S. Jebali, Chaouki Belgacem, A. Labidi, Rafika Bensghaier, Haykel Galai, L. Latrous
A sensitive, precise, accurate, and green analytical HPLC–ESI–MS method for the quantification of delafloxacin and its degradation products in pharmaceutical dosage forms has been optimized and validated. The best separation was achieved with isocratic elution, the mobile phase is composed of a mixture of 0.1% trifluoroacetic acid in water and acetonitrile 65:35 (v/v), the flow rate is 0.5 mL min−1, and the column used is Kinetex Core‐Shell C18 (250 × 4.6 mm, 5 µm). Forced degradation studies were performed to prove that the method indicates stability. The pharmaceutical substance is prone to oxidative (H2O2 3%), acidic (HCl 0.1 M), and basic (0.1 M) conditions. Delafloxacin proved to be susceptible to acidic (HCl 0.1 M), basic (0.1 M), and oxidative (H2O2 3%) conditions. The proposition of the structures of degradation products has been based on the MS spectrum and the known reactivity of delafloxacin in the oxidative medium. The validation of the analytical method was carried out following the International Conference on Harmonization guidelines. The method was validated in terms of specificity, precision, linearity, and accuracy. The limits of detection and quantification of delafloxacin are, respectively, 0.005 and 0.017 µg mL−1.
{"title":"Sustainable and Stability Indicating Liquid Chromatography–Mass Spectrometry Method for the Quantitation of Delafloxacin in Pharmaceutical Formulations","authors":"S. Jebali, Chaouki Belgacem, A. Labidi, Rafika Bensghaier, Haykel Galai, L. Latrous","doi":"10.1002/sscp.202400083","DOIUrl":"https://doi.org/10.1002/sscp.202400083","url":null,"abstract":"A sensitive, precise, accurate, and green analytical HPLC–ESI–MS method for the quantification of delafloxacin and its degradation products in pharmaceutical dosage forms has been optimized and validated. The best separation was achieved with isocratic elution, the mobile phase is composed of a mixture of 0.1% trifluoroacetic acid in water and acetonitrile 65:35 (v/v), the flow rate is 0.5 mL min−1, and the column used is Kinetex Core‐Shell C18 (250 × 4.6 mm, 5 µm). Forced degradation studies were performed to prove that the method indicates stability. The pharmaceutical substance is prone to oxidative (H2O2 3%), acidic (HCl 0.1 M), and basic (0.1 M) conditions. Delafloxacin proved to be susceptible to acidic (HCl 0.1 M), basic (0.1 M), and oxidative (H2O2 3%) conditions. The proposition of the structures of degradation products has been based on the MS spectrum and the known reactivity of delafloxacin in the oxidative medium. The validation of the analytical method was carried out following the International Conference on Harmonization guidelines. The method was validated in terms of specificity, precision, linearity, and accuracy. The limits of detection and quantification of delafloxacin are, respectively, 0.005 and 0.017 µg mL−1.","PeriodicalId":508518,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-07-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141644800","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}
Poloxamer 188 is a commonly used excipient in formulations to protect products against mechanical stress and adsorption loss. In this work, an analytical method was developed to directly and accurately quantitate the amount of Poloxamer 188 in the drug substance of three different adeno‐associated virus (AAV) serotypes. The method is based on reversed‐phase liquid chromatography separation of virus particles from Poloxamer 188 using a charged aerosol detector and provides linearity from 5 to 200 ppm. A good assay precision and analyte recovery allows its adaptability to potentially various applications from process development support to AAV drug product release testing.
{"title":"Direct Quantitation of Poloxamer 188 in Adeno‐Associated Virus Products Using Reversed‐Phase Chromatography With Charged Aerosol Detection","authors":"Tai Nguyen, Zoran Sosic, Chong-Feng Xu","doi":"10.1002/sscp.202400045","DOIUrl":"https://doi.org/10.1002/sscp.202400045","url":null,"abstract":"Poloxamer 188 is a commonly used excipient in formulations to protect products against mechanical stress and adsorption loss. In this work, an analytical method was developed to directly and accurately quantitate the amount of Poloxamer 188 in the drug substance of three different adeno‐associated virus (AAV) serotypes. The method is based on reversed‐phase liquid chromatography separation of virus particles from Poloxamer 188 using a charged aerosol detector and provides linearity from 5 to 200 ppm. A good assay precision and analyte recovery allows its adaptability to potentially various applications from process development support to AAV drug product release testing.","PeriodicalId":508518,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-07-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141652790","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}
Polygalae Radix is a commonly used traditional Chinese medicine with multiple pharmacological activities. Modern research have revealed that saponins, xanthones, and oligosaccharide esters are its effective component groups. However, up to date the chemical substances in these effective component groups are still unclear, which has become a fundamental scientific issue needing to be addressed. In our study, an analysis strategy based on targeted tandem mass spectrometry (MS/MS) analysis was proposed to comprehensively identify the chemical substances in effective component groups. First, the extract of the Polygalae Radix was detected by ultra‐performance liquid chromatography coupled with electrospray ionization–orbitrap mass spectrometry in a full MS scan mode to minimize the losses of signals; second, the precursor ions of all compounds were extracted from the obtained full MS scan data using Compound Discoverer software; third, the interested precursor ions were locked based on their molecular features and constructed in a precursor ion list; finally, each precursor ion in the list was subjected to targeted MS/MS analysis for structure characterization. Using our analysis strategy, a total of 565 components were successfully identified.
{"title":"Comprehensive Identification of the Chemical Substances in Effective Component Groups of Polygalae Radix Based on Targeted Tandem Mass Spectrometry Analysis Strategy","authors":"Hongping Wang, Chunlan Fan, Ping Peng, Zijian Wang, Zhao-Zhou Lin, Shuwu Zhao","doi":"10.1002/sscp.202400026","DOIUrl":"https://doi.org/10.1002/sscp.202400026","url":null,"abstract":"Polygalae Radix is a commonly used traditional Chinese medicine with multiple pharmacological activities. Modern research have revealed that saponins, xanthones, and oligosaccharide esters are its effective component groups. However, up to date the chemical substances in these effective component groups are still unclear, which has become a fundamental scientific issue needing to be addressed. In our study, an analysis strategy based on targeted tandem mass spectrometry (MS/MS) analysis was proposed to comprehensively identify the chemical substances in effective component groups. First, the extract of the Polygalae Radix was detected by ultra‐performance liquid chromatography coupled with electrospray ionization–orbitrap mass spectrometry in a full MS scan mode to minimize the losses of signals; second, the precursor ions of all compounds were extracted from the obtained full MS scan data using Compound Discoverer software; third, the interested precursor ions were locked based on their molecular features and constructed in a precursor ion list; finally, each precursor ion in the list was subjected to targeted MS/MS analysis for structure characterization. Using our analysis strategy, a total of 565 components were successfully identified.","PeriodicalId":508518,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-07-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141663270","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}
Artemisiae Scopariae Herba (Chinese name Yinchen), the dried aerial part of Artemisia capillaris Thunb. (A. capillaris) or Artemisia scoparia Waldst. et Kit. (A. scoparia), is one of the most commonly used herbal drugs; the one harvested in the spring is habitually named “Mian Yinchen,” and the one harvested in the autumn is habitually named “Hua Yinchen,” but only the former is used in clinical practice in China. There are significant differences in quality between two species of A. Scopariae Herba and among A. Scopariae Herba from different harvest seasons and different producing areas, but the current comparative studies on the differences in quality of A. Scopariae Herba mainly focus on the latter; there are few comparative studies on the difference in quality between A. capillaris and A. scoparia. In this paper, the HPLC fingerprints of 13 batches of A. capillaris and 7 batches of A. scoparia harvested in spring were established, 21 common peaks in the fingerprints were demarcated, the constituents of these common peaks were identified by quadrupole‐TOF‐MS/MS, the chemical pattern recognition analysis, including hierarchical cluster analysis, principal component analysis, and orthogonal partial least squares discriminant analysis, were conducted with the quantified peak areas of common peaks as variables, and the contents of 12 constituents unambiguously confirmed by reference substances in 20 batches of A. Scopariae Herba were determined. The results showed that there exist obvious differences in quality between two species of A. Scopariae Herba, and 3,4‐dicaffeoylquinic acid, 4,5‐dicaffeoylquinic acid, 3,5‐dicaffeoylquinic acid, and chlorogenic acid can be selectively used as markers to distinguish the two species of A. Scopariae Herba.
{"title":"Quality Comparison Between Two Species of Artemisiae Scopariae Herba Through Qualitative Analysis of HPLC Fingerprint and Quantitative Analysis of 12 Representative Constituents","authors":"Luyao Wang, Jiale Geng, Chuanjuan Li, Rongrong Zhou, Ying Dai, Zhihua Dou","doi":"10.1002/sscp.202400077","DOIUrl":"https://doi.org/10.1002/sscp.202400077","url":null,"abstract":"Artemisiae Scopariae Herba (Chinese name Yinchen), the dried aerial part of Artemisia capillaris Thunb. (A. capillaris) or Artemisia scoparia Waldst. et Kit. (A. scoparia), is one of the most commonly used herbal drugs; the one harvested in the spring is habitually named “Mian Yinchen,” and the one harvested in the autumn is habitually named “Hua Yinchen,” but only the former is used in clinical practice in China. There are significant differences in quality between two species of A. Scopariae Herba and among A. Scopariae Herba from different harvest seasons and different producing areas, but the current comparative studies on the differences in quality of A. Scopariae Herba mainly focus on the latter; there are few comparative studies on the difference in quality between A. capillaris and A. scoparia. In this paper, the HPLC fingerprints of 13 batches of A. capillaris and 7 batches of A. scoparia harvested in spring were established, 21 common peaks in the fingerprints were demarcated, the constituents of these common peaks were identified by quadrupole‐TOF‐MS/MS, the chemical pattern recognition analysis, including hierarchical cluster analysis, principal component analysis, and orthogonal partial least squares discriminant analysis, were conducted with the quantified peak areas of common peaks as variables, and the contents of 12 constituents unambiguously confirmed by reference substances in 20 batches of A. Scopariae Herba were determined. The results showed that there exist obvious differences in quality between two species of A. Scopariae Herba, and 3,4‐dicaffeoylquinic acid, 4,5‐dicaffeoylquinic acid, 3,5‐dicaffeoylquinic acid, and chlorogenic acid can be selectively used as markers to distinguish the two species of A. Scopariae Herba.","PeriodicalId":508518,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-07-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141664100","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}
Bhavna Mahajan, Pankaj Miniyar, R. Chodankar, Anand Mahajan
The objective of the present research work was to demonstrate the application of liquid chromatography coupled with tandem mass spectrometry (LC‐MS/MS) for the separation, identification, and characterization of degradation products (DPs) of the drug lobeglitazone. The drug was subjected to various stress conditions such as oxidation, hydrolysis, thermal, and photolytic degradation as per the guidelines of the International Conference on Harmonization Q1A (R2). The drug was stable under thermal stress conditions, whereas it was susceptible to degradation in the other stress conditions forming four DPs. DPs were separated using a high‐performance LC system equipped with Zorbax SB C18 column (250 × 4.6 mm, 5 µm particles) using isocratic elution mode. The DPs were identified and characterized using MS and MS/MS. The chemical structure and fragmentation pattern were predicted for each degradant from the data obtained by mass studies. The drug and identified DPs were assessed by in‐silico approaches for predicting absorption, distribution, metabolism, and toxicity behavior. The in‐silico tools used for prediction were the pkCSM web server, ToxTree, and OSIRIS property explorer.
{"title":"Liquid chromatography and liquid chromatography coupled with tandem mass spectrometry studies for the identification and characterization of degradation products of lobeglitazone","authors":"Bhavna Mahajan, Pankaj Miniyar, R. Chodankar, Anand Mahajan","doi":"10.1002/sscp.202300223","DOIUrl":"https://doi.org/10.1002/sscp.202300223","url":null,"abstract":"The objective of the present research work was to demonstrate the application of liquid chromatography coupled with tandem mass spectrometry (LC‐MS/MS) for the separation, identification, and characterization of degradation products (DPs) of the drug lobeglitazone. The drug was subjected to various stress conditions such as oxidation, hydrolysis, thermal, and photolytic degradation as per the guidelines of the International Conference on Harmonization Q1A (R2). The drug was stable under thermal stress conditions, whereas it was susceptible to degradation in the other stress conditions forming four DPs. DPs were separated using a high‐performance LC system equipped with Zorbax SB C18 column (250 × 4.6 mm, 5 µm particles) using isocratic elution mode. The DPs were identified and characterized using MS and MS/MS. The chemical structure and fragmentation pattern were predicted for each degradant from the data obtained by mass studies. The drug and identified DPs were assessed by in‐silico approaches for predicting absorption, distribution, metabolism, and toxicity behavior. The in‐silico tools used for prediction were the pkCSM web server, ToxTree, and OSIRIS property explorer.","PeriodicalId":508518,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-06-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141273625","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}
Boyu Chen, Shengkai Liu, Hongxin Zhi, Jin Huang, Han Song, Jiashen Fan, Yujie Fu, Zhiguo Liu
Green extraction of the active lignans from Schisandra chinensis has received considerable attention due to their promising applications in the biomedical field. In this study, microwave‐assisted deep eutectic solvent method was used to simultaneously extract five lignans: Schizandrol A, Schizandrol B, Schisantherin A, Schisandrin A and Schizandrin B. The extraction parameters were optimized according to the calculated comprehensive score obtained from the analytic hierarchy process combined with the entropy weight method. The optimal extraction conditions were that the molar ratio of choline chloride and glycolic acid is 4:1, water content is 30% (V/V), solid–liquid ratio is 1:20 (Wg:VmL), extraction time is 20 min, and extraction temperature is 70°C, under which the extraction rate of the five lignans were 10.89, 8.616, 4.019, 4.893, and 5.318 mg/g. These results confirmed that our extraction method is efficient and feasible for green extraction of lignans from S. chinensis.
{"title":"Microwave‐assisted deep eutectic solvent extraction of five lignans from Schisandra chinensis","authors":"Boyu Chen, Shengkai Liu, Hongxin Zhi, Jin Huang, Han Song, Jiashen Fan, Yujie Fu, Zhiguo Liu","doi":"10.1002/sscp.202400006","DOIUrl":"https://doi.org/10.1002/sscp.202400006","url":null,"abstract":"Green extraction of the active lignans from Schisandra chinensis has received considerable attention due to their promising applications in the biomedical field. In this study, microwave‐assisted deep eutectic solvent method was used to simultaneously extract five lignans: Schizandrol A, Schizandrol B, Schisantherin A, Schisandrin A and Schizandrin B. The extraction parameters were optimized according to the calculated comprehensive score obtained from the analytic hierarchy process combined with the entropy weight method. The optimal extraction conditions were that the molar ratio of choline chloride and glycolic acid is 4:1, water content is 30% (V/V), solid–liquid ratio is 1:20 (Wg:VmL), extraction time is 20 min, and extraction temperature is 70°C, under which the extraction rate of the five lignans were 10.89, 8.616, 4.019, 4.893, and 5.318 mg/g. These results confirmed that our extraction method is efficient and feasible for green extraction of lignans from S. chinensis.","PeriodicalId":508518,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-03-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140223392","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}
Ruihua Liu, Zhengqiao Kong, Dan Wu, Jiasi Yu, Ping Liu
The application of veterinary drugs has brought great economic benefits, but its unreasonable application has also caused a series of safety problems. The study aimed to establish methods that will provide accurate quantitative information for the monitoring of veterinary drug residues in animal‐derived foods. Selecting nine veterinary drugs in four categories, the study combined quick, easy, cheap, effective, rugged, and safe technology with high‐performance liquid chromatography (HPLC) to detect multiple veterinary drugs in animal foods simultaneously. The study established two rapid, efficient, and accurate HPLC‐diode array detection methods to achieve the simultaneous detection of nitroimidazoles and β‐adrenergic agonists, and the simultaneous detection of benzimidazoles and diethylstilbestrol. The limit of detection of the former was 1.36–2.05 μg/kg and the latter 0.42–0.72 μg/kg. Then the two methods were used to detect veterinary drug residues in 297 animal foods from 10 categories to investigate the drug residues. For the seven banned drugs, the detection rates ranged from 1.35% to 7.41%. And for the two restricted drugs, the over‐standard rates were 4.38% and 0.00%.
{"title":"The combined determinations of multiple veterinary drugs in animal foods by high‐performance liquid chromatography‐diode array detection and their application in drug residue investigation","authors":"Ruihua Liu, Zhengqiao Kong, Dan Wu, Jiasi Yu, Ping Liu","doi":"10.1002/sscp.202300234","DOIUrl":"https://doi.org/10.1002/sscp.202300234","url":null,"abstract":"The application of veterinary drugs has brought great economic benefits, but its unreasonable application has also caused a series of safety problems. The study aimed to establish methods that will provide accurate quantitative information for the monitoring of veterinary drug residues in animal‐derived foods. Selecting nine veterinary drugs in four categories, the study combined quick, easy, cheap, effective, rugged, and safe technology with high‐performance liquid chromatography (HPLC) to detect multiple veterinary drugs in animal foods simultaneously. The study established two rapid, efficient, and accurate HPLC‐diode array detection methods to achieve the simultaneous detection of nitroimidazoles and β‐adrenergic agonists, and the simultaneous detection of benzimidazoles and diethylstilbestrol. The limit of detection of the former was 1.36–2.05 μg/kg and the latter 0.42–0.72 μg/kg. Then the two methods were used to detect veterinary drug residues in 297 animal foods from 10 categories to investigate the drug residues. For the seven banned drugs, the detection rates ranged from 1.35% to 7.41%. And for the two restricted drugs, the over‐standard rates were 4.38% and 0.00%.","PeriodicalId":508518,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-03-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140252775","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}
Z. Aydoğmuş, E. Yılmaz, Narin Öztürk Seyhan, A. Okyar
This study reports a rapid and sensitive reversed‐phase high‐performance liquid chromatography method with ultraviolet detection for the determination of regorafenib (REG) in rat plasma. For the extraction of REG from plasma and the precipitation of plasma proteins, a rapid one‐step precipitation method was performed with methanol. The separation was performed in a methanol‐water mixture (80:20, v:v) mobile phase system with a C18 column and monitored at a wavelength of 258 nm. Nilotinib was used as an internal standard. The linear dynamic range of REG was determined between 5 and 500 ng/mL in standard solution and plasma. The limit of detection of REG from the standard solution was found to be 1.23 ng/mL and the limit of quantitation was 3.73 ng/mL. The limit of detection of REG from plasma was found to be 1.55 ng/mL and the limit of quantitation was 4.70 ng/mL. Regorafenib was administered at 5 mg/kg to 10 healthy male Sprague Dawley rats, and pharmacokinetic results were evaluated. It exhibited a high recovery of 93.82% in plasma. Due to ease of sample preparation, high susceptibility, specificity, and certainty, the described method can be used successfully in the quantification of REG in in‐vivo plasma and in routine analyses in clinical laboratories.
{"title":"A new validated high‐performance liquid chromatography method for the determination of regorafenib in rat plasma: Application for pharmacokinetic study","authors":"Z. Aydoğmuş, E. Yılmaz, Narin Öztürk Seyhan, A. Okyar","doi":"10.1002/sscp.202400013","DOIUrl":"https://doi.org/10.1002/sscp.202400013","url":null,"abstract":"This study reports a rapid and sensitive reversed‐phase high‐performance liquid chromatography method with ultraviolet detection for the determination of regorafenib (REG) in rat plasma. For the extraction of REG from plasma and the precipitation of plasma proteins, a rapid one‐step precipitation method was performed with methanol. The separation was performed in a methanol‐water mixture (80:20, v:v) mobile phase system with a C18 column and monitored at a wavelength of 258 nm. Nilotinib was used as an internal standard. The linear dynamic range of REG was determined between 5 and 500 ng/mL in standard solution and plasma. The limit of detection of REG from the standard solution was found to be 1.23 ng/mL and the limit of quantitation was 3.73 ng/mL. The limit of detection of REG from plasma was found to be 1.55 ng/mL and the limit of quantitation was 4.70 ng/mL. Regorafenib was administered at 5 mg/kg to 10 healthy male Sprague Dawley rats, and pharmacokinetic results were evaluated. It exhibited a high recovery of 93.82% in plasma. Due to ease of sample preparation, high susceptibility, specificity, and certainty, the described method can be used successfully in the quantification of REG in in‐vivo plasma and in routine analyses in clinical laboratories.","PeriodicalId":508518,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-03-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140255343","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}
Taibai ginseng (roots of Pedicularis decora Franch.) has been reported to possess anti‐Alzheimer's disease (anti‐AD) activity and can be potentially used for treating AD. However, the chemical constituents of taibai ginseng have not yet been elucidated because of the paucity of relevant studies, which hinders further research on the pharmacological mechanism and utilization of taibai ginseng. In this study, a rapid and efficient method for comprehensively analyzing the chemical constituents of taibai ginseng was established for the first time. We used ultra‐high performance liquid chromatography‐quadrupole time of flight mass spectrometry in combination with the UNIFI data‐processing platform to automatically characterize and identify the chemical profile of taibai ginseng. As a result, more than 76 compounds were detected, and their structures were characterized. These compounds include 24 iridoid glycosides, 24 phenylethanol glycosides, 15 terpenoids, and 13 other components. More than fifty of these compounds from taibai ginseng were reported for the first time. Our results provide a reference for the quality control of taibai ginseng and establish a higher quality standard for pharmacodynamic research. Appropriate modification of the method reported herein can enable its use for the screening and characterization of taibai ginseng and other compounds from the Pedicularis genus.
{"title":"Profiling and characterization of the constituents of taibai ginseng using ultra‐high performance liquid chromatography‐quadrupole time of flight mass spectrometry","authors":"Xin Gao, Wenjun Sun, Yaxuan Wang, Xiaohui Li, Xia Liu, Yunzhe Li, Xiaofeng Niu","doi":"10.1002/sscp.202300206","DOIUrl":"https://doi.org/10.1002/sscp.202300206","url":null,"abstract":"Taibai ginseng (roots of Pedicularis decora Franch.) has been reported to possess anti‐Alzheimer's disease (anti‐AD) activity and can be potentially used for treating AD. However, the chemical constituents of taibai ginseng have not yet been elucidated because of the paucity of relevant studies, which hinders further research on the pharmacological mechanism and utilization of taibai ginseng. In this study, a rapid and efficient method for comprehensively analyzing the chemical constituents of taibai ginseng was established for the first time. We used ultra‐high performance liquid chromatography‐quadrupole time of flight mass spectrometry in combination with the UNIFI data‐processing platform to automatically characterize and identify the chemical profile of taibai ginseng. As a result, more than 76 compounds were detected, and their structures were characterized. These compounds include 24 iridoid glycosides, 24 phenylethanol glycosides, 15 terpenoids, and 13 other components. More than fifty of these compounds from taibai ginseng were reported for the first time. Our results provide a reference for the quality control of taibai ginseng and establish a higher quality standard for pharmacodynamic research. Appropriate modification of the method reported herein can enable its use for the screening and characterization of taibai ginseng and other compounds from the Pedicularis genus.","PeriodicalId":508518,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-03-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140256534","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}
Deucravacitinib, SOTYKTU was approved recently in the year 2022 to treat psoriasis. The present work attempts to identify and characterize degradation products formed when the drug is exposed to hydrolytic, oxidative, thermal, and photolytic stress conditions as well as to study the kinetics of the drug's degradation under various stress conditions. A high‐performance liquid chromatography method was developed for the separation of deucravacitinib and its degradation product comprising mobile phase of ammonium acetate (pH 4.75) buffer as solvent A and acetonitrile as solvent B and Phenomenex Gemini, C‐18 (250 × 4.6 mm, 5µ) column as stationary phase. Injection volume, flow rate, and detection wavelength for the method were optimized as 10 µL, 1.0 mL/min, and 254 nm, respectively. Accuracy, precision, linearity, robustness, and selectivity were found to be acceptable when validated in the concentration range between 5 and 150 µg/mL of deucravacitinib. The structure of the degradation product was characterized using liquid chromatography‐tandem mass spectrometry which shows a protonated molecular ion peak at m/z 358.1805 in the electrospray ionization positive mode. In silico mutagenicity tests yielded positive results for deucravacitinib and its degradation product, triggering an alarm for mutagenicity for both structures, whereas in silico toxicity studies did not generate any structural alerts.
{"title":"Separation and characterization of hydrolytic degradation product of deucravacitinib by validated high‐performance liquid chromatography method and liquid chromatography‐mass spectrometry","authors":"Vijaya Madhyanapu Golla, Rahul Khemchandani, Sowmya Chaganti, Gananadhamu Samanthula","doi":"10.1002/sscp.202300180","DOIUrl":"https://doi.org/10.1002/sscp.202300180","url":null,"abstract":"Deucravacitinib, SOTYKTU was approved recently in the year 2022 to treat psoriasis. The present work attempts to identify and characterize degradation products formed when the drug is exposed to hydrolytic, oxidative, thermal, and photolytic stress conditions as well as to study the kinetics of the drug's degradation under various stress conditions. A high‐performance liquid chromatography method was developed for the separation of deucravacitinib and its degradation product comprising mobile phase of ammonium acetate (pH 4.75) buffer as solvent A and acetonitrile as solvent B and Phenomenex Gemini, C‐18 (250 × 4.6 mm, 5µ) column as stationary phase. Injection volume, flow rate, and detection wavelength for the method were optimized as 10 µL, 1.0 mL/min, and 254 nm, respectively. Accuracy, precision, linearity, robustness, and selectivity were found to be acceptable when validated in the concentration range between 5 and 150 µg/mL of deucravacitinib. The structure of the degradation product was characterized using liquid chromatography‐tandem mass spectrometry which shows a protonated molecular ion peak at m/z 358.1805 in the electrospray ionization positive mode. In silico mutagenicity tests yielded positive results for deucravacitinib and its degradation product, triggering an alarm for mutagenicity for both structures, whereas in silico toxicity studies did not generate any structural alerts.","PeriodicalId":508518,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-03-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140080302","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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