Pub Date : 2021-11-30DOI: 10.3390/analytica2040016
R. Mandrioli, M. Protti, Lorenzo Marincich, L. Mercolini
The term seizures includes a wide array of different disorders with variable etiology, which currently represent one of the most important classes of neurological illnesses. As a consequence, many different antiepileptic drugs (AEDs) are currently available, exploiting different activity mechanisms and providing different levels of performance in terms of selectivity, safety, and efficacy. AEDs are currently among the psychoactive drugs most frequently involved in therapeutic drug monitoring (TDM) practices. Thus, the plasma levels of AEDs and their metabolites are monitored and correlated to administered doses, therapeutic efficacy, side effects, and toxic effects. As for any analytical endeavour, the quality of plasma concentration data is only as good as the analytical method allows. In this review, the main techniques and methods are described, suitable for the TDM of three AEDs belonging to the class of ion channel agents: ezogabine (or retigabine), lacosamide, and zonisamide. In addition to this analytical overview, data are provided, pertaining to two of the most important use cases for the TDM of antiepileptics: drug–drug interactions and neuroprotection activity studies. This review contains 146 references.
{"title":"Ion-Channel Antiepileptic Drugs: An Analytical Perspective on the Therapeutic Drug Monitoring (TDM) of Ezogabine, Lacosamide, and Zonisamide","authors":"R. Mandrioli, M. Protti, Lorenzo Marincich, L. Mercolini","doi":"10.3390/analytica2040016","DOIUrl":"https://doi.org/10.3390/analytica2040016","url":null,"abstract":"The term seizures includes a wide array of different disorders with variable etiology, which currently represent one of the most important classes of neurological illnesses. As a consequence, many different antiepileptic drugs (AEDs) are currently available, exploiting different activity mechanisms and providing different levels of performance in terms of selectivity, safety, and efficacy. AEDs are currently among the psychoactive drugs most frequently involved in therapeutic drug monitoring (TDM) practices. Thus, the plasma levels of AEDs and their metabolites are monitored and correlated to administered doses, therapeutic efficacy, side effects, and toxic effects. As for any analytical endeavour, the quality of plasma concentration data is only as good as the analytical method allows. In this review, the main techniques and methods are described, suitable for the TDM of three AEDs belonging to the class of ion channel agents: ezogabine (or retigabine), lacosamide, and zonisamide. In addition to this analytical overview, data are provided, pertaining to two of the most important use cases for the TDM of antiepileptics: drug–drug interactions and neuroprotection activity studies. This review contains 146 references.","PeriodicalId":7829,"journal":{"name":"Analytica","volume":"458 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2021-11-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"79789892","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}
Pub Date : 2021-10-13DOI: 10.3390/analytica2040015
L. Sánchez-Magraner, M. de la Fuente, C. Evans, J. Miles, Ane Elexpe, Maddalen Rodriguez-Astigarraga, E. Astigarraga, Gabriel Barreda-Gómez
Melanoma is a carcinoma known to evade the host immune defenses via the downregulation of the immune response. One of the molecules involved in this mechanism is programmed cell death ligand 1 (PD-L1), which interacts with its receptor, programmed cell death protein 1 (PD-1), expressed on T cells, leading to a reduction in cytokine release and cytotoxic activity, as well as a halt in T-cell proliferation. The approved therapeutic monoclonal antibodies, such as pembrolizumab, target the PD-1/PD-L1 interaction and are revolutionizing cancer treatments. We developed an assay that provides a quantitative readout of PD-1/PD-L1 interactive states between cell membranes of human immune cells (peripheral blood mononuclear cells, PBMCs) and PD-L1-expressing samples. For this purpose, cell membrane microarrays (CMMAs) were developed from membranes isolated from a HT144 cell line and melanoma samples, and PD-L1 expression was quantified using immunofluorescence (IF). CMMAs were incubated with cell membranes of PBMCs expressing PD-1, and the interaction with PD-L1 was quantified by time-resolved Förster resonance energy transfer, in the presence and absence of pembrolizumab as a blocking drug. The developed assay was able to quantify the PD-1/PD-L1 interaction, and this engagement was disrupted in the presence of the blocking antibody. This demonstrates the potential of the method to analyze monoclonal antibody drugs, as well as the functional states of immune checkpoint regulators. Furthermore, our findings provide evidence to support the future implementation of this methodology for both drug discovery and immune system monitoring in cancer, transplantation, and inflammatory and autoimmune diseases.
{"title":"Quantification of PD-1/PD-L1 Interaction between Membranes from PBMCs and Melanoma Samples Using Cell Membrane Microarray and Time-Resolved Förster Resonance Energy Transfer","authors":"L. Sánchez-Magraner, M. de la Fuente, C. Evans, J. Miles, Ane Elexpe, Maddalen Rodriguez-Astigarraga, E. Astigarraga, Gabriel Barreda-Gómez","doi":"10.3390/analytica2040015","DOIUrl":"https://doi.org/10.3390/analytica2040015","url":null,"abstract":"Melanoma is a carcinoma known to evade the host immune defenses via the downregulation of the immune response. One of the molecules involved in this mechanism is programmed cell death ligand 1 (PD-L1), which interacts with its receptor, programmed cell death protein 1 (PD-1), expressed on T cells, leading to a reduction in cytokine release and cytotoxic activity, as well as a halt in T-cell proliferation. The approved therapeutic monoclonal antibodies, such as pembrolizumab, target the PD-1/PD-L1 interaction and are revolutionizing cancer treatments. We developed an assay that provides a quantitative readout of PD-1/PD-L1 interactive states between cell membranes of human immune cells (peripheral blood mononuclear cells, PBMCs) and PD-L1-expressing samples. For this purpose, cell membrane microarrays (CMMAs) were developed from membranes isolated from a HT144 cell line and melanoma samples, and PD-L1 expression was quantified using immunofluorescence (IF). CMMAs were incubated with cell membranes of PBMCs expressing PD-1, and the interaction with PD-L1 was quantified by time-resolved Förster resonance energy transfer, in the presence and absence of pembrolizumab as a blocking drug. The developed assay was able to quantify the PD-1/PD-L1 interaction, and this engagement was disrupted in the presence of the blocking antibody. This demonstrates the potential of the method to analyze monoclonal antibody drugs, as well as the functional states of immune checkpoint regulators. Furthermore, our findings provide evidence to support the future implementation of this methodology for both drug discovery and immune system monitoring in cancer, transplantation, and inflammatory and autoimmune diseases.","PeriodicalId":7829,"journal":{"name":"Analytica","volume":"41 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2021-10-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"86496042","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}
Pub Date : 2021-10-09DOI: 10.3390/analytica2040014
Mowei Zhou, Ju Yeon Lee, Gun Wook Park, Neha Malhan, Tao Liu, J. Shaw
Despite the successful application of tandem mass tags (TMT) for peptide quantitation, missing reporter ions in higher energy collisional dissociation (HCD) spectra remains a challenge for consistent quantitation, especially for peptides with labile post-translational modifications. Ultraviolet photodissociation (UVPD) is an alternative ion activation method shown to provide superior coverage for sequencing of peptides and intact proteins. Here, we optimized and evaluated 193 nm UVPD for the characterization of TMT-labeled model peptides, HeLa proteome, and N-glycopeptides from model proteins. UVPD yielded the same TMT reporter ions as HCD, at m/z 126–131. Additionally, UVPD produced a wide range of fragments that yielded more complete characterization of glycopeptides and less frequent missing TMT reporter ion channels, whereas HCD yielded a strong tradeoff between characterization and quantitation of TMT-labeled glycopeptides. However, the lower fragmentation efficiency of UVPD yielded fewer peptide identifications than HCD. Overall, 193 nm UVPD is a valuable tool that provides an alternative to HCD for the quantitation of large and highly modified peptides with labile PTMs. Continued development of instrumentation specific to UVPD will yield greater fragmentation efficiency and fulfil the potential of UVPD to be an all-in-one spectrum ion activation method for broad use in the field of proteomics.
{"title":"Evaluating the Performance of 193 nm Ultraviolet Photodissociation for Tandem Mass Tag Labeled Peptides","authors":"Mowei Zhou, Ju Yeon Lee, Gun Wook Park, Neha Malhan, Tao Liu, J. Shaw","doi":"10.3390/analytica2040014","DOIUrl":"https://doi.org/10.3390/analytica2040014","url":null,"abstract":"Despite the successful application of tandem mass tags (TMT) for peptide quantitation, missing reporter ions in higher energy collisional dissociation (HCD) spectra remains a challenge for consistent quantitation, especially for peptides with labile post-translational modifications. Ultraviolet photodissociation (UVPD) is an alternative ion activation method shown to provide superior coverage for sequencing of peptides and intact proteins. Here, we optimized and evaluated 193 nm UVPD for the characterization of TMT-labeled model peptides, HeLa proteome, and N-glycopeptides from model proteins. UVPD yielded the same TMT reporter ions as HCD, at m/z 126–131. Additionally, UVPD produced a wide range of fragments that yielded more complete characterization of glycopeptides and less frequent missing TMT reporter ion channels, whereas HCD yielded a strong tradeoff between characterization and quantitation of TMT-labeled glycopeptides. However, the lower fragmentation efficiency of UVPD yielded fewer peptide identifications than HCD. Overall, 193 nm UVPD is a valuable tool that provides an alternative to HCD for the quantitation of large and highly modified peptides with labile PTMs. Continued development of instrumentation specific to UVPD will yield greater fragmentation efficiency and fulfil the potential of UVPD to be an all-in-one spectrum ion activation method for broad use in the field of proteomics.","PeriodicalId":7829,"journal":{"name":"Analytica","volume":"12 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2021-10-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"82632855","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}
Pub Date : 2021-10-03DOI: 10.3390/analytica2040013
Antonio Marín-Romero, Mavys Tabraue-Chávez, Bárbara López-Longarela, M. A. Fara, R. Sánchez-Martín, J. Dear, Hugh Ilyine, J. Díaz-Mochón, Salvatore Pernagallo
Drug-induced liver injury (DILI) is a potentially fatal adverse event and a leading cause for pre- and post-marketing drug withdrawal. Several multinational DILI initiatives have now recommended a panel of protein and microRNA (miRNA) biomarkers that can detect early liver injury and inform about mechanistic basis. This manuscript describes the development of seqCOMBO, a unique combo-multiplexed assay which combines the dynamic chemical labelling approach and an antibody-dependant method on the Luminex MAGPIX system. SeqCOMBO enables a versatile multiplexing platform to perform qualitative and quantitative analysis of proteins and miRNAs in patient serum samples simultaneously. To the best of our knowledge, this is the first method to profile protein and miRNA biomarkers to diagnose DILI in a single-step assay.
{"title":"Simultaneous Detection of Drug-Induced Liver Injury Protein and microRNA Biomarkers Using Dynamic Chemical Labelling on a Luminex MAGPIX System","authors":"Antonio Marín-Romero, Mavys Tabraue-Chávez, Bárbara López-Longarela, M. A. Fara, R. Sánchez-Martín, J. Dear, Hugh Ilyine, J. Díaz-Mochón, Salvatore Pernagallo","doi":"10.3390/analytica2040013","DOIUrl":"https://doi.org/10.3390/analytica2040013","url":null,"abstract":"Drug-induced liver injury (DILI) is a potentially fatal adverse event and a leading cause for pre- and post-marketing drug withdrawal. Several multinational DILI initiatives have now recommended a panel of protein and microRNA (miRNA) biomarkers that can detect early liver injury and inform about mechanistic basis. This manuscript describes the development of seqCOMBO, a unique combo-multiplexed assay which combines the dynamic chemical labelling approach and an antibody-dependant method on the Luminex MAGPIX system. SeqCOMBO enables a versatile multiplexing platform to perform qualitative and quantitative analysis of proteins and miRNAs in patient serum samples simultaneously. To the best of our knowledge, this is the first method to profile protein and miRNA biomarkers to diagnose DILI in a single-step assay.","PeriodicalId":7829,"journal":{"name":"Analytica","volume":"45 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2021-10-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"72826790","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}
Pub Date : 2021-09-24DOI: 10.3390/analytica2040011
Sofia Karanikolopoulou, Panagiota-Kyriaki Revelou, Marinos Xagoraris, Maroula G. Kokotou, V. Constantinou-Kokotou
Cruciferous vegetables are characterized by the presence of sulfur-containing secondary plant metabolites known as glucosinolates (GLS). The consumption of cruciferous vegetables such as broccoli, cabbage, rocket salad, and cauliflower has been related to the prevention of non-communicable diseases. Their beneficial effects are attributed to the enzymatic degradation products of GLS, e.g., isothiocyanates and indoles. Owing to these properties, there has been a shift in the last few years towards the research of these compounds and a wide range of methods for their extraction and analytical determination have been developed. The aim of this review is to present the sample preparation and extraction procedures of isothiocyanates and indoles from cruciferous vegetables and the analytical methods for their determination. The majority of the references that have been reviewed are from the last decade. Although efforts towards the application of eco-friendly non-conventional extraction methods have been made, the use of conventional solvent extraction is mainly applied. The major analytical techniques employed for the qualitative and quantitative analysis of isothiocyanates and indoles are high-performance liquid chromatography and gas chromatography coupled with or without mass spectrometry detection. Nevertheless, the analytical determination of isothiocyanates presents several problems due to their instability and the absence of chromophores, making the simultaneous determination of isothiocyanates and indoles a challenging task.
{"title":"Current Methods for the Extraction and Analysis of Isothiocyanates and Indoles in Cruciferous Vegetables","authors":"Sofia Karanikolopoulou, Panagiota-Kyriaki Revelou, Marinos Xagoraris, Maroula G. Kokotou, V. Constantinou-Kokotou","doi":"10.3390/analytica2040011","DOIUrl":"https://doi.org/10.3390/analytica2040011","url":null,"abstract":"Cruciferous vegetables are characterized by the presence of sulfur-containing secondary plant metabolites known as glucosinolates (GLS). The consumption of cruciferous vegetables such as broccoli, cabbage, rocket salad, and cauliflower has been related to the prevention of non-communicable diseases. Their beneficial effects are attributed to the enzymatic degradation products of GLS, e.g., isothiocyanates and indoles. Owing to these properties, there has been a shift in the last few years towards the research of these compounds and a wide range of methods for their extraction and analytical determination have been developed. The aim of this review is to present the sample preparation and extraction procedures of isothiocyanates and indoles from cruciferous vegetables and the analytical methods for their determination. The majority of the references that have been reviewed are from the last decade. Although efforts towards the application of eco-friendly non-conventional extraction methods have been made, the use of conventional solvent extraction is mainly applied. The major analytical techniques employed for the qualitative and quantitative analysis of isothiocyanates and indoles are high-performance liquid chromatography and gas chromatography coupled with or without mass spectrometry detection. Nevertheless, the analytical determination of isothiocyanates presents several problems due to their instability and the absence of chromophores, making the simultaneous determination of isothiocyanates and indoles a challenging task.","PeriodicalId":7829,"journal":{"name":"Analytica","volume":"20 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2021-09-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"73390005","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}
Pub Date : 2021-08-30DOI: 10.3390/analytica2030010
S. Arduini, Alessandro Zappi, M. Locatelli, Salvatore Sgrò, D. Melucci
An authenticity study on Italian grape marc spirit was carried out by gas chromatography (GC) and chemometrics. A grape marc spirit produced in Italy takes the particular name of “grappa”, a product which has peculiar tradition and production in its country of origin. Therefore, the evaluation of its authenticity plays an important role for its consumption in Italy, as well as for its exportation all around the world. For the present work, 123 samples of grappa and several kinds of spirits were analyzed in their alcohol content by electronic densimetry, and in their volatile fraction by gas-chromatography with a flame-ionization detector. Part of these samples (94) was employed as a training set to compute a chemometric model (by linear discriminant analysis, LDA) and the other part (29 samples) was used as a test set to validate it. Finally, two grappa samples seized from the market by the Italian Customs and Monopolies Agency and considered suspicious due to their aroma reported as non-compliant were projected onto the LDA model to evaluate the compliance with the “grappa” class. A further one-class classification method by principal component analysis (PCA) was carried out to evaluate the compliance with other classes. Results showed that the suspicious samples were not recognized as belonging to any of the analyzed spirit classes, confirming the starting hypothesis that they could be grappa samples adulterated in some way.
{"title":"An Authentication Study on Grappa Spirit: The Use of Chemometrics to Detect a Food Fraud","authors":"S. Arduini, Alessandro Zappi, M. Locatelli, Salvatore Sgrò, D. Melucci","doi":"10.3390/analytica2030010","DOIUrl":"https://doi.org/10.3390/analytica2030010","url":null,"abstract":"An authenticity study on Italian grape marc spirit was carried out by gas chromatography (GC) and chemometrics. A grape marc spirit produced in Italy takes the particular name of “grappa”, a product which has peculiar tradition and production in its country of origin. Therefore, the evaluation of its authenticity plays an important role for its consumption in Italy, as well as for its exportation all around the world. For the present work, 123 samples of grappa and several kinds of spirits were analyzed in their alcohol content by electronic densimetry, and in their volatile fraction by gas-chromatography with a flame-ionization detector. Part of these samples (94) was employed as a training set to compute a chemometric model (by linear discriminant analysis, LDA) and the other part (29 samples) was used as a test set to validate it. Finally, two grappa samples seized from the market by the Italian Customs and Monopolies Agency and considered suspicious due to their aroma reported as non-compliant were projected onto the LDA model to evaluate the compliance with the “grappa” class. A further one-class classification method by principal component analysis (PCA) was carried out to evaluate the compliance with other classes. Results showed that the suspicious samples were not recognized as belonging to any of the analyzed spirit classes, confirming the starting hypothesis that they could be grappa samples adulterated in some way.","PeriodicalId":7829,"journal":{"name":"Analytica","volume":"140 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2021-08-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"79999039","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}
Pub Date : 2021-08-03DOI: 10.3390/analytica2030009
D. Melucci, S. Casolari, M. Locatelli, C. Locatelli
The present paper reports a new application: the voltammetric determination in herbal medicines of ultra-trace thallium(I), in the presence of lead(II), tin(II) and antimony(III) as interfering metals, by square wave anodic stripping voltammetry (SWASV). A conventional three-electrodes voltammetric cell was employed with a stationary hanging mercury drop electrode (HMDE) as working electrode and a platinum electrode and an Ag|AgCl|KClsatd. electrode as auxiliary and reference electrodes, respectively. The supporting electrolyte was 0.5 mol L−1 ammonium citrate buffer pH 6.5 + 7.3·10−3 mol L−1 EDTA-Na2. The analytical procedure was verified by the analysis of the standard reference materials: spinach Leaves NIST-SRM 1570a and tomato leaves NIST-SRM 1573a from National Institute of Standards and Technology. Precision and trueness, expressed as relative standard deviation and relative error, respectively, were generally lower than 7% in all cases. Once set up on the standard reference materials, the analytical procedure was transferred and applied to herbal medicines samples—Taraxacun officinale weber, Eucalyptus globulus and Harpagophytum procumbens DC—sold on the market. A critical comparison with spectroscopic measurements is also discussed.
{"title":"Thallium: A Polluting Metal of New Generation. Its Voltammetric Determination in Herbal Medicines in Presence of Metal Interferences","authors":"D. Melucci, S. Casolari, M. Locatelli, C. Locatelli","doi":"10.3390/analytica2030009","DOIUrl":"https://doi.org/10.3390/analytica2030009","url":null,"abstract":"The present paper reports a new application: the voltammetric determination in herbal medicines of ultra-trace thallium(I), in the presence of lead(II), tin(II) and antimony(III) as interfering metals, by square wave anodic stripping voltammetry (SWASV). A conventional three-electrodes voltammetric cell was employed with a stationary hanging mercury drop electrode (HMDE) as working electrode and a platinum electrode and an Ag|AgCl|KClsatd. electrode as auxiliary and reference electrodes, respectively. The supporting electrolyte was 0.5 mol L−1 ammonium citrate buffer pH 6.5 + 7.3·10−3 mol L−1 EDTA-Na2. The analytical procedure was verified by the analysis of the standard reference materials: spinach Leaves NIST-SRM 1570a and tomato leaves NIST-SRM 1573a from National Institute of Standards and Technology. Precision and trueness, expressed as relative standard deviation and relative error, respectively, were generally lower than 7% in all cases. Once set up on the standard reference materials, the analytical procedure was transferred and applied to herbal medicines samples—Taraxacun officinale weber, Eucalyptus globulus and Harpagophytum procumbens DC—sold on the market. A critical comparison with spectroscopic measurements is also discussed.","PeriodicalId":7829,"journal":{"name":"Analytica","volume":"50 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2021-08-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"91058136","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}
Pub Date : 2021-08-02DOI: 10.3390/analytica2030008
Toshiki Horikoshi, C. Kitaoka, Yosuke Fujii, T. Asano, Jiawei Xu, T. Fujino
The ingredients of an antipyretic (acetaminophen, AAP) and their metabolites excreted into fingerprint were detected by surface-assisted laser desorption ionization (SALDI) mass spectrometry using zeolite. In the fingerprint taken 4 h after AAP ingestion, not only AAP but also the glucuronic acid conjugate of AAP (GAAP), caffeine (Caf), ethenzamide (Eth), salicylamide (Sala; a metabolite of Eth), and urea were detected. Fingerprints were collected over time to determine how the amounts of AAP and its metabolite changed with time, and the time dependence of the peak intensities of protonated AAP and GAAP was measured. It was found that the increase of [GAAP+H]+ peak started later than that of [AAP+H]+ peak, reflecting the metabolism of AAP. Both AAP and GAAP reached maximum concentrations approximately 3 h after ingestion, and were excreted from the body with a half-life of approximately 3.3 h. In addition, fingerprint preservation was confirmed by optical microscopy, and fingerprint shape was retained even after laser irradiation of the fingerprint. Our method may be used in fingerprint analysis.
{"title":"Detection of Acetaminophen and Its Glucuronide in Fingerprint by SALDI Mass Spectrometry Using Zeolite and Study of Time-Dependent Changes in Detected Ion Amount","authors":"Toshiki Horikoshi, C. Kitaoka, Yosuke Fujii, T. Asano, Jiawei Xu, T. Fujino","doi":"10.3390/analytica2030008","DOIUrl":"https://doi.org/10.3390/analytica2030008","url":null,"abstract":"The ingredients of an antipyretic (acetaminophen, AAP) and their metabolites excreted into fingerprint were detected by surface-assisted laser desorption ionization (SALDI) mass spectrometry using zeolite. In the fingerprint taken 4 h after AAP ingestion, not only AAP but also the glucuronic acid conjugate of AAP (GAAP), caffeine (Caf), ethenzamide (Eth), salicylamide (Sala; a metabolite of Eth), and urea were detected. Fingerprints were collected over time to determine how the amounts of AAP and its metabolite changed with time, and the time dependence of the peak intensities of protonated AAP and GAAP was measured. It was found that the increase of [GAAP+H]+ peak started later than that of [AAP+H]+ peak, reflecting the metabolism of AAP. Both AAP and GAAP reached maximum concentrations approximately 3 h after ingestion, and were excreted from the body with a half-life of approximately 3.3 h. In addition, fingerprint preservation was confirmed by optical microscopy, and fingerprint shape was retained even after laser irradiation of the fingerprint. Our method may be used in fingerprint analysis.","PeriodicalId":7829,"journal":{"name":"Analytica","volume":"31 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2021-08-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"91171399","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}
Pub Date : 2021-07-07DOI: 10.3390/ANALYTICA2030007
F. A. Isse, S. Mahmoud
Clobazam (CLB) is a benzodiazepine that is used in many types of epilepsy. Although therapeutic drug monitoring (TDM) of CLB is not routine, there is evidence that TDM may be of value in conditions where pharmacokinetic alterations are suspected. Therefore, determination of both CLB and its active metabolite concentrations is essential for TDM. Herein, we present a simple and practical method for determination of CLB and N-desmethylclobazam (NDMCLB) in human plasma by high-performance liquid chromatography (HPLC). The drugs were extracted by hexane:dichloromethane (1:1, v/v) from 0.3 mL plasma. The separation was carried out with a C18 reverse phase column using a mobile phase of water:acetonitrile (57:43, v/v) pumped at 0.8 mL/min. The analytes were detected at 228 nm. The method was linear over the concentration range 20–500 ng/mL for CLB and 200–3000 ng/mL for NDMCLB. The intra-day coefficient of variation (CV) was <10% for CLB and <6% for NDMCLB, while the inter-day CV for CLB was <16%. The metabolite inter-day CV was <6%. The accuracy of intra- and inter-day assessments determined for CLB and NDMCLB was within ±10%. This paper describes a rapid, reliable, and simple method for measuring CLB and its metabolite NDMCLB in human plasma. This UV-HPLC procedure offers acceptable precision and accuracy to quantify CLB and its metabolite in human plasma.
{"title":"Determination of Clobazam and Its Major Metabolite N-desmethylclobazam in Human Plasma with High-Performance Liquid Chromatography","authors":"F. A. Isse, S. Mahmoud","doi":"10.3390/ANALYTICA2030007","DOIUrl":"https://doi.org/10.3390/ANALYTICA2030007","url":null,"abstract":"Clobazam (CLB) is a benzodiazepine that is used in many types of epilepsy. Although therapeutic drug monitoring (TDM) of CLB is not routine, there is evidence that TDM may be of value in conditions where pharmacokinetic alterations are suspected. Therefore, determination of both CLB and its active metabolite concentrations is essential for TDM. Herein, we present a simple and practical method for determination of CLB and N-desmethylclobazam (NDMCLB) in human plasma by high-performance liquid chromatography (HPLC). The drugs were extracted by hexane:dichloromethane (1:1, v/v) from 0.3 mL plasma. The separation was carried out with a C18 reverse phase column using a mobile phase of water:acetonitrile (57:43, v/v) pumped at 0.8 mL/min. The analytes were detected at 228 nm. The method was linear over the concentration range 20–500 ng/mL for CLB and 200–3000 ng/mL for NDMCLB. The intra-day coefficient of variation (CV) was <10% for CLB and <6% for NDMCLB, while the inter-day CV for CLB was <16%. The metabolite inter-day CV was <6%. The accuracy of intra- and inter-day assessments determined for CLB and NDMCLB was within ±10%. This paper describes a rapid, reliable, and simple method for measuring CLB and its metabolite NDMCLB in human plasma. This UV-HPLC procedure offers acceptable precision and accuracy to quantify CLB and its metabolite in human plasma.","PeriodicalId":7829,"journal":{"name":"Analytica","volume":"1224 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2021-07-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"90768974","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}
Pub Date : 2021-05-28DOI: 10.3390/ANALYTICA2030006
J. Nuzillard
The recent revival of the study of organic natural products as renewable sources of medicinal drugs, cosmetics, dyes, and materials motivated the creation of general-purpose structural databases. Dereplication, the efficient identification of already reported compounds, relies on the grouping of structural, taxonomic and spectroscopic databases that focus on a particular taxon (species, genus, family, order…). A set of freely available python scripts, CNMRPredict, is proposed for the quick supplementation of taxon-oriented search results from the LOTUS database (lotus.naturalproducts.net) with predicted carbon-13 NMR data from the ACD/Labs (acdlabs.com) CNMR predictor and DB software to provide easily searchable databases. The database construction process is illustrated using Brassica rapa as taxon example.
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