Mahmoud Tareq Abdelwahed, Maha A. Hegazy, Ekram H Mohamed
Abstract Ashwagandha (Withania somnifera) is a very popular medicinal herb originated mainly in India and found in the Middle East and parts of Africa. Ashwagandha has gained recognition as the most revered plant in Ayurvedic medicine. Studies indicated that it is used as anxiolytic, anti-inflammatory, antioxidant, adaptogen, memory enhancer, and possess an effect on neurodegenerative diseases. Additionally, it was revealed that the plant exerts antibacterial, antiviral, antitumor, aphrodisiac, and cardiovascular protection activities. Due to the biological and nutritional importance of nutraceuticals, particularly ashwagandha, and as part of the ongoing research of the natural products and its bioactive phytochemicals, this review aims to summarize the recent analytical techniques that have been reported for the determination of different chemical constituents of Withania somnifera quantitatively and qualitatively, and to highlight new challenges.
{"title":"Major biochemical constituents of Withania somnifera (ashwagandha) extract: A review of chemical analysis","authors":"Mahmoud Tareq Abdelwahed, Maha A. Hegazy, Ekram H Mohamed","doi":"10.1515/revac-2022-0055","DOIUrl":"https://doi.org/10.1515/revac-2022-0055","url":null,"abstract":"Abstract Ashwagandha (Withania somnifera) is a very popular medicinal herb originated mainly in India and found in the Middle East and parts of Africa. Ashwagandha has gained recognition as the most revered plant in Ayurvedic medicine. Studies indicated that it is used as anxiolytic, anti-inflammatory, antioxidant, adaptogen, memory enhancer, and possess an effect on neurodegenerative diseases. Additionally, it was revealed that the plant exerts antibacterial, antiviral, antitumor, aphrodisiac, and cardiovascular protection activities. Due to the biological and nutritional importance of nutraceuticals, particularly ashwagandha, and as part of the ongoing research of the natural products and its bioactive phytochemicals, this review aims to summarize the recent analytical techniques that have been reported for the determination of different chemical constituents of Withania somnifera quantitatively and qualitatively, and to highlight new challenges.","PeriodicalId":21090,"journal":{"name":"Reviews in Analytical Chemistry","volume":"36 1","pages":""},"PeriodicalIF":4.3,"publicationDate":"2023-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"88956990","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
G. Granados-Guzmán, Mónica Díaz-Hernández, R. Álvarez-Román, Norma Cavazos-Rocha, Omar J. Portillo-Castillo
Abstract Currently, sample preparation is the most laborious part of the analytical process, requiring the most time and being susceptible to the most errors. In this context, numerous investigations have focused on the miniaturization of these techniques to reduce work time, costs, and errors. In this regard, microextraction by packed sorbent (MEPS) is a simple, fast, and robust sample preparation technique suitable for easy automation in several analytical systems and is applied to a wide variety of samples. Antibiotics are among the most commonly used drugs; however, their extensive and inappropriate use has garnered significant attention in the environment, human health, and food safety. This brief review is intended to provide an overview of recently reported antibiotic extraction methods based on MEPS, with a special interest in those applied to the analysis of biological, environmental, and food samples. In addition, the sample pretreatment step before extraction by the MEPS device was highlighted, as was the description of the sample-related steps within the MEPS procedure, such as extraction, washing, and elution.
{"title":"A brief review of the application of microextraction by packed sorbent for antibiotics analysis from biological, food, and environmental samples","authors":"G. Granados-Guzmán, Mónica Díaz-Hernández, R. Álvarez-Román, Norma Cavazos-Rocha, Omar J. Portillo-Castillo","doi":"10.1515/revac-2023-0057","DOIUrl":"https://doi.org/10.1515/revac-2023-0057","url":null,"abstract":"Abstract Currently, sample preparation is the most laborious part of the analytical process, requiring the most time and being susceptible to the most errors. In this context, numerous investigations have focused on the miniaturization of these techniques to reduce work time, costs, and errors. In this regard, microextraction by packed sorbent (MEPS) is a simple, fast, and robust sample preparation technique suitable for easy automation in several analytical systems and is applied to a wide variety of samples. Antibiotics are among the most commonly used drugs; however, their extensive and inappropriate use has garnered significant attention in the environment, human health, and food safety. This brief review is intended to provide an overview of recently reported antibiotic extraction methods based on MEPS, with a special interest in those applied to the analysis of biological, environmental, and food samples. In addition, the sample pretreatment step before extraction by the MEPS device was highlighted, as was the description of the sample-related steps within the MEPS procedure, such as extraction, washing, and elution.","PeriodicalId":21090,"journal":{"name":"Reviews in Analytical Chemistry","volume":"2 1","pages":""},"PeriodicalIF":4.3,"publicationDate":"2023-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"85000995","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Liu Yang, Molin Qin, Genwei Zhang, Jie Yang, Junchao Yang, Jiang Zhao
Abstract Chemical warfare agents (CWAs) are chemical substances intended for use in military operations to kill, injure, or incapacitate an enemy. It is very important to detect toxic CWAs at trace levels on site. Compared with traditional CWA analysis instrument methods, chemiresistive gas sensors present advantages of being small, fast, and inexpensive. Chemiresistive gas sensors are still an important research topic with the development of nanofabrication technology and new kinds of sensing materials, including carbon nanotubes, graphene, and black phosphorus (BP). Chemiresistive gas sensors are divided into three categories according to the type of sensitive materials: carbon- and BP-based materials, conductive polymers, and metal oxide semiconductors. A brief analysis was carried out on fabrication strategies using sensitive materials, including hydrogen bonding strategies, nanostructures, morphology, doping effects, composite materials, and other material application methods, and the sensitive materials and detection effects are summarized in this study. This review aims to provide guidance in the development of chemiresistive sensors for the detection of CWAs. Graphical abstract
{"title":"Progress of sensitive materials in chemiresistive sensors for detecting chemical warfare agent simulants: A review","authors":"Liu Yang, Molin Qin, Genwei Zhang, Jie Yang, Junchao Yang, Jiang Zhao","doi":"10.1515/revac-2022-0052","DOIUrl":"https://doi.org/10.1515/revac-2022-0052","url":null,"abstract":"Abstract Chemical warfare agents (CWAs) are chemical substances intended for use in military operations to kill, injure, or incapacitate an enemy. It is very important to detect toxic CWAs at trace levels on site. Compared with traditional CWA analysis instrument methods, chemiresistive gas sensors present advantages of being small, fast, and inexpensive. Chemiresistive gas sensors are still an important research topic with the development of nanofabrication technology and new kinds of sensing materials, including carbon nanotubes, graphene, and black phosphorus (BP). Chemiresistive gas sensors are divided into three categories according to the type of sensitive materials: carbon- and BP-based materials, conductive polymers, and metal oxide semiconductors. A brief analysis was carried out on fabrication strategies using sensitive materials, including hydrogen bonding strategies, nanostructures, morphology, doping effects, composite materials, and other material application methods, and the sensitive materials and detection effects are summarized in this study. This review aims to provide guidance in the development of chemiresistive sensors for the detection of CWAs. Graphical abstract","PeriodicalId":21090,"journal":{"name":"Reviews in Analytical Chemistry","volume":"196 1","pages":""},"PeriodicalIF":4.3,"publicationDate":"2023-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"78979649","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Dikshita Panwar, D. Shrivastava, Shalaka Bhawal, L. K. Gupta, N. S. S. Kumar, A. D. Chintagunta
Abstract Exosomes are nanosized cell-derived vesicles that have recently gained attention for their use as a biomarker since the biomolecules encountered in these vesicles are directly linked to specific diseases including immuno-inflammatory, cardiovascular, and hepatic disorders. Furthermore, due to their nano size and safe travel in extracellular fluids, exosomes have been investigated as natural drug delivery systems, delivering cargo to destined cells with excellent specificity and efficiency, and crossing the blood–brain barrier. This necessitates the isolation and detection of exosomes. However, numerous exosome isolation techniques are available, including ultracentrifugation, size-based chromatography, polymer precipitation, microfluidics, and immunoaffinity-based isolation, with the downfalls of non-specificity and lower cost-effectiveness. This article introduces an immunoaffinity-based detection of exosomes using targeted anti-exosome antibodies raised in chickens due to its economic and commercial viability. The current study is unique in that it identified a specific antigenic region on exosomal surface tetraspanins (CD9, CD63, CD81) and constructed a multiple antigenic peptide dendrimer for making a small peptide as an immunogen without the use of a carrier protein. The antigenic region selection is critical to the study because it determines the efficiency of antibodies for exosome capture. This technique was validated using enzyme-linked immunosorbent assay in various biological fluids such as serum, urine, milk, plasma, and blood due to its numerous advantages including high sensitivity, specificity, handling multiple samples at once, requiring a small sample amount, and no purification as an antigen. In light of this technique, it is a useful tool for clinical monitoring of the patient’s biological conditions. Graphical abstract
{"title":"Detection of exosomes in various biological fluids utilizing specific epitopes and directed multiple antigenic peptide antibodies","authors":"Dikshita Panwar, D. Shrivastava, Shalaka Bhawal, L. K. Gupta, N. S. S. Kumar, A. D. Chintagunta","doi":"10.1515/revac-2023-0056","DOIUrl":"https://doi.org/10.1515/revac-2023-0056","url":null,"abstract":"Abstract Exosomes are nanosized cell-derived vesicles that have recently gained attention for their use as a biomarker since the biomolecules encountered in these vesicles are directly linked to specific diseases including immuno-inflammatory, cardiovascular, and hepatic disorders. Furthermore, due to their nano size and safe travel in extracellular fluids, exosomes have been investigated as natural drug delivery systems, delivering cargo to destined cells with excellent specificity and efficiency, and crossing the blood–brain barrier. This necessitates the isolation and detection of exosomes. However, numerous exosome isolation techniques are available, including ultracentrifugation, size-based chromatography, polymer precipitation, microfluidics, and immunoaffinity-based isolation, with the downfalls of non-specificity and lower cost-effectiveness. This article introduces an immunoaffinity-based detection of exosomes using targeted anti-exosome antibodies raised in chickens due to its economic and commercial viability. The current study is unique in that it identified a specific antigenic region on exosomal surface tetraspanins (CD9, CD63, CD81) and constructed a multiple antigenic peptide dendrimer for making a small peptide as an immunogen without the use of a carrier protein. The antigenic region selection is critical to the study because it determines the efficiency of antibodies for exosome capture. This technique was validated using enzyme-linked immunosorbent assay in various biological fluids such as serum, urine, milk, plasma, and blood due to its numerous advantages including high sensitivity, specificity, handling multiple samples at once, requiring a small sample amount, and no purification as an antigen. In light of this technique, it is a useful tool for clinical monitoring of the patient’s biological conditions. Graphical abstract","PeriodicalId":21090,"journal":{"name":"Reviews in Analytical Chemistry","volume":"73 1","pages":""},"PeriodicalIF":4.3,"publicationDate":"2023-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"78062402","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Abstract This study presents an in-depth review of non-dispersive infrared (NDIR) sensors for methane detection, focusing on their principles of operation, performance characteristics, advanced signal processing techniques, multi-gas detection capabilities, and applications in various industries. NDIR sensors offer significant advantages in methane sensing, including high sensitivity, selectivity, and long-term stability. The underlying principles of NDIR sensors involve measuring the absorption of infrared radiation by the target gas molecules, leading to precise and reliable methane concentration measurements. Advanced signal processing techniques, such as single-frequency filtering and wavelet filtering algorithms, have been explored to improve the performance of the sensor by reducing noise, enhancing the signal-to-noise ratio, and achieving more accurate results. In the context of multi-gas detection, NDIR sensors face challenges due to overlapping absorption spectra. However, various solutions, including narrow-band optical bandpass filters, gas filter correlation techniques, and machine learning algorithms, have been proposed to address these issues effectively. This study delves into specific applications of NDIR sensors in various industries, such as coal mines, wastewater treatment plants, and agriculture. In these settings, NDIR sensors have demonstrated their reliability, accuracy, and real-time monitoring capabilities, contributing to environmental protection, safety, and energy recovery. Furthermore, the anticipated future trends and developments in NDIR methane detection technology are explored, including increased miniaturization, integration with artificial intelligence, improvements in power efficiency, and the development of multi-gas NDIR sensors. These advancements are expected to further enhance the capabilities and widespread adoption of NDIR sensors in methane detection applications.
{"title":"Enhancing methane sensing with NDIR technology: Current trends and future prospects","authors":"Li Fu, Shixi You, Guangjun Li, Zengchang Fan","doi":"10.1515/revac-2023-0062","DOIUrl":"https://doi.org/10.1515/revac-2023-0062","url":null,"abstract":"Abstract This study presents an in-depth review of non-dispersive infrared (NDIR) sensors for methane detection, focusing on their principles of operation, performance characteristics, advanced signal processing techniques, multi-gas detection capabilities, and applications in various industries. NDIR sensors offer significant advantages in methane sensing, including high sensitivity, selectivity, and long-term stability. The underlying principles of NDIR sensors involve measuring the absorption of infrared radiation by the target gas molecules, leading to precise and reliable methane concentration measurements. Advanced signal processing techniques, such as single-frequency filtering and wavelet filtering algorithms, have been explored to improve the performance of the sensor by reducing noise, enhancing the signal-to-noise ratio, and achieving more accurate results. In the context of multi-gas detection, NDIR sensors face challenges due to overlapping absorption spectra. However, various solutions, including narrow-band optical bandpass filters, gas filter correlation techniques, and machine learning algorithms, have been proposed to address these issues effectively. This study delves into specific applications of NDIR sensors in various industries, such as coal mines, wastewater treatment plants, and agriculture. In these settings, NDIR sensors have demonstrated their reliability, accuracy, and real-time monitoring capabilities, contributing to environmental protection, safety, and energy recovery. Furthermore, the anticipated future trends and developments in NDIR methane detection technology are explored, including increased miniaturization, integration with artificial intelligence, improvements in power efficiency, and the development of multi-gas NDIR sensors. These advancements are expected to further enhance the capabilities and widespread adoption of NDIR sensors in methane detection applications.","PeriodicalId":21090,"journal":{"name":"Reviews in Analytical Chemistry","volume":"25 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2023-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"134980954","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Abstract In recent years, there has been a significant increase in the application of green chemistry principles in analytical chemistry. One of the key factors affecting the environmental sustainability of analytical methods is the choice of solvent. In this particular study, a two-factor, three-level response surface design was employed to develop an environmentally friendly chromatographic technique for a mixture of metformin, glimepiride, and pioglitazone. Ethanol, which is known to be harmless to the environment, was chosen as the organic modifier in the mobile phase. The separation of the mixture was achieved using a phosphate buffer solution (pH 3) mixed with ethanol (30:70 v/v). The linearity of the developed method covered a concentration of metformin of 10–120 µg·mL −1 with a correlation coefficient of 0.9998, glimepiride of 0.1–20 µg·mL −1 with a correlation coefficient of 0.9997, and pioglitazone of 1–50 µg·mL −1 with a correlation coefficient of 0.9999. To evaluate the environmental friendliness of the developed method, two assessment tools were employed: The Analytical GREEnness metric and Green Analytical Procedure Index. The results revealed that the developed method performed exceptionally well in terms of its eco-friendliness. Furthermore, the developed method was compared to other reported methods in terms of both accuracy and environmental sustainability. The results demonstrated that the developed method serves as an excellent alternative to well-established techniques for the separation and quantification of the analyzed mixture. Overall, this study highlights the importance of integrating green chemistry principles into analytical chemistry practices.
{"title":"Eco-friendly HPLC method by using response surface design to measure a combination of three antidiabetic drugs","authors":"Naser F. Al-Tannak, Ahmed Hemdan","doi":"10.1515/revac-2023-0063","DOIUrl":"https://doi.org/10.1515/revac-2023-0063","url":null,"abstract":"Abstract In recent years, there has been a significant increase in the application of green chemistry principles in analytical chemistry. One of the key factors affecting the environmental sustainability of analytical methods is the choice of solvent. In this particular study, a two-factor, three-level response surface design was employed to develop an environmentally friendly chromatographic technique for a mixture of metformin, glimepiride, and pioglitazone. Ethanol, which is known to be harmless to the environment, was chosen as the organic modifier in the mobile phase. The separation of the mixture was achieved using a phosphate buffer solution (pH 3) mixed with ethanol (30:70 v/v). The linearity of the developed method covered a concentration of metformin of 10–120 µg·mL −1 with a correlation coefficient of 0.9998, glimepiride of 0.1–20 µg·mL −1 with a correlation coefficient of 0.9997, and pioglitazone of 1–50 µg·mL −1 with a correlation coefficient of 0.9999. To evaluate the environmental friendliness of the developed method, two assessment tools were employed: The Analytical GREEnness metric and Green Analytical Procedure Index. The results revealed that the developed method performed exceptionally well in terms of its eco-friendliness. Furthermore, the developed method was compared to other reported methods in terms of both accuracy and environmental sustainability. The results demonstrated that the developed method serves as an excellent alternative to well-established techniques for the separation and quantification of the analyzed mixture. Overall, this study highlights the importance of integrating green chemistry principles into analytical chemistry practices.","PeriodicalId":21090,"journal":{"name":"Reviews in Analytical Chemistry","volume":"273 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2023-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135508720","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Abstract Komagataella phaffii is an important cell factory for recombinant protein production under methanol induction. Tracking of recombinant protein expression by single K. phaffii cell is a hot topic to identify the variation of expression level in submerge cultivation system. In this study, a platform system harnessing Aspergillus niger pellets for K. phaffii cell immobilization in fabricated glass plate was developed to measure the green fluorescent protein (GFP) expression of single cell using fluorescence microscope. This system was optimized through pellets preparation, K. phaffii cell absorption, inducer comparison, methanol concentration, flow velocity of medium, and obtaining a successful platform to track GFP expression of single K. phaffii cell. This system provided an on-line analytical technology to discover the heterogeneous capability of various K. phaffii cells.
{"title":"Real-time monitoring of recombinant GFP expression in single-cell <i>Komagataella phaffii</i> through filamentous pelletization technology","authors":"Xiao Zheng, Wenjie Cong, Hualan Zhou, Jianguo Zhang","doi":"10.1515/revac-2023-0059","DOIUrl":"https://doi.org/10.1515/revac-2023-0059","url":null,"abstract":"Abstract Komagataella phaffii is an important cell factory for recombinant protein production under methanol induction. Tracking of recombinant protein expression by single K. phaffii cell is a hot topic to identify the variation of expression level in submerge cultivation system. In this study, a platform system harnessing Aspergillus niger pellets for K. phaffii cell immobilization in fabricated glass plate was developed to measure the green fluorescent protein (GFP) expression of single cell using fluorescence microscope. This system was optimized through pellets preparation, K. phaffii cell absorption, inducer comparison, methanol concentration, flow velocity of medium, and obtaining a successful platform to track GFP expression of single K. phaffii cell. This system provided an on-line analytical technology to discover the heterogeneous capability of various K. phaffii cells.","PeriodicalId":21090,"journal":{"name":"Reviews in Analytical Chemistry","volume":"10 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2023-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"136258919","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Abstract Apixaban (APX) is a novel anticoagulant drug used in the treatment of ischemic stroke and venous thromboembolism. In this study, two different chromatographic methods were developed for the determination of APX in pharmaceutical products. In the first method, an Agilent C18 column (250 mm × 4.6 mm, 5 μm) was used, and the temperature was kept constant at 30°C. The mobile phase was chosen to be 0.1% trifluoroacetic acid solution and acetonitrile (65:35, v/v), and isocratic elution was applied. The flow rate of the mobile phase was found to be 1.0 mL·min−1 and the injection volume was 20 µL. The detection was carried out at a wavelength of 276 nm using a UV detector. In the second method, ethanol was used as an organic modifier. The only difference between these methods was the organic modifier. All other conditions of the methods were the same. Both chromatographic methods were validated in accordance with ICH guidelines for various parameters such as selectivity, linearity, accuracy, precision, detection and quantification limit, and robustness. The determination coefficients of chromatographic methods were greater than 0.999 in the concentration range of 5–30 mg·mL−1 of APX. Later, these chromatographic methods were applied to tablet formulations. Comparison of the obtained results in terms of mean was made using Student’s (t) test, and comparisons in terms of standard deviations were made using the Fisher (F) test. It was observed that there was no significant difference between these methods. These two methods were then evaluated using AGREE-Analytical greenness metric software. The chromatographic method using ethanol as an organic modifier has been proposed as an excellent eco-friendly and analyst-friendly alternative for the determination of APX in pharmaceutical formulations. Graphical abstract
阿哌沙班(apxaban, APX)是一种用于治疗缺血性脑卒中和静脉血栓栓塞的新型抗凝药物。本文建立了两种不同的色谱法测定药品中APX的方法。第一种方法采用Agilent C18色谱柱(250 mm × 4.6 mm, 5 μm)，温度为30℃。流动相为0.1%三氟乙酸溶液-乙腈(65:35,v/v)，等密度洗脱。流动相流速为1.0 mL·min−1，进样量为20µL。用紫外检测器在276 nm波长下进行检测。在第二种方法中，乙醇作为有机改性剂。这些方法之间的唯一区别是有机改性剂。所有方法的其他条件相同。根据ICH指南对两种色谱方法进行了各种参数的验证，如选择性、线性、准确度、精密度、检测和定量限以及鲁棒性。在APX 5 ~ 30 mg·mL−1的浓度范围内，色谱法测定系数均大于0.999，可用于片剂配方的分析。所得结果的均值比较采用Student’s (t)检验，标准差比较采用Fisher (F)检验。结果表明，两种方法间无显著性差异。然后使用AGREE-Analytical绿色度量软件对这两种方法进行评估。以乙醇为有机改性剂的色谱法是测定制剂中APX的一种环境友好、分析人员友好的方法。图形抽象
{"title":"A green HPLC method for the determination of apixaban in pharmaceutical products: Development and validation","authors":"Erten Akbel, I. Bulduk, Süleyman Gökçe","doi":"10.1515/revac-2023-0058","DOIUrl":"https://doi.org/10.1515/revac-2023-0058","url":null,"abstract":"Abstract Apixaban (APX) is a novel anticoagulant drug used in the treatment of ischemic stroke and venous thromboembolism. In this study, two different chromatographic methods were developed for the determination of APX in pharmaceutical products. In the first method, an Agilent C18 column (250 mm × 4.6 mm, 5 μm) was used, and the temperature was kept constant at 30°C. The mobile phase was chosen to be 0.1% trifluoroacetic acid solution and acetonitrile (65:35, v/v), and isocratic elution was applied. The flow rate of the mobile phase was found to be 1.0 mL·min−1 and the injection volume was 20 µL. The detection was carried out at a wavelength of 276 nm using a UV detector. In the second method, ethanol was used as an organic modifier. The only difference between these methods was the organic modifier. All other conditions of the methods were the same. Both chromatographic methods were validated in accordance with ICH guidelines for various parameters such as selectivity, linearity, accuracy, precision, detection and quantification limit, and robustness. The determination coefficients of chromatographic methods were greater than 0.999 in the concentration range of 5–30 mg·mL−1 of APX. Later, these chromatographic methods were applied to tablet formulations. Comparison of the obtained results in terms of mean was made using Student’s (t) test, and comparisons in terms of standard deviations were made using the Fisher (F) test. It was observed that there was no significant difference between these methods. These two methods were then evaluated using AGREE-Analytical greenness metric software. The chromatographic method using ethanol as an organic modifier has been proposed as an excellent eco-friendly and analyst-friendly alternative for the determination of APX in pharmaceutical formulations. Graphical abstract","PeriodicalId":21090,"journal":{"name":"Reviews in Analytical Chemistry","volume":"43 1","pages":""},"PeriodicalIF":4.3,"publicationDate":"2023-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"90391980","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Miranda F. Kamal, Mona M. Abdel Moneim, Mohamed M. A. Hamdy
Abstract Green assessment of analytical procedures has become an environmental obligation in equivalence to their International Council of Harmonization analytical validation obligation. Worldwide awareness of our planet and ecological hazards have raised the shades of green and sustainable chemistry in pure or formulated API assays. The Green Analytical Procedure Index (GAPI) is instant five pentagrams for evaluating the greenness of each step in the developed analytical procedure, in discriminative colors: green, yellow, and red. In the present study, GAPI is applied to assess three novel direct analytical methods: spectrophotometric, fluorimetric, and high-performance thin-layer chromatography (HPTLC) for remdesivir (RDV) quantitation, both in bulk and pharmaceutical vials. Furthermore, a comparative green level calculated GAPI study has been assembled for the proposed methods versus the previously reported methods, for RDV assay, of similar techniques. Spectrophotometric direct A max method at 240 nm, fluorimetric emission at 404 nm upon excitation at 275 nm as well as the HPTLC densitometric measurement using ethanol and distilled water (7:3, v/v) as mobile phase, all three methodologies are developed, optimized, and fully validated for RDV quantitation. They have been applied to assay RDV pharmaceutical vials and results are compared together with a one-way ANOVA test. Satisfactory recoveries and nano-level sensitivities in addition to the least standard deviations encourage the use of developed methods for routine analysis in quality control laboratories. Their promising greenness profile satisfies the beliefs of ecological sustainability of Green Agenda 2030.
{"title":"Green novel photometric and planar chromatographic assays of remdesivir: Comparative greenness assessment study using estimated GAPI tool versus ISO technical reported methods","authors":"Miranda F. Kamal, Mona M. Abdel Moneim, Mohamed M. A. Hamdy","doi":"10.1515/revac-2023-0060","DOIUrl":"https://doi.org/10.1515/revac-2023-0060","url":null,"abstract":"Abstract Green assessment of analytical procedures has become an environmental obligation in equivalence to their International Council of Harmonization analytical validation obligation. Worldwide awareness of our planet and ecological hazards have raised the shades of green and sustainable chemistry in pure or formulated API assays. The Green Analytical Procedure Index (GAPI) is instant five pentagrams for evaluating the greenness of each step in the developed analytical procedure, in discriminative colors: green, yellow, and red. In the present study, GAPI is applied to assess three novel direct analytical methods: spectrophotometric, fluorimetric, and high-performance thin-layer chromatography (HPTLC) for remdesivir (RDV) quantitation, both in bulk and pharmaceutical vials. Furthermore, a comparative green level calculated GAPI study has been assembled for the proposed methods versus the previously reported methods, for RDV assay, of similar techniques. Spectrophotometric direct A max method at 240 nm, fluorimetric emission at 404 nm upon excitation at 275 nm as well as the HPTLC densitometric measurement using ethanol and distilled water (7:3, v/v) as mobile phase, all three methodologies are developed, optimized, and fully validated for RDV quantitation. They have been applied to assay RDV pharmaceutical vials and results are compared together with a one-way ANOVA test. Satisfactory recoveries and nano-level sensitivities in addition to the least standard deviations encourage the use of developed methods for routine analysis in quality control laboratories. Their promising greenness profile satisfies the beliefs of ecological sustainability of Green Agenda 2030.","PeriodicalId":21090,"journal":{"name":"Reviews in Analytical Chemistry","volume":"28 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2023-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135311306","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
E. Deconinck, Céline Duchateau, Margot Balcaen, L. Gremeaux, P. Courselle
Abstract Spectroscopic techniques such as infrared spectroscopy and Raman spectroscopy are used for a long time in the context of the analysis of illicit drugs, and their use is increasing due to the development of more performant portable devices and easy application in the context of harm reduction through drug checking or onsite forensic analysis. Although these instruments are routinely used with a spectral library, the importance of chemometric techniques to extract relevant information and give a full characterisation of samples, especially in the context of adulteration, is increasing. This review gives an overview of the applications described in the context of the analysis of illicit drug products exploiting the advantages of the combination of spectroscopy with chemometrics. Next to an overview of the literature, the review also tries to emphasize the shortcomings of the presented research papers and to give an incentive to what is needed to include chemometrics as a part of the daily routine of drug checking services and mobile forensic applications.
{"title":"Chemometrics and infrared spectroscopy – A winning team for the analysis of illicit drug products","authors":"E. Deconinck, Céline Duchateau, Margot Balcaen, L. Gremeaux, P. Courselle","doi":"10.1515/revac-2022-0046","DOIUrl":"https://doi.org/10.1515/revac-2022-0046","url":null,"abstract":"Abstract Spectroscopic techniques such as infrared spectroscopy and Raman spectroscopy are used for a long time in the context of the analysis of illicit drugs, and their use is increasing due to the development of more performant portable devices and easy application in the context of harm reduction through drug checking or onsite forensic analysis. Although these instruments are routinely used with a spectral library, the importance of chemometric techniques to extract relevant information and give a full characterisation of samples, especially in the context of adulteration, is increasing. This review gives an overview of the applications described in the context of the analysis of illicit drug products exploiting the advantages of the combination of spectroscopy with chemometrics. Next to an overview of the literature, the review also tries to emphasize the shortcomings of the presented research papers and to give an incentive to what is needed to include chemometrics as a part of the daily routine of drug checking services and mobile forensic applications.","PeriodicalId":21090,"journal":{"name":"Reviews in Analytical Chemistry","volume":"119 1","pages":"228 - 255"},"PeriodicalIF":4.3,"publicationDate":"2022-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"78400059","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"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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