Pub Date : 2024-06-24DOI: 10.2174/0115734129303749240607083542
Dhanya B. Sen, Krunal Baldha, Ashim Kumar Sen, Rajesh A. Maheshwari, Aarti S. Zanwar, K. P. Greeshma, Prasanna Kumar Pradhan
Background: A combination of fixed-doses containing 0.5 mg lobeglitazone sulfate and 1000 mg metformin hydrochloride has demonstrated efficacy in enhancing glycemic control in diabetes. Aim: The projected work aimed to establish and validate a high-performance thin-layer chromatographic methodology for the quantification of both drugs in tablet formulations. Objective: The task involves creating and validating a method in accordance with ICH guidelines to quantify two particular drugs in tablet formulations accurately. Methods: The high-performance thin-layer chromatographic analysis utilized aluminum plates layered with silica gel 60F254, and the solvent system consisted of acetonitrile, 1 M ammonium acetate (methanol), toluene, and triethyl amine (1.5:2.5:4:0.2 v/v/v/v), followed by densitometric scanning at 237 nm. Results: The methodology exhibited linearity in the range of 100-1500 ng/band for lobeglitazone sulfate and 1000-15000 ng/band for metformin hydrochloride, with correlation coefficients of 0.9991 and 0.9992, correspondingly. Exceptional sensitivity was observed, with detection limits of 8.17 ng/band for lobeglitazone sulfate and 271.34 ng/band for metformin hydrochloride, along with quantification limits of 24.75 ng/band for lobeglitazone sulfate and 822.24 ng/band for metformin hydrochloride. The method demonstrated precision (% relative standard deviation of peak area <360;2) and accuracy (recovery between 96 and 103%). Conclusion: The suggested methodology is fit for the concurrent quantification of both drugs in tablet formulations, making it applicable for routine quality control assessments in laboratories.
{"title":"Synchronized Assessment of Lobeglitazone Sulfate and Metformin Hydrochloride in Tablet by Robust, High-performance Thin-layer Chromatographic Method","authors":"Dhanya B. Sen, Krunal Baldha, Ashim Kumar Sen, Rajesh A. Maheshwari, Aarti S. Zanwar, K. P. Greeshma, Prasanna Kumar Pradhan","doi":"10.2174/0115734129303749240607083542","DOIUrl":"https://doi.org/10.2174/0115734129303749240607083542","url":null,"abstract":"Background: A combination of fixed-doses containing 0.5 mg lobeglitazone sulfate and 1000 mg metformin hydrochloride has demonstrated efficacy in enhancing glycemic control in diabetes. Aim: The projected work aimed to establish and validate a high-performance thin-layer chromatographic methodology for the quantification of both drugs in tablet formulations. Objective: The task involves creating and validating a method in accordance with ICH guidelines to quantify two particular drugs in tablet formulations accurately. Methods: The high-performance thin-layer chromatographic analysis utilized aluminum plates layered with silica gel 60F254, and the solvent system consisted of acetonitrile, 1 M ammonium acetate (methanol), toluene, and triethyl amine (1.5:2.5:4:0.2 v/v/v/v), followed by densitometric scanning at 237 nm. Results: The methodology exhibited linearity in the range of 100-1500 ng/band for lobeglitazone sulfate and 1000-15000 ng/band for metformin hydrochloride, with correlation coefficients of 0.9991 and 0.9992, correspondingly. Exceptional sensitivity was observed, with detection limits of 8.17 ng/band for lobeglitazone sulfate and 271.34 ng/band for metformin hydrochloride, along with quantification limits of 24.75 ng/band for lobeglitazone sulfate and 822.24 ng/band for metformin hydrochloride. The method demonstrated precision (% relative standard deviation of peak area <360;2) and accuracy (recovery between 96 and 103%). Conclusion: The suggested methodology is fit for the concurrent quantification of both drugs in tablet formulations, making it applicable for routine quality control assessments in laboratories.","PeriodicalId":10889,"journal":{"name":"Current Pharmaceutical Analysis","volume":"95 1","pages":""},"PeriodicalIF":0.6,"publicationDate":"2024-06-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141509527","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-05-06DOI: 10.2174/0115734129295505240430092112
Mario Theodore, Vorasit Vongsutilers
Objective: The objective of this study is to develop and validate a routine screening test for the determination of three common antipyretic-analgesic synthetic drugs (paracetamol, ibuprofen, and aspirin) adulteration in herbal products using Attenuated Total Reflectance Fourier Transform Infrared (ATR-FTIR) coupled with chemometric method. Method: ATR-FTIR spectra of sixteen testing sets of herbal product samples for pain and fever indications were used for multivariate chemometrics model construction. Linear Discriminant Analysis (LDA) was selected as a method for model construction with IBM SPSS for statistical analysis. Model development employed feature selection, such as the stepwise method for variable selection. The model with a high %correct classification and cross-validation was selected and was then validated with an independent testing data set with an auto-prediction test, confusion matrix, and Receiver Operating Characteristic (ROC) curve. To validate the developed test for routine use, the result from ATR-FTIR method was compared with the standard HPLC and TLC analyses used for adulteration screening. objective: Creating validated screening tools for herbal products adulterated with three common antipyretic-analgesic synthetic drugs (Paracetamol, Ibuprofen, and Aspirin) using ATR-FTIR couple with chemometric method Results: The selected model's overall %correct classification result was 97.7%, with a cross-validation of 93.8% rate in training set samples. External validation with an independent testing dataset gave an overall correct classification of 93.8%, with an area under the curve of ROC at 0.979. Comparative testing revealed that model performance was comparable with the HPLC and TLC methods, which routinely detect the presence of paracetamol, aspirin, and ibuprofen. The results of testing set samples classification were consistent with training set samples. Conclusion: Against the standard chromatographic methods, the multivariate chemometric model based on ATR-FTIR demonstrates comparable detection capability to determine adulteration of paracetamol, ibuprofen, and aspirin in herbal products.
{"title":"Development of Attenuated Total Reflectance Fourier Transform Infrared Spectroscopy Coupled with Multivariate Classification Chemometric Model for Routine Screening of Paracetamol, Ibuprofen, and Aspirin Adulteration in Herbal Products","authors":"Mario Theodore, Vorasit Vongsutilers","doi":"10.2174/0115734129295505240430092112","DOIUrl":"https://doi.org/10.2174/0115734129295505240430092112","url":null,"abstract":"Objective: The objective of this study is to develop and validate a routine screening test for the determination of three common antipyretic-analgesic synthetic drugs (paracetamol, ibuprofen, and aspirin) adulteration in herbal products using Attenuated Total Reflectance Fourier Transform Infrared (ATR-FTIR) coupled with chemometric method. Method: ATR-FTIR spectra of sixteen testing sets of herbal product samples for pain and fever indications were used for multivariate chemometrics model construction. Linear Discriminant Analysis (LDA) was selected as a method for model construction with IBM SPSS for statistical analysis. Model development employed feature selection, such as the stepwise method for variable selection. The model with a high %correct classification and cross-validation was selected and was then validated with an independent testing data set with an auto-prediction test, confusion matrix, and Receiver Operating Characteristic (ROC) curve. To validate the developed test for routine use, the result from ATR-FTIR method was compared with the standard HPLC and TLC analyses used for adulteration screening. objective: Creating validated screening tools for herbal products adulterated with three common antipyretic-analgesic synthetic drugs (Paracetamol, Ibuprofen, and Aspirin) using ATR-FTIR couple with chemometric method Results: The selected model's overall %correct classification result was 97.7%, with a cross-validation of 93.8% rate in training set samples. External validation with an independent testing dataset gave an overall correct classification of 93.8%, with an area under the curve of ROC at 0.979. Comparative testing revealed that model performance was comparable with the HPLC and TLC methods, which routinely detect the presence of paracetamol, aspirin, and ibuprofen. The results of testing set samples classification were consistent with training set samples. Conclusion: Against the standard chromatographic methods, the multivariate chemometric model based on ATR-FTIR demonstrates comparable detection capability to determine adulteration of paracetamol, ibuprofen, and aspirin in herbal products.","PeriodicalId":10889,"journal":{"name":"Current Pharmaceutical Analysis","volume":"16 1","pages":""},"PeriodicalIF":0.6,"publicationDate":"2024-05-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140885047","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Background: The screening of active ingredients in traditional Chinese medicine is an important task in the modernization of traditional Chinese medicine, and the commonly used analytical means in the past were mainly to screen the extracts of traditional Chinese medicine through pharmacological experiments, but the method has major defects. The target fishing strategy provides a new idea for the screening of active ingredients, and it has rapidly become a hot research direction, but there are many methods that need to be summarized and aggregated. Objective: It aims to provide readers with an understanding of the achievements, developments, and dilemmas of target fishing techniques over the past few years and to provide new ideas for subsequent research. Methods: Research articles in recent years using target fishing as an entry point are used as a basis to summarize the types of literature based on their principles and characteristics and to discuss the advantages and disadvantages of each method. Conclusion: This paper summarizes the classification and development of fishing techniques such as ultrafiltration, equilibrium dialysis, cell membrane chromatography, and immobilization of target molecules and target fishing and describes the principles and characteristics of these methods. The applications of these methods in the active ingredients of traditional Chinese medicine are summarized, and the problems and solutions of these methods are discussed.
{"title":"Application and Development of Targeted Fishing Technology in Natural Product Screening - A Simple Minireview","authors":"Yingying Su, Weiping Wang, Ying Wang, Chen Wang, Shuai Sun, Xianhong Zhu, Xiao Dai, Shiyu Li, Xun Gao, Kunming Qin","doi":"10.2174/0115734129301241240429114323","DOIUrl":"https://doi.org/10.2174/0115734129301241240429114323","url":null,"abstract":"Background: The screening of active ingredients in traditional Chinese medicine is an important task in the modernization of traditional Chinese medicine, and the commonly used analytical means in the past were mainly to screen the extracts of traditional Chinese medicine through pharmacological experiments, but the method has major defects. The target fishing strategy provides a new idea for the screening of active ingredients, and it has rapidly become a hot research direction, but there are many methods that need to be summarized and aggregated. Objective: It aims to provide readers with an understanding of the achievements, developments, and dilemmas of target fishing techniques over the past few years and to provide new ideas for subsequent research. Methods: Research articles in recent years using target fishing as an entry point are used as a basis to summarize the types of literature based on their principles and characteristics and to discuss the advantages and disadvantages of each method. Conclusion: This paper summarizes the classification and development of fishing techniques such as ultrafiltration, equilibrium dialysis, cell membrane chromatography, and immobilization of target molecules and target fishing and describes the principles and characteristics of these methods. The applications of these methods in the active ingredients of traditional Chinese medicine are summarized, and the problems and solutions of these methods are discussed.","PeriodicalId":10889,"journal":{"name":"Current Pharmaceutical Analysis","volume":"12 1","pages":""},"PeriodicalIF":0.6,"publicationDate":"2024-05-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140889912","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-05-06DOI: 10.2174/0115734129307329240430071035
Bharat Sharma, Rohit Bhatia, Subrahmanya S. Ganti, Naresh Kumar Rangra
: Alkaloids provide significant health benefits in moderation, but excessive levels can pose health hazards. They play an important role in the creation of numerous pharmacological medications, acting as potent antispasmodics, analgesics, and even anti-cancer medicines. A detailed review of sensitive and accurate alkaloid analytical techniques can be used as a guide for future analyses of alkaloids in pertinent research. The main aim of this manuscript is to review the literature on the detection and separation of alkaloids by using various methods like analytical, bioanalytical, and electrochemical techniques, published during 2018-2023. An in-depth review of the literature was carried out using a variety of databases, including Web of Knowledge, PubMed, and Google Scholar. Consulting relevant published materials, including books, was another aspect of this research. The keywords used in the search were alkaloids, analytical techniques, bio-analytical techniques, electrochemical techniques, and biosensors. These were carefully examined in more detail, and significant data and findings were collected and presented using tables. The publication highlights the significance of advanced chromatographic techniques in the separation and isolation of alkaloids. It discusses several analytical, bio-analytical, and electrochemical analytical techniques, which include sensors and biosensors, and adds to the extensive review of alkaloid detection techniques. Recent advancements and methodologies for improving the knowledge of the detection and separation of alkaloids are presented in this article, which is beneficial for the researcher involved in developing analytical methods for alkaloid detection. Current efforts and advanced analytical approaches for alkaloid detection are given in this manuscript, which is crucial in favor of improving the health and wellness of society.
:适量的生物碱对健康大有裨益，但过量则会危害健康。生物碱在许多药理药物的制造过程中发挥着重要作用，可作为强效解痉药、镇痛药甚至抗癌药。对灵敏、准确的生物碱分析技术进行详细综述，可为今后相关研究中的生物碱分析提供指导。本手稿的主要目的是综述 2018-2023 年间发表的关于使用分析、生物分析和电化学技术等各种方法检测和分离生物碱的文献。利用 Web of Knowledge、PubMed 和 Google Scholar 等多种数据库对文献进行了深入查阅。查阅相关出版资料（包括书籍）是本研究的另一个方面。搜索中使用的关键词是生物碱、分析技术、生物分析技术、电化学技术和生物传感器。研究人员对这些关键词进行了仔细研究，收集了重要数据和发现，并用表格进行了介绍。该出版物强调了先进色谱技术在分离生物碱方面的重要意义。它讨论了几种分析、生物分析和电化学分析技术，其中包括传感器和生物传感器，并增加了对生物碱检测技术的广泛评论。本文介绍了在提高生物碱检测和分离知识方面的最新进展和方法，对参与开发生物碱检测分析方法的研究人员大有裨益。本手稿介绍了生物碱检测的当前工作和先进分析方法，这对改善社会健康和福祉至关重要。
{"title":"Recent Trends in the Detection of Alkaloids through Analytical, Bioanalytical, and Electrochemical Techniques : Analytical Techniques Used in Detection of Alkaloids","authors":"Bharat Sharma, Rohit Bhatia, Subrahmanya S. Ganti, Naresh Kumar Rangra","doi":"10.2174/0115734129307329240430071035","DOIUrl":"https://doi.org/10.2174/0115734129307329240430071035","url":null,"abstract":": Alkaloids provide significant health benefits in moderation, but excessive levels can pose health hazards. They play an important role in the creation of numerous pharmacological medications, acting as potent antispasmodics, analgesics, and even anti-cancer medicines. A detailed review of sensitive and accurate alkaloid analytical techniques can be used as a guide for future analyses of alkaloids in pertinent research. The main aim of this manuscript is to review the literature on the detection and separation of alkaloids by using various methods like analytical, bioanalytical, and electrochemical techniques, published during 2018-2023. An in-depth review of the literature was carried out using a variety of databases, including Web of Knowledge, PubMed, and Google Scholar. Consulting relevant published materials, including books, was another aspect of this research. The keywords used in the search were alkaloids, analytical techniques, bio-analytical techniques, electrochemical techniques, and biosensors. These were carefully examined in more detail, and significant data and findings were collected and presented using tables. The publication highlights the significance of advanced chromatographic techniques in the separation and isolation of alkaloids. It discusses several analytical, bio-analytical, and electrochemical analytical techniques, which include sensors and biosensors, and adds to the extensive review of alkaloid detection techniques. Recent advancements and methodologies for improving the knowledge of the detection and separation of alkaloids are presented in this article, which is beneficial for the researcher involved in developing analytical methods for alkaloid detection. Current efforts and advanced analytical approaches for alkaloid detection are given in this manuscript, which is crucial in favor of improving the health and wellness of society.","PeriodicalId":10889,"journal":{"name":"Current Pharmaceutical Analysis","volume":"25 1","pages":""},"PeriodicalIF":0.6,"publicationDate":"2024-05-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140889654","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-05-02DOI: 10.2174/0115734129282400240417115747
Siwen Wang, Mingyu Cui, Fan Wu, Chao Yu, Yue Sui, Xueying Yan, Yingli Gai
Background and Objective: Rivaroxaban, a direct oral anticoagulant, has become the first-line therapy medicine to prevent and treat Venous Thromboembolism (VTE). Patients with femoropopliteal venous thrombosis may use rivaroxaban along with diosmin. Rivaroxaban is the substrate of CYP3A4 and P-glycoprotein (P-gp), but diosmin is the inhibitor. The combination might lead to Drug-drug Interaction (DDI). The aim of this study was to assess the effect of diosmin on the pharmacokinetics and pharmacodynamics of rivaroxaban in rats. Methods: Plasma concentration of rivaroxaban in the absence or presence of diosmin groups was determined by High-performance Liquid Chromatography (HPLC). Pharmacokinetics parameters were calculated and used to evaluate pharmacokinetics interactions. Anticoagulation was investigated by Prothrombin Time (PT), International Normalized Ratio (INR), and Activated Partial Thromboplastin Time (APTT). Antithrombotic efficacy was investigated by the length of tail thrombosis, the content levels of Interleukin-1β (IL-1β) and D-dimer (D-D) in rats, and histopathological sections in the tail thrombosis model. Results: Maximum concentration (Cmax), 0-t Area Under the Curve (AUC0–t), 0-∞ Area Under the Curve (AUC0–∞) of rivaroxaban increased significantly in the combination group. PT, INR, and APPT in the combination group exhibited an increase compared to the Rivaroxaban group. Simultaneously, the length of tail thrombosis and levels of IL-1β and D-D were significantly reduced. Significant improvement of tissue histology in tail thrombosis could be observed. Conclusion: Taken together, diosmin could significantly affect the pharmacokinetics and pharmacodynamics of rivaroxaban, and enhance anticoagulant and antithrombotic efficacy in rats. More attention should be paid to avoid harmful DDI in the clinic.
{"title":"Effect of Diosmin on Pharmacokinetics and Pharmacodynamics of Rivaroxaban in Rats","authors":"Siwen Wang, Mingyu Cui, Fan Wu, Chao Yu, Yue Sui, Xueying Yan, Yingli Gai","doi":"10.2174/0115734129282400240417115747","DOIUrl":"https://doi.org/10.2174/0115734129282400240417115747","url":null,"abstract":"Background and Objective: Rivaroxaban, a direct oral anticoagulant, has become the first-line therapy medicine to prevent and treat Venous Thromboembolism (VTE). Patients with femoropopliteal venous thrombosis may use rivaroxaban along with diosmin. Rivaroxaban is the substrate of CYP3A4 and P-glycoprotein (P-gp), but diosmin is the inhibitor. The combination might lead to Drug-drug Interaction (DDI). The aim of this study was to assess the effect of diosmin on the pharmacokinetics and pharmacodynamics of rivaroxaban in rats. Methods: Plasma concentration of rivaroxaban in the absence or presence of diosmin groups was determined by High-performance Liquid Chromatography (HPLC). Pharmacokinetics parameters were calculated and used to evaluate pharmacokinetics interactions. Anticoagulation was investigated by Prothrombin Time (PT), International Normalized Ratio (INR), and Activated Partial Thromboplastin Time (APTT). Antithrombotic efficacy was investigated by the length of tail thrombosis, the content levels of Interleukin-1β (IL-1β) and D-dimer (D-D) in rats, and histopathological sections in the tail thrombosis model. Results: Maximum concentration (Cmax), 0-t Area Under the Curve (AUC0–t), 0-∞ Area Under the Curve (AUC0–∞) of rivaroxaban increased significantly in the combination group. PT, INR, and APPT in the combination group exhibited an increase compared to the Rivaroxaban group. Simultaneously, the length of tail thrombosis and levels of IL-1β and D-D were significantly reduced. Significant improvement of tissue histology in tail thrombosis could be observed. Conclusion: Taken together, diosmin could significantly affect the pharmacokinetics and pharmacodynamics of rivaroxaban, and enhance anticoagulant and antithrombotic efficacy in rats. More attention should be paid to avoid harmful DDI in the clinic.","PeriodicalId":10889,"journal":{"name":"Current Pharmaceutical Analysis","volume":"87 1","pages":""},"PeriodicalIF":0.6,"publicationDate":"2024-05-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140838907","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Background:: Antiviral drugs can cure more than 95 percent of people with hepatitis C, but the inaccessibility of quality affordable medicines and the lack of their uninterrupted supply pose a major challenge. Impurities in drugs have a significant impact on their quality and are one of the substantial causes of drug recalls, ultimately leading to the unavailability of the drug in the market. Hence, there is a need for a robust, quality risk management and quality by design-driven analytical method that can detect the antiviral drug, Daclatasvir dihydrochloride, in the presence of its probable impurities. Objective:: This study aimed to develop a Quality by Design-driven stability- indicating liquid chromatography method for Daclatasvir dihydrochloride and the characterization of its putative degradants by LC-MS. Method:: The fishbone diagram and quality risk assessment investigated twenty-four process parameters and concluded that three risk parameters, i.e., flow rate, buffer pH, and stationary phase type, were the critical process parameters. The critical quality attributes viz. resolution between impurity 6 and DCV and impurity 2 & 3 (Rs˃1.5), the shape of the peak of DCV which is decided by the Number of Theoretical Plates (NTP˃5000), and the retention time of Daclatasvir (tR14-23 mins) were optimized using a two-level three-factor full factorial design with five center points. Results:: The optimized method is stability-indicating in its true sense as it can separate the sample with its degradants generated in basic (three), acidic (two), oxidative (H2O2: three, Azobisisobutyronitrile: one), photo (three), and dry heat (one) conditions. Degradants structures were elucidated, and degradation routes were established, using LC-MS and LC-MS/MS analyses. Conclusion:: The drug is highly susceptible to acid, base hydrolysis, and oxidation degradation conditions and poses a significant risk to the analytical method to fail in system suitability criteria. Hence, a robust and flexible chromatographic method with the capacity for continuous improvement was developed and successfully validated within the criteria of design space.
{"title":"Quality by Design-driven Analytical Method: A Quality Risk Management-Based Liquid Chromatography Method for Daclatasvir and Characterization of its Putative Degradants by LC-MS/MS","authors":"Prashant Chaturvedi, Shruti Chopra, Kalyani Joshi, Savita Tauro","doi":"10.2174/0115734129285465240408044841","DOIUrl":"https://doi.org/10.2174/0115734129285465240408044841","url":null,"abstract":"Background:: Antiviral drugs can cure more than 95 percent of people with hepatitis C, but the inaccessibility of quality affordable medicines and the lack of their uninterrupted supply pose a major challenge. Impurities in drugs have a significant impact on their quality and are one of the substantial causes of drug recalls, ultimately leading to the unavailability of the drug in the market. Hence, there is a need for a robust, quality risk management and quality by design-driven analytical method that can detect the antiviral drug, Daclatasvir dihydrochloride, in the presence of its probable impurities. Objective:: This study aimed to develop a Quality by Design-driven stability- indicating liquid chromatography method for Daclatasvir dihydrochloride and the characterization of its putative degradants by LC-MS. Method:: The fishbone diagram and quality risk assessment investigated twenty-four process parameters and concluded that three risk parameters, i.e., flow rate, buffer pH, and stationary phase type, were the critical process parameters. The critical quality attributes viz. resolution between impurity 6 and DCV and impurity 2 & 3 (Rs˃1.5), the shape of the peak of DCV which is decided by the Number of Theoretical Plates (NTP˃5000), and the retention time of Daclatasvir (tR14-23 mins) were optimized using a two-level three-factor full factorial design with five center points. Results:: The optimized method is stability-indicating in its true sense as it can separate the sample with its degradants generated in basic (three), acidic (two), oxidative (H2O2: three, Azobisisobutyronitrile: one), photo (three), and dry heat (one) conditions. Degradants structures were elucidated, and degradation routes were established, using LC-MS and LC-MS/MS analyses. Conclusion:: The drug is highly susceptible to acid, base hydrolysis, and oxidation degradation conditions and poses a significant risk to the analytical method to fail in system suitability criteria. Hence, a robust and flexible chromatographic method with the capacity for continuous improvement was developed and successfully validated within the criteria of design space.","PeriodicalId":10889,"journal":{"name":"Current Pharmaceutical Analysis","volume":"60 1","pages":""},"PeriodicalIF":0.6,"publicationDate":"2024-04-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140838757","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Background: The reverse-phase high-performance liquid chromatography (RP-HPLC) method was developed for the quantitative measurement of monoclonal antibodies (Maftivimab, Atoltivimab, and Odesivimab) in the pharmaceutical dosage form. The Food and Drug Administration (FDA) has approved these monoclonal antibodies for the treatment of Zaire ebolavirus infection in adults. Methods: Maftivimab, Atoltivimab, and Odesivimab were separated chromatographically on the Waters Alliance-e2695 platform using the Luna Phenyl Hexyl (250 x 4.6 mm, 5 μm) column and a mobile phase made up of Acetonitrile (ACN) and ortho-phosphoric acid (OPA) buffer in a ratio of 70:30 (v/v). Results: The flow rate was 1.0 ml/min, and a photodiode array (PDA) detector operating at room temperature was used to measure absorption at 282 nm. For Maftivimab, Atoltivimab, and Odesivimab, the theoretical plates were not less than 2000, and the tailing factor shouldn't be greater than 2, accordingly. All measurements have a constant relative standard deviation of peak areas that is less than 2.0. Conclusion: The suggested procedure was approved following the International Conference on Harmonisation (ICH) recommendations. When used for the quantitative analysis of Maftivimab, Atoltivimab, and Odesivimab, the approach was found to be straightforward, affordable, appropriate, exact, accurate, and robust.
{"title":"Rapid Development and Validation of Atoltivimab, Maftivimab and Odesivimab in Pharmaceutical Dosage form by using the RP-HPLC Method","authors":"Pallepogu Venkateswara Rao, Naidu Srinivasa Rao, Biswa Mohan Sahoo, Nayaka Raghavendra Babu","doi":"10.2174/0115734129300296240416070559","DOIUrl":"https://doi.org/10.2174/0115734129300296240416070559","url":null,"abstract":"Background: The reverse-phase high-performance liquid chromatography (RP-HPLC) method was developed for the quantitative measurement of monoclonal antibodies (Maftivimab, Atoltivimab, and Odesivimab) in the pharmaceutical dosage form. The Food and Drug Administration (FDA) has approved these monoclonal antibodies for the treatment of Zaire ebolavirus infection in adults. Methods: Maftivimab, Atoltivimab, and Odesivimab were separated chromatographically on the Waters Alliance-e2695 platform using the Luna Phenyl Hexyl (250 x 4.6 mm, 5 μm) column and a mobile phase made up of Acetonitrile (ACN) and ortho-phosphoric acid (OPA) buffer in a ratio of 70:30 (v/v). Results: The flow rate was 1.0 ml/min, and a photodiode array (PDA) detector operating at room temperature was used to measure absorption at 282 nm. For Maftivimab, Atoltivimab, and Odesivimab, the theoretical plates were not less than 2000, and the tailing factor shouldn't be greater than 2, accordingly. All measurements have a constant relative standard deviation of peak areas that is less than 2.0. Conclusion: The suggested procedure was approved following the International Conference on Harmonisation (ICH) recommendations. When used for the quantitative analysis of Maftivimab, Atoltivimab, and Odesivimab, the approach was found to be straightforward, affordable, appropriate, exact, accurate, and robust.","PeriodicalId":10889,"journal":{"name":"Current Pharmaceutical Analysis","volume":"106 1","pages":""},"PeriodicalIF":0.6,"publicationDate":"2024-04-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140811612","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Objective:: Ketamine, commonly known as “K-powder,” is increasingly being abused as a “prom drug.” Palmatine, a typical isoquinoline alkaloid, is mainly found in the roots and stems of natural Chinese herbal medicine plants such as Phellodendron chinense, Coptis chinensis, Sankezhen and Nantianzhu. Herein, we aim to establish a UHPLC-MS/MS method to determine ketamine and palmatine concentrations in rat plasma and investigate the pharmacokinetic interaction of ketamine and palmatine. Methods:: Three groups of eighteen rats each were assigned to ketamine, palmatine, ketamine and palmatine. The pharmacokinetic interaction between ketamine and palmatine was demonstrated using UHPLC-MS/MS. Results:: When ketamine was combined with palmatine, the mean residence time (MRT) was significantly different from that of the ketamine group. MRT decreased after combined use. The interaction showed that palmatine can influence the mean residence time of ketamine; no significant differences were observed for other pharmacokinetic parameters between the ketamine or palmatine group and the ketamine-palmatine group. Conclusion:: Palmatine may influence the mean residence time of ketamine.
{"title":"Determination of Ketamine and Palmatine in Rat Plasma by UHPLC-MS/ MS and their Pharmacokinetic Interaction","authors":"Xueli Huang, Yizhe Ma, Ziyue Wang, Wanhang Wang, Congcong Wen, Xianqin Wang, Meiling Zhang","doi":"10.2174/0115734129304769240403075839","DOIUrl":"https://doi.org/10.2174/0115734129304769240403075839","url":null,"abstract":"Objective:: Ketamine, commonly known as “K-powder,” is increasingly being abused as a “prom drug.” Palmatine, a typical isoquinoline alkaloid, is mainly found in the roots and stems of natural Chinese herbal medicine plants such as Phellodendron chinense, Coptis chinensis, Sankezhen and Nantianzhu. Herein, we aim to establish a UHPLC-MS/MS method to determine ketamine and palmatine concentrations in rat plasma and investigate the pharmacokinetic interaction of ketamine and palmatine. Methods:: Three groups of eighteen rats each were assigned to ketamine, palmatine, ketamine and palmatine. The pharmacokinetic interaction between ketamine and palmatine was demonstrated using UHPLC-MS/MS. Results:: When ketamine was combined with palmatine, the mean residence time (MRT) was significantly different from that of the ketamine group. MRT decreased after combined use. The interaction showed that palmatine can influence the mean residence time of ketamine; no significant differences were observed for other pharmacokinetic parameters between the ketamine or palmatine group and the ketamine-palmatine group. Conclusion:: Palmatine may influence the mean residence time of ketamine.","PeriodicalId":10889,"journal":{"name":"Current Pharmaceutical Analysis","volume":"207 1","pages":""},"PeriodicalIF":0.6,"publicationDate":"2024-04-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140593451","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
: Ultraviolet-Visible (UV-Vis) spectroscopy has emerged as a powerful analytical tool with diverse applications in pharmaceutical and bio-allied sciences. This article provides a comprehensive overview of the extensive utility of UV-Vis spectroscopy, emphasizing its pivotal role in characterizing and analyzing various compounds critical for drug development and bio-allied research. In the pharmaceutical sector, UV-Vis spectroscopy is a fundamental technique for quantifying the concentrations of active pharmaceutical ingredients (APIs) in formulations. Its non-destructive nature and high sensitivity make it an indispensable tool for quality control, ensuring the consistency and potency of pharmaceutical products. Furthermore, this technique has been employed in the study of drug-receptor interactions to elucidate the molecular mechanisms underlying therapeutic effects. In bio-allied applications, UV-Vis spectroscopy is used to analyze biomolecules like proteins, nucleic acids, and enzymes. This technique allows for the study of protein conformational changes, DNA structure, and enzymatic activity, offering crucial insights into fundamental biological processes. Additionally, UV-Vis spectroscopy aids in determining biomarker concentrations, assisting in the early diagnosis and monitoring of various diseases. This article also explores recent advancements in UV-Vis spectroscopy, including the integration of nanomaterials and computational approaches to enhance sensitivity and selectivity. Moreover, it discusses the potential of UV-Vis spectroscopy in emerging areas such as personalized medicine and point-of-care diagnostics. As technology continues to evolve, UV-Visible spectroscopy is poised to significantly contribute to the ever-expanding landscape of pharmaceutical and bio-related research.
{"title":"UV-Visible Spectroscopy: A Review on its Pharmaceutical and Bio-allied Sciences Applications","authors":"Abhinav Singhal, Urvashi Saini, Bhawna Chopra, Ashwani K. Dhingra, Akash Jain, Jasmine Chaudhary","doi":"10.2174/0115734129300562240408042614","DOIUrl":"https://doi.org/10.2174/0115734129300562240408042614","url":null,"abstract":": Ultraviolet-Visible (UV-Vis) spectroscopy has emerged as a powerful analytical tool with diverse applications in pharmaceutical and bio-allied sciences. This article provides a comprehensive overview of the extensive utility of UV-Vis spectroscopy, emphasizing its pivotal role in characterizing and analyzing various compounds critical for drug development and bio-allied research. In the pharmaceutical sector, UV-Vis spectroscopy is a fundamental technique for quantifying the concentrations of active pharmaceutical ingredients (APIs) in formulations. Its non-destructive nature and high sensitivity make it an indispensable tool for quality control, ensuring the consistency and potency of pharmaceutical products. Furthermore, this technique has been employed in the study of drug-receptor interactions to elucidate the molecular mechanisms underlying therapeutic effects. In bio-allied applications, UV-Vis spectroscopy is used to analyze biomolecules like proteins, nucleic acids, and enzymes. This technique allows for the study of protein conformational changes, DNA structure, and enzymatic activity, offering crucial insights into fundamental biological processes. Additionally, UV-Vis spectroscopy aids in determining biomarker concentrations, assisting in the early diagnosis and monitoring of various diseases. This article also explores recent advancements in UV-Vis spectroscopy, including the integration of nanomaterials and computational approaches to enhance sensitivity and selectivity. Moreover, it discusses the potential of UV-Vis spectroscopy in emerging areas such as personalized medicine and point-of-care diagnostics. As technology continues to evolve, UV-Visible spectroscopy is poised to significantly contribute to the ever-expanding landscape of pharmaceutical and bio-related research.","PeriodicalId":10889,"journal":{"name":"Current Pharmaceutical Analysis","volume":"57 1","pages":""},"PeriodicalIF":0.6,"publicationDate":"2024-04-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140593461","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-04-09DOI: 10.2174/0115734129293569240327093703
Ceylan Hepokur, Sema Misir, Mehmet Cicek, Solomon Habtemariam, Javad Sharifi-Rad
Background:: Salvia species known as "Sage" are among the important aromatic plants used in the world. This study, it was investigated the antioxidant capacity of Salvia cadmica and to investigate its protective effect on oxidative damage in t-BHP-induced fibroblast cells. Methods:: Antioxidant activity and phenolic characterization of the extract were evaluated using DPPH, TPC, TFC, FRAP, and HPLC, respectively.TAS, TOS, MDA and 8-oxo-guanine, CAT, SOD, and GPx values were examined using enzyme-linked immunosorbent assay (ELISA). The antiproliferative and apoptosis effects of Salvia cadmica ethanolic extract were determined using MTT assay and fluorescent probes in fibroblast cells. Results:: As a result of GC-MS analysis of Salvia cadmica ethanolic extract, carvacrol content was found to be high. The IC50 value of the DPPH antioxidant assay of the Salvia cadmica ethanolic extract was 80 ± 0.51 μg/mL. TPC, TFC, and FRAP values were found to be 18.25 ± 0.64 (mg gallic acid/g powder), 1.691±0.314 (mg quercetin /g powder), 31.5 ± 0.10 (mg Trolox/g powder), respectively. Total antioxidant and TOS values were found to be 0.383±0.033 (mmol Trolox Equ L-1), 16.31±0.71 (μmol H2O2 L-1) for 0.25 mg/mL, and 0.725±0.05 (mmol Trolox Equ L-1), 12.02 ±0.56 (μmol H2O2 L-1) for 0.5 mg/mL. In addition, while CAT and GPx significantly decreased enzyme activities, no significant change was observed in SOD enzyme activity. Ethanolic Salvia cadmica extract exhibited apoptotic features compared to only the t-BHP group. Conclusion:: These results suggest that Salvica cadmica extract works through a free radical mechanism.
{"title":"Protective Effect of Salvia cadmica on Fibroblast Cells from t-bhp-induced Oxidative Damage","authors":"Ceylan Hepokur, Sema Misir, Mehmet Cicek, Solomon Habtemariam, Javad Sharifi-Rad","doi":"10.2174/0115734129293569240327093703","DOIUrl":"https://doi.org/10.2174/0115734129293569240327093703","url":null,"abstract":"Background:: Salvia species known as \"Sage\" are among the important aromatic plants used in the world. This study, it was investigated the antioxidant capacity of Salvia cadmica and to investigate its protective effect on oxidative damage in t-BHP-induced fibroblast cells. Methods:: Antioxidant activity and phenolic characterization of the extract were evaluated using DPPH, TPC, TFC, FRAP, and HPLC, respectively.TAS, TOS, MDA and 8-oxo-guanine, CAT, SOD, and GPx values were examined using enzyme-linked immunosorbent assay (ELISA). The antiproliferative and apoptosis effects of Salvia cadmica ethanolic extract were determined using MTT assay and fluorescent probes in fibroblast cells. Results:: As a result of GC-MS analysis of Salvia cadmica ethanolic extract, carvacrol content was found to be high. The IC50 value of the DPPH antioxidant assay of the Salvia cadmica ethanolic extract was 80 ± 0.51 μg/mL. TPC, TFC, and FRAP values were found to be 18.25 ± 0.64 (mg gallic acid/g powder), 1.691±0.314 (mg quercetin /g powder), 31.5 ± 0.10 (mg Trolox/g powder), respectively. Total antioxidant and TOS values were found to be 0.383±0.033 (mmol Trolox Equ L-1), 16.31±0.71 (μmol H2O2 L-1) for 0.25 mg/mL, and 0.725±0.05 (mmol Trolox Equ L-1), 12.02 ±0.56 (μmol H2O2 L-1) for 0.5 mg/mL. In addition, while CAT and GPx significantly decreased enzyme activities, no significant change was observed in SOD enzyme activity. Ethanolic Salvia cadmica extract exhibited apoptotic features compared to only the t-BHP group. Conclusion:: These results suggest that Salvica cadmica extract works through a free radical mechanism.","PeriodicalId":10889,"journal":{"name":"Current Pharmaceutical Analysis","volume":"121 1","pages":""},"PeriodicalIF":0.6,"publicationDate":"2024-04-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140602916","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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