Priyanka Rani, Bibhu Prasad Nanda, R. Narang, Rohit Bhatia
Solvent microextraction (SME) is designed to selectively isolate desired analytes while minimizing the presence of interfering substances in the extracted sample. There are different approaches from which single‐drop microextraction (SDME) can be amalgamated with various analytical methods to enhance its functionalities and improve the analysis of extracted compounds like gas chromatography, and liquid chromatography amplify sensitivity, selectivity, and the capacity to detect trace amounts of analytes in complex matrices. The review focuses on the intricacies of solid‐phase microextraction and elucidates its operational principles. Additionally, it explores various types of SDMEs, detailing their respective benefits, drawbacks, and potential applications in the future. A typical explanation of the construction and working of hollow fiber‐liquid phase microextraction as well as its types has been discussed. The applications of SMEs in the medical and biomedical fields from food analysis to environmental analysis like analysis and purification of water, organic pollutants, drug analysis, and screening of new drugs have been discussed and also illustrated in tabular form. The pros and cons of both analytical techniques are given in a tabular manner as well a broad comparison between different types of advanced SME techniques provides a new direction for environmental monitoring, food safety, and refining of impurities from water samples. The review provides a comprehensive overview of the current progress, recent obstacles, and future possibilities of SMEs in an appropriate manner. Despite numerous promising advancements, the utilization of SMEs remains a challenging field.
溶剂微萃取（SME）旨在选择性地分离出所需的分析物，同时尽量减少萃取样品中干扰物质的存在。单滴微萃取（SDME）可以通过不同的方法与各种分析方法相结合，以增强其功能并改进对萃取化合物的分析，如气相色谱和液相色谱法可以提高灵敏度、选择性和检测复杂基质中痕量分析物的能力。综述重点介绍了固相微萃取的复杂性，并阐明了其操作原理。此外，它还探讨了各种类型的固相微萃取器，详细介绍了它们各自的优点、缺点以及在未来的潜在应用。文中还对中空纤维-液相微萃取的构造和工作原理及其类型进行了典型解释。还讨论了中小型企业在医疗和生物医学领域的应用，从食品分析到环境分析，如水的分析和净化、有机污染物、药物分析和新药筛选，并以表格形式进行了说明。两种分析技术的优缺点都以表格的形式给出，不同类型的先进 SME 技术之间的广泛比较也为环境监测、食品安全和提炼水样中的杂质提供了新的方向。综述以适当的方式全面概述了中小型企业的当前进展、近期障碍和未来可能性。尽管取得了许多令人鼓舞的进展，但中小型企业的利用仍然是一个充满挑战的领域。
{"title":"Advancements in solvent microextraction: Recent developments and diverse applications in the modern era","authors":"Priyanka Rani, Bibhu Prasad Nanda, R. Narang, Rohit Bhatia","doi":"10.1002/sscp.202300243","DOIUrl":"https://doi.org/10.1002/sscp.202300243","url":null,"abstract":"Solvent microextraction (SME) is designed to selectively isolate desired analytes while minimizing the presence of interfering substances in the extracted sample. There are different approaches from which single‐drop microextraction (SDME) can be amalgamated with various analytical methods to enhance its functionalities and improve the analysis of extracted compounds like gas chromatography, and liquid chromatography amplify sensitivity, selectivity, and the capacity to detect trace amounts of analytes in complex matrices. The review focuses on the intricacies of solid‐phase microextraction and elucidates its operational principles. Additionally, it explores various types of SDMEs, detailing their respective benefits, drawbacks, and potential applications in the future. A typical explanation of the construction and working of hollow fiber‐liquid phase microextraction as well as its types has been discussed. The applications of SMEs in the medical and biomedical fields from food analysis to environmental analysis like analysis and purification of water, organic pollutants, drug analysis, and screening of new drugs have been discussed and also illustrated in tabular form. The pros and cons of both analytical techniques are given in a tabular manner as well a broad comparison between different types of advanced SME techniques provides a new direction for environmental monitoring, food safety, and refining of impurities from water samples. The review provides a comprehensive overview of the current progress, recent obstacles, and future possibilities of SMEs in an appropriate manner. Despite numerous promising advancements, the utilization of SMEs remains a challenging field.","PeriodicalId":508518,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-03-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140081225","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}
Shivam Kumar, Sourabh Satapathy, B. Kurmi, Ghanshyam Das Gupta, Preeti Patel
This work presents a comprehensive overview of solidified floating organic drop microextraction, with a particular emphasis on its applications in the analysis of heavy metal ions and different pharmaceutical compounds by sample pretreatment, complexation, and their identification by various analytical techniques. Here, we discussed basic principles, procedures, applications of the technique, and effects of different variables like pH, temperature, stirring rate, extraction time, salts addition, extraction solvent and extraction volume, centrifugation speed, and, vortex time on preconcentration. In brief, the review summarises the various modes of solidified floating organic drop microextraction such as dispersive liquid‐liquid microextraction, ultrasound‐assisted, air‐assisted liquid‐liquid microextraction, and vortex‐assisted solidified floating organic drop microextraction. this review covers the methods combined with analytical techniques such as inductively coupled plasma‐optical emission spectrometry, electrothermal atomic absorption spectrometry, flame atomic absorption spectroscopy, graphite furnace atomic absorption spectrometry, electrothermal vaporization inductively coupled plasma mass spectrometry, high‐performance liquid chromatography, and gas chromatography/mass spectrometry. among these, the incorporation of ultrasonic, vortex, and air agitation improves the dispersion mechanism. The coupling of solidified floating organic drop microextraction with other techniques enhances the selectivity and efficiency of the preconcentration procedure. This review provides a potential overview of the fundamental principles, advancements in various modes, influencing factors, and applications of solidified floating organic drop microextraction, showing its potential for advancements in sample preparation and analytical methodologies across various domains.
{"title":"Recent overview of microextraction of metal ions and pharmaceuticals by solidified floating organic drop microextraction techniques","authors":"Shivam Kumar, Sourabh Satapathy, B. Kurmi, Ghanshyam Das Gupta, Preeti Patel","doi":"10.1002/sscp.202400018","DOIUrl":"https://doi.org/10.1002/sscp.202400018","url":null,"abstract":"This work presents a comprehensive overview of solidified floating organic drop microextraction, with a particular emphasis on its applications in the analysis of heavy metal ions and different pharmaceutical compounds by sample pretreatment, complexation, and their identification by various analytical techniques. Here, we discussed basic principles, procedures, applications of the technique, and effects of different variables like pH, temperature, stirring rate, extraction time, salts addition, extraction solvent and extraction volume, centrifugation speed, and, vortex time on preconcentration. In brief, the review summarises the various modes of solidified floating organic drop microextraction such as dispersive liquid‐liquid microextraction, ultrasound‐assisted, air‐assisted liquid‐liquid microextraction, and vortex‐assisted solidified floating organic drop microextraction. this review covers the methods combined with analytical techniques such as inductively coupled plasma‐optical emission spectrometry, electrothermal atomic absorption spectrometry, flame atomic absorption spectroscopy, graphite furnace atomic absorption spectrometry, electrothermal vaporization inductively coupled plasma mass spectrometry, high‐performance liquid chromatography, and gas chromatography/mass spectrometry. among these, the incorporation of ultrasonic, vortex, and air agitation improves the dispersion mechanism. The coupling of solidified floating organic drop microextraction with other techniques enhances the selectivity and efficiency of the preconcentration procedure. This review provides a potential overview of the fundamental principles, advancements in various modes, influencing factors, and applications of solidified floating organic drop microextraction, showing its potential for advancements in sample preparation and analytical methodologies across various domains.","PeriodicalId":508518,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-03-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140081165","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}
Aqeel Shahzad, Farzana Batool, Kamran Bashir, Jiameng Xu, Qiang Fu
Prostaglandin analogs (PGAs) are commonly used to treat ocular hypertension and glaucoma patients. Nowadays, the use of PGAs enhances eyelashes in cosmetics, particularly in the condition of hypotrichosis. A method was developed in which surface molecularly imprinted polymers were synthesized for selective extraction of PGAs (bimatoprost, latanoprost, and travoprost) by using bimatoprost as template molecules which were coupled with liquid chromatography‐mass spectrometry (LC‐MS) system. Scanning electron microscopy and Fourier‐transform infrared spectroscopy techniques were used to study the morphological and physical characterization. The adsorption selectivity studies showed the high selectivity of PGAs. The adsorption capacities of bimatoprost, latanoprost, and travoprost were 93.8, 92.3, and 91.5 μg/g, respectively. The recoveries and precision of samples at three concentration levels (10–30 ng/mL) of bimatoprost, latanoprost, and travoprost were tested (98.5%–102.5%, 1.2%–4.5%, n = 3). The % relative standard deviation for repeatability of the method for bimatoprost, latanoprost, and travoprost ranged from 1.8 to 5.6, 1.5 to 4.8, and 1.6 to 5.2, respectively. While the limit of detection for bimatoprost, latanoprost, and travoprost was 0.20, 0.25, and 0.45 ng/mL, respectively. The method of surface molecularly imprinted polymer coupled with LC‐MS was successfully applied to cosmetic products for selective extraction of PGAs.
{"title":"Preparation and characterization of vinyl silica‐supported surface molecularly imprinted polymers coupled with liquid chromatography‐mass spectrometry for extraction of prostaglandin analogs from cosmetic products","authors":"Aqeel Shahzad, Farzana Batool, Kamran Bashir, Jiameng Xu, Qiang Fu","doi":"10.1002/sscp.202300184","DOIUrl":"https://doi.org/10.1002/sscp.202300184","url":null,"abstract":"Prostaglandin analogs (PGAs) are commonly used to treat ocular hypertension and glaucoma patients. Nowadays, the use of PGAs enhances eyelashes in cosmetics, particularly in the condition of hypotrichosis. A method was developed in which surface molecularly imprinted polymers were synthesized for selective extraction of PGAs (bimatoprost, latanoprost, and travoprost) by using bimatoprost as template molecules which were coupled with liquid chromatography‐mass spectrometry (LC‐MS) system. Scanning electron microscopy and Fourier‐transform infrared spectroscopy techniques were used to study the morphological and physical characterization. The adsorption selectivity studies showed the high selectivity of PGAs. The adsorption capacities of bimatoprost, latanoprost, and travoprost were 93.8, 92.3, and 91.5 μg/g, respectively. The recoveries and precision of samples at three concentration levels (10–30 ng/mL) of bimatoprost, latanoprost, and travoprost were tested (98.5%–102.5%, 1.2%–4.5%, n = 3). The % relative standard deviation for repeatability of the method for bimatoprost, latanoprost, and travoprost ranged from 1.8 to 5.6, 1.5 to 4.8, and 1.6 to 5.2, respectively. While the limit of detection for bimatoprost, latanoprost, and travoprost was 0.20, 0.25, and 0.45 ng/mL, respectively. The method of surface molecularly imprinted polymer coupled with LC‐MS was successfully applied to cosmetic products for selective extraction of PGAs.","PeriodicalId":508518,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-02-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139963794","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}
R. Mahajan, Sai Teja Chandragiri, Vivek Borse, Gananadhamu Samanthula, Amit Asthana
This paper described a short and precise reverse‐phase high‐performance liquid chromatography (HPLC) method for quantifying mafenide in a film‐forming spray and preliminary in‐vitro release study. Following the International Council for Harmonization guidelines Q2 (R1), the method was validated. The chromatographic separation was achieved using a 10 mM potassium dihydrogen phosphate solution (mobile phase A) mixed with HPLC‐grade methanol (mobile phase B) in an 85:15 v/v ratio. Inert Sustain C8 (4.6 × 250 mm), 5 μm column was selected as the stationary phase. The flow rate was set as 0.8 mL/min, and detection was carried out at a wavelength of 222 nm. The developed HPLC method showed an accuracy between 98% and 102%. The primary diffusion study of film‐forming spray was performed using the Franz vertical diffusion cell apparatus. It was observed that an average of 26.94% of drug releases at 24 h. This indicates the drug has a slower release rate and shows local pharmacological action. The Weibull dissolution model was more fitting with regression square 0.9953. Furthermore, the drug excipient compatibility study revealed no interactions as the only drug peak was found in the chromatographic method, indicating that the chosen excipients were appropriate for a stable formulation.
{"title":"Reverse‐phase high‐performance liquid chromatography methodology for film‐forming mafenide spray: Compatibility, assay, and in‐vitro release evaluation using Franz vertical diffusion cell apparatus","authors":"R. Mahajan, Sai Teja Chandragiri, Vivek Borse, Gananadhamu Samanthula, Amit Asthana","doi":"10.1002/sscp.202300148","DOIUrl":"https://doi.org/10.1002/sscp.202300148","url":null,"abstract":"This paper described a short and precise reverse‐phase high‐performance liquid chromatography (HPLC) method for quantifying mafenide in a film‐forming spray and preliminary in‐vitro release study. Following the International Council for Harmonization guidelines Q2 (R1), the method was validated. The chromatographic separation was achieved using a 10 mM potassium dihydrogen phosphate solution (mobile phase A) mixed with HPLC‐grade methanol (mobile phase B) in an 85:15 v/v ratio. Inert Sustain C8 (4.6 × 250 mm), 5 μm column was selected as the stationary phase. The flow rate was set as 0.8 mL/min, and detection was carried out at a wavelength of 222 nm. The developed HPLC method showed an accuracy between 98% and 102%. The primary diffusion study of film‐forming spray was performed using the Franz vertical diffusion cell apparatus. It was observed that an average of 26.94% of drug releases at 24 h. This indicates the drug has a slower release rate and shows local pharmacological action. The Weibull dissolution model was more fitting with regression square 0.9953. Furthermore, the drug excipient compatibility study revealed no interactions as the only drug peak was found in the chromatographic method, indicating that the chosen excipients were appropriate for a stable formulation.","PeriodicalId":508518,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-02-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139683520","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}
Haiqiang Zhang, Jinqin Han, Qiao Li, Jianing Nie, Luanwei Han, Yang Yu, Chongning Lv, Jincai Lu
In the present study, a comprehensive strategy based on substances profiling in vivo and network pharmacology method was applied to screen out the potential immunomodulatory activity substances and mechanism of Wu Shen Wan. As a result, a total of 121 constituents were identified or tentatively characterized, including 26 flavonoids, 16 alkaloids, 10 tanshinones, four diterpenes, seven iridoid glycosides, eight coumarin, 18 phenolic acids, 29 ginsenosides, and three others. Moreover, 57 prototypes were clearly screened out in rat plasma and urine after ingestion of Wu Shen Wan. The Wu Shen Wan exhibited immunomodulatory effects via significantly increasing the phagocytic activity of macrophages and inducing the release of nitric oxide, tumor necrosis factor‐α, and interleukin 6 in RAW264.7 cells. In addition, the network pharmacology results showed that the top 20 Kyoto Encyclopedia of Genes and Genomes clusters were enriched, such as mitogen‐activated protein kinases pathway. This is the first systematic study on the chemical constituents of Wu Shen Wan. The analytical method features a quick and comprehensive dissection of the chemical composition and provides a basis for exploring its immunomodulatory effects.
{"title":"Dissection of the potential immunomodulatory activity materials and mechanism of Wu Shen Wan (a classical traditional Chinese medicine prescription) based on in vivo substances profiling and network pharmacology","authors":"Haiqiang Zhang, Jinqin Han, Qiao Li, Jianing Nie, Luanwei Han, Yang Yu, Chongning Lv, Jincai Lu","doi":"10.1002/sscp.202300155","DOIUrl":"https://doi.org/10.1002/sscp.202300155","url":null,"abstract":"In the present study, a comprehensive strategy based on substances profiling in vivo and network pharmacology method was applied to screen out the potential immunomodulatory activity substances and mechanism of Wu Shen Wan. As a result, a total of 121 constituents were identified or tentatively characterized, including 26 flavonoids, 16 alkaloids, 10 tanshinones, four diterpenes, seven iridoid glycosides, eight coumarin, 18 phenolic acids, 29 ginsenosides, and three others. Moreover, 57 prototypes were clearly screened out in rat plasma and urine after ingestion of Wu Shen Wan. The Wu Shen Wan exhibited immunomodulatory effects via significantly increasing the phagocytic activity of macrophages and inducing the release of nitric oxide, tumor necrosis factor‐α, and interleukin 6 in RAW264.7 cells. In addition, the network pharmacology results showed that the top 20 Kyoto Encyclopedia of Genes and Genomes clusters were enriched, such as mitogen‐activated protein kinases pathway. This is the first systematic study on the chemical constituents of Wu Shen Wan. The analytical method features a quick and comprehensive dissection of the chemical composition and provides a basis for exploring its immunomodulatory effects.","PeriodicalId":508518,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-01-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139622556","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 physicochemical diversity of the structurally related aromatic probe drugs, used together in a drug cocktail to assess metabolic and transport phenotypes, require optimized analytical procedures for simultaneous quantification. The analytical conditions can greatly influence the analyte selectivity, retention, stability, and ultimately the robustness of the method. The aim of this study was to assess the selectivity of the structurally related ionizable analytes between the commonly used C18 column chemistry and an alternative biphenyl column chemistry as well as the influence of changes in the analytical conditions on method robustness using liquid chromatography‐tandem mass spectrometry. A repeated measure two‐factor analysis of variance with Geisser‐Greenhouse correction was used to determine statistical significance. The results showed that a biphenyl stationary phase in combination with methanol as the organic eluent, could provide improved resolution and analyte selectivity. Changes in analytical conditions caused statistically significant variation in the retention behavior, selectivity, column efficiency, and sensitivity of the analytes of interest The robustness experiment confirmed the importance of controlling analytical conditions to ensure the reproducibility and reliability of the quantitative method.
{"title":"Bioanalytical method optimization for simultaneous quantification of structurally related probe drugs in a phenotyping cocktail using liquid chromatography‐tandem mass spectrometry","authors":"Machel Leuschner, Duncan Cromarty","doi":"10.1002/sscp.202300241","DOIUrl":"https://doi.org/10.1002/sscp.202300241","url":null,"abstract":"The physicochemical diversity of the structurally related aromatic probe drugs, used together in a drug cocktail to assess metabolic and transport phenotypes, require optimized analytical procedures for simultaneous quantification. The analytical conditions can greatly influence the analyte selectivity, retention, stability, and ultimately the robustness of the method. The aim of this study was to assess the selectivity of the structurally related ionizable analytes between the commonly used C18 column chemistry and an alternative biphenyl column chemistry as well as the influence of changes in the analytical conditions on method robustness using liquid chromatography‐tandem mass spectrometry. A repeated measure two‐factor analysis of variance with Geisser‐Greenhouse correction was used to determine statistical significance. The results showed that a biphenyl stationary phase in combination with methanol as the organic eluent, could provide improved resolution and analyte selectivity. Changes in analytical conditions caused statistically significant variation in the retention behavior, selectivity, column efficiency, and sensitivity of the analytes of interest The robustness experiment confirmed the importance of controlling analytical conditions to ensure the reproducibility and reliability of the quantitative method.","PeriodicalId":508518,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-01-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139626263","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 simple quality by design aided stability indicating method was developed for quantification of sonidegib (SONI) and its process related impurities using on ultra‐performance liquid chromatography in bulk drug substance. AutoChrom and Design‐Expert software were used to predict physicochemical properties, draw Ionization graphs, and generate analytical target profile. SONI was subjected to forced degradation conditions, such as oxidative, acid hydrolysis, base hydrolysis, hydrolytic, thermal, and photolytic hydrolysis. All degradation products and process contaminants were separated using an Acquity Ethylene Bridged Hybrid C18 column in gradient elution mode with a mobile phase containing 0.02 M ammonium acetate buffer and acetonitrile: methanol (80:20 v/v). The predicted physicochemical properties are accurate and they facilitated for selection of robust conditions in development of chromatographic method with minimal trials. The developed method can be used for quantification of drug and its process related impurities in bulk drugs.
利用超高效液相色谱法，开发了一种简单的质量设计辅助稳定性指示方法，用于定量检测散装药物中的索尼吉布（SONI）及其工艺相关杂质。使用 AutoChrom 和 Design-Expert 软件预测理化性质、绘制电离图并生成分析目标曲线。对 SONI 进行了强制降解，如氧化、酸水解、碱水解、水解、热水解和光解。使用 Acquity 乙烯桥接混合型 C18 色谱柱，以 0.02 M 乙酸铵缓冲液和乙腈：甲醇（80:20 v/v）为流动相，在梯度洗脱模式下分离所有降解产物和工艺污染物。所预测的理化性质非常准确，有助于在开发色谱方法时以最少的试验选择可靠的条件。所开发的方法可用于定量检测散装药物中的药物及其工艺相关杂质。
{"title":"Analytical quality by design aided stability indicating a robust ultra‐performance liquid chromatographic technique for the quantification of sonidegib and its organic impurities in bulk drug substance","authors":"Kasturi Rajashekhar, Challa Gangu Naidu, Chebolu Naga Sesha Sai Pavan Kumar, Bondigalla Ramachandra, Raju Padiya","doi":"10.1002/sscp.202300181","DOIUrl":"https://doi.org/10.1002/sscp.202300181","url":null,"abstract":"A simple quality by design aided stability indicating method was developed for quantification of sonidegib (SONI) and its process related impurities using on ultra‐performance liquid chromatography in bulk drug substance. AutoChrom and Design‐Expert software were used to predict physicochemical properties, draw Ionization graphs, and generate analytical target profile. SONI was subjected to forced degradation conditions, such as oxidative, acid hydrolysis, base hydrolysis, hydrolytic, thermal, and photolytic hydrolysis. All degradation products and process contaminants were separated using an Acquity Ethylene Bridged Hybrid C18 column in gradient elution mode with a mobile phase containing 0.02 M ammonium acetate buffer and acetonitrile: methanol (80:20 v/v). The predicted physicochemical properties are accurate and they facilitated for selection of robust conditions in development of chromatographic method with minimal trials. The developed method can be used for quantification of drug and its process related impurities in bulk drugs.","PeriodicalId":508518,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-01-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139625869","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}
Babu Reddy Goguladinne, Pulipaka Shyamala, K. M. V. N. Rao
Etoricoxib (ETO) is a selective cyclooxygenase‐2 inhibitor, used as a nonsteroidal anti‐inflammatory drug. In this study, a detailed investigation was conducted on the degradation behavior of ETO under acidic, basic, neutral, photolytic, oxidative, and thermal degradation conditions as per the International Conference on Harmonization (ICH) guideline Q1A (R2). A gradient “ultra‐performance liquid chromatography (UPLC)” method was developed for separating the degradation products formed under various degradation conditions along with process‐related impurities. Acquity BEH phenyl column was used for the separation of analytes and 0.1% formic acid in water and 0.05% formic acid in acetonitrile:methanol (8:2 %v/v) were used as mobile phase‐A and mobile phase‐B. A major degradant namely, N‐oxide impurity was observed in oxidative degradation along with two minor degradants where N‐oxide was confirmed based on LC‐mass spectrometry (LC‐MS) studies. Further, the major degradant was enriched and isolated using preparative HPLC and the conformation of the N‐oxide impurity was established using nuclear magnetic resonance techniques including two‐dimensional studies and high‐resolution MS. In addition, the method for related substances by UPLC has been validated by considering a major degradant, namely N‐oxide along with process‐related impurities as per the ICH guidelines validation parameters.
依托考昔（ETO）是一种选择性环氧化酶-2 抑制剂，用作非甾体抗炎药。本研究根据国际协调会议（ICH）指南 Q1A (R2)，对 ETO 在酸性、碱性、中性、光解、氧化和热降解条件下的降解行为进行了详细调查。开发了一种梯度 "超高效液相色谱（UPLC）"方法，用于分离在各种降解条件下形成的降解产物以及与工艺相关的杂质。Acquity BEH苯基色谱柱用于分离分析物，0.1%甲酸水溶液和0.05%甲酸乙腈：甲醇（8:2 %v/v）水溶液分别用作流动相A和流动相B。在氧化降解过程中观察到一种主要降解物，即 N-氧化物杂质，以及两种次要降解物，其中 N-氧化物是根据 LC-MS 研究确认的。此外，还利用制备型高效液相色谱法富集和分离了主要降解物，并利用核磁共振技术（包括二维研究和高分辨率质谱）确定了 N-氧化物杂质的构象。此外，还根据 ICH 指南的验证参数，考虑了一种主要降解剂（即 N-氧化物）以及与工艺相关的杂质，验证了通过 UPLC 检测相关物质的方法。
{"title":"Stress degradation study of Etoricoxib, isolation, and characterization of major degradation impurity by preparative high‐performance liquid chromatography, liquid chromatography‐mass spectrometry, and nuclear magnetic resonance: Validation of ultra‐performance liquid chromatography method","authors":"Babu Reddy Goguladinne, Pulipaka Shyamala, K. M. V. N. Rao","doi":"10.1002/sscp.202300106","DOIUrl":"https://doi.org/10.1002/sscp.202300106","url":null,"abstract":"Etoricoxib (ETO) is a selective cyclooxygenase‐2 inhibitor, used as a nonsteroidal anti‐inflammatory drug. In this study, a detailed investigation was conducted on the degradation behavior of ETO under acidic, basic, neutral, photolytic, oxidative, and thermal degradation conditions as per the International Conference on Harmonization (ICH) guideline Q1A (R2). A gradient “ultra‐performance liquid chromatography (UPLC)” method was developed for separating the degradation products formed under various degradation conditions along with process‐related impurities. Acquity BEH phenyl column was used for the separation of analytes and 0.1% formic acid in water and 0.05% formic acid in acetonitrile:methanol (8:2 %v/v) were used as mobile phase‐A and mobile phase‐B. A major degradant namely, N‐oxide impurity was observed in oxidative degradation along with two minor degradants where N‐oxide was confirmed based on LC‐mass spectrometry (LC‐MS) studies. Further, the major degradant was enriched and isolated using preparative HPLC and the conformation of the N‐oxide impurity was established using nuclear magnetic resonance techniques including two‐dimensional studies and high‐resolution MS. In addition, the method for related substances by UPLC has been validated by considering a major degradant, namely N‐oxide along with process‐related impurities as per the ICH guidelines validation parameters.","PeriodicalId":508518,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-01-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139444689","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}
Zolfaghar Aladaghlo, Ali Sahragard, Alireza Fakhari
Solvent‐assisted dispersive solid‐phase extraction (SA‐DSPE) approach was developed to measure triazole fungicides (TFs). In the SA‐DSPE technique, the addition of 1000 μL of ethanol as a disperser solvent, along with a small quantity of benzil as a sorbent to the sample solution, led to a cloudy solution. After completion of the extraction, the mixture was subjected to centrifugation to isolate benzil. Next, benzil was dissolved in ethanol, and the resulting solution was subsequently analyzed by a gas chromatography‐flame ionization detector. This method demonstrated high linearity (R2 > 0.9963) and repeatability (relative standard deviation % < 4.3) for the quantification of TFs under the optimal conditions (sorbent: benzil, amount of benzil: 2% w/v, pH of solution: 7.0, disperser solvent: ethanol, volumes of ethanol: 1000 μL, centrifuge time: 3 min, extraction temperature: 25°C, and ionic strength: without salt addition). The proposed SA‐DSPE yielded detection limits, quantification limits, and preconcentration factors within the ranges of 0.3–0.9 ng/mL, 1.0–3.0 ng/mL, and 419–426, respectively. Finally, the validated method was employed to determine TFs in a diverse range of real samples, encompassing waters, fruits, vegetables, and agricultural soils, with relative recoveries ranging from 93.0% to 104%.
{"title":"Development of a simple and fast method named solvent‐assisted dispersive solid phase extraction for trace detection of triazole fungicides in water, fruit, vegetable, and agricultural soil samples","authors":"Zolfaghar Aladaghlo, Ali Sahragard, Alireza Fakhari","doi":"10.1002/sscp.202300191","DOIUrl":"https://doi.org/10.1002/sscp.202300191","url":null,"abstract":"Solvent‐assisted dispersive solid‐phase extraction (SA‐DSPE) approach was developed to measure triazole fungicides (TFs). In the SA‐DSPE technique, the addition of 1000 μL of ethanol as a disperser solvent, along with a small quantity of benzil as a sorbent to the sample solution, led to a cloudy solution. After completion of the extraction, the mixture was subjected to centrifugation to isolate benzil. Next, benzil was dissolved in ethanol, and the resulting solution was subsequently analyzed by a gas chromatography‐flame ionization detector. This method demonstrated high linearity (R2 > 0.9963) and repeatability (relative standard deviation % < 4.3) for the quantification of TFs under the optimal conditions (sorbent: benzil, amount of benzil: 2% w/v, pH of solution: 7.0, disperser solvent: ethanol, volumes of ethanol: 1000 μL, centrifuge time: 3 min, extraction temperature: 25°C, and ionic strength: without salt addition). The proposed SA‐DSPE yielded detection limits, quantification limits, and preconcentration factors within the ranges of 0.3–0.9 ng/mL, 1.0–3.0 ng/mL, and 419–426, respectively. Finally, the validated method was employed to determine TFs in a diverse range of real samples, encompassing waters, fruits, vegetables, and agricultural soils, with relative recoveries ranging from 93.0% to 104%.","PeriodicalId":508518,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-01-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139448387","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 quantitative high‐performance thin‐layer chromatography method has been developed for the estimation of three markers gallic acid, quercetin, and ursolic acid in the extracts and combined formulation of Emblica officinalis, Punica granatum Linn, and Ocimum sanctum Linn extracts. Chromatographic development was performed using precoated silica gel 60 F254 TLC plate and final optimized mobile phase as toluene:ethyl acetate:formic acid (4.5:3:0.2 v/v/v), resulting in optimum resolution with Rf of 0.29, 0.51, and 0.78 for gallic acid, quercetin, and ursolic acid, respectively. Gallic acid and quercetin were detected at 258 nm and ursolic acid at 529 nm after derivatization. All markers showed a good correlation coefficient of 0.9950 for gallic acid, 0.9953 for quercetin, and 0.9945 for ursolic acid. The accuracy and precision measured were less than 2% relative standard deviation for all markers. The mean percent recovery found for gallic acid, quercetin, and ursolic acid were within acceptable limits in formulation indicating that the excipients present have no interference. The proposed method was found to be specific, accurate, linear, precise, and robust, and can be applicable for the simultaneous estimation of gallic acid, quercetin, and ursolic acid for the analysis of individual plant extracts and herbal formulation.
{"title":"Validated high‐performance thin‐layer chromatographic densitometric method for quantification of gallic acid, quercetin, and ursolic acid in the combined formulation of Emblica officinalis, Punica granatum Linn, and Ocimum sanctum Linn extracts","authors":"K. Patel, Gandhi Vasima, P. Shah, V. Thakkar","doi":"10.1002/sscp.202300083","DOIUrl":"https://doi.org/10.1002/sscp.202300083","url":null,"abstract":"A quantitative high‐performance thin‐layer chromatography method has been developed for the estimation of three markers gallic acid, quercetin, and ursolic acid in the extracts and combined formulation of Emblica officinalis, Punica granatum Linn, and Ocimum sanctum Linn extracts. Chromatographic development was performed using precoated silica gel 60 F254 TLC plate and final optimized mobile phase as toluene:ethyl acetate:formic acid (4.5:3:0.2 v/v/v), resulting in optimum resolution with Rf of 0.29, 0.51, and 0.78 for gallic acid, quercetin, and ursolic acid, respectively. Gallic acid and quercetin were detected at 258 nm and ursolic acid at 529 nm after derivatization. All markers showed a good correlation coefficient of 0.9950 for gallic acid, 0.9953 for quercetin, and 0.9945 for ursolic acid. The accuracy and precision measured were less than 2% relative standard deviation for all markers. The mean percent recovery found for gallic acid, quercetin, and ursolic acid were within acceptable limits in formulation indicating that the excipients present have no interference. The proposed method was found to be specific, accurate, linear, precise, and robust, and can be applicable for the simultaneous estimation of gallic acid, quercetin, and ursolic acid for the analysis of individual plant extracts and herbal formulation.","PeriodicalId":508518,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-01-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139386237","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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