameters affecting the extraction efficiencies the proposed method were carefully optimized. Under the optimum conditions, the calibration graphs were linear in the concentration range of 0.6–100 ng/mL with coefficients of determinations in the range of 0.9927–0.9991. The limits of detection and quantification determined as 3 and 10 times the signal‐to‐noise ratio were in the range of 0.01–0.03 and 0.6–1.0 ng/mL, respectively. Intra‐ and inter‐day precision studies of the proposed method, expressed as relative standard deviations, were in the range of 2.1%–9.2% and 2.2%–9.7%, respectively. The recoveries of the spiked fruit juices samples were in the range of 81.4%–105.1% with the corresponding relative standard deviations ranging from 1.0%–8.8%. In general, the proposed method demonstrated satisfactory analytical performance. Thus,it could be used as simple and attracive alternative method for the extraction of organochlorine pesticides from fruit juice sample and other related matrices.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":1.1,"publicationDate":"2023-12-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138982252","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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