Assessment method for deamidation in proteins using carboxylic acid derivatization-liquid chromatography-tandem mass spectrometry
Publication date: Available online 3 January 2020Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Shimba Kawasue, Yohei Sakaguchi, Reiko Koga, Hideyuki Yoshida, Hitoshi NohtaAbstractAn analytical method for the degree of protein deamidation has been developed by using carboxy group derivatization and liquid chromatography-tandem mass spectrometry (LC-MS/MS). The fragment peptides (LGEYGFQNALIVR and YNGVFQECCQAEDK) obtained by digesting bovine serum albumin (BSA) with trypsin and their asparagine deamidated peptides (LGEYGFQDALIVR and YDGVFQECCQAEDK) were selected as model peptides, and their carboxy grou...
Source: Journal of Pharmaceutical and Biomedical Analysis - January 7, 2020 Category: Drugs & Pharmacology Source Type: research

Chemical Analysis of Saffron by HPLC based Crocetin Estimation
Publication date: Available online 3 January 2020Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Chilakala Nagarjuna Reddy, Sandip B. Bharate, Ram A. Vishwakarma, Sonali S. BharateAbstractSaffron is one of the most expensive and valuable spice having tremendous commercial value in food industry and thus its quality-check is of utmost importance. Crocins are unique group of extremely hydrophilic apocarotenoids which are main components of saffron. Crocetin is an aglycone of crocins which do occur naturally in saffron, and is produced in biological system as a bioactive-metabolite via hydrolytic cleavage ...
Source: Journal of Pharmaceutical and Biomedical Analysis - January 7, 2020 Category: Drugs & Pharmacology Source Type: research

A sensitive nanocomposite design via carbon nanotube and silver nanoparticles: Selective probing of Emedastine Difumarate
In this study, a novel and sensitive nanocomposite of carboxylate-functionalized multiwalled carbon nanotube (COOH-fMWCNT) and silver nanoparticles (AgNPs) was fabricated and used to modify a glassy carbon electrode (GCE) by a simple drop casting method. Modified electrode was then applied for selective determination of emedastine difumarate (EDD). The COOH-fMWCNT/AgNPs nanocomposite was characterized by electrochemical impedance spectroscopy (EIS), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX) and cyclic voltammetry (CV). EDD showed two oxidation peaks at 0.634 and 1.2 V on the GCE ...
Source: Journal of Pharmaceutical and Biomedical Analysis - January 7, 2020 Category: Drugs & Pharmacology Source Type: research

Development and investigation of a QuEChERS-based method for determination of phthalate metabolites in human milk
Publication date: 20 March 2020Source: Journal of Pharmaceutical and Biomedical Analysis, Volume 181Author(s): Jinyoung An, Ye-Yeong Kim, Hyun-Deok Cho, Junhee Kim, Ji-Youn Lee, Yeoreum Lee, Eunji Jo, Jaeick Lee, Sangwon Cha, Sang Beom HanAbstractPhthalates are commonly used as plasticizers and are known as risk factors toward several conditions such as cancer, birth defects, and endocrine disruption. Biomonitoring of phthalates is necessary to assess the potentially harmful effects of long-term exposure. In this work, we have developed a novel QuEChERS method to determine eight phthalate metabolites—mono-(3-carboxyp...
Source: Journal of Pharmaceutical and Biomedical Analysis - January 7, 2020 Category: Drugs & Pharmacology Source Type: research

Development and validation of a UPLC–MS/MS method for simultaneous determination of vicagrel and its major metabolites in rat or human plasma: An optimized novel strategy for the stabilization of vicagrel
In this study, an optimized strategy was developed and validated to stabilize vicagrel, 2-oxo-clopidogrel (thiolactone metabolite), and H4 (active thiol metabolite) before quantification of the analytes, such as addition of citric acid (for plasma acidification) and NaF (a non-specific esterase inhibitor) to inhibit esterase activity, immediate addition of a thiol-alkylating reagent MPB into blood samples to derivatize H4 for the formation of stable H4 derivative (i.e., MP-H4), use of the anticoagulant K2EDTA to minimize the conversion of 2-oxo-clopidogrel to H-endo, and keeping the analytes at 4 °C or on wet ice to ...
Source: Journal of Pharmaceutical and Biomedical Analysis - January 1, 2020 Category: Drugs & Pharmacology Source Type: research

Enantioselective separation of Novel Psychoactive Substances using a Lux® AMP 3 μm column and HPLC-UV
Publication date: 5 February 2020Source: Journal of Pharmaceutical and Biomedical Analysis, Volume 179Author(s): Johannes S. Hägele, Martina Basrak, Martin G. SchmidAbstractThe abuse of Novel Psychoactive Substances (NPS) still cause severe problems. A lot of them contain a stereogenic centre which leads to possible different pharmacological effects of the enantiomers.The aim of this study was to establish an enantioselective HPLC-UV method with applicability to a broad spectrum of NPS. Different compound classes including mainly amphetamines, cathinones, ketamines, pyrovalerones and benzofuries were tested for succes...
Source: Journal of Pharmaceutical and Biomedical Analysis - January 1, 2020 Category: Drugs & Pharmacology Source Type: research

Metabolomic study of raw and bran-fried Atractylodis Rhizoma on rats with spleen deficiency
This study showed that Atractylodis Rhizoma could provide satisfactory therapeutic effects on spleen deficiency and metabolomics study can be utilized to further understand the molecular mechanisms. (Source: Journal of Pharmaceutical and Biomedical Analysis)
Source: Journal of Pharmaceutical and Biomedical Analysis - December 31, 2019 Category: Drugs & Pharmacology Source Type: research

A quality control system for ligand-binding assay of plasma renin activity: Proof-of-concept within a pharmacodynamic study
Publication date: Available online 28 December 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Fabian Konstantin Suessenbach, Nina Makowski, Martin Feickert, Tanja Gangnus, Jutta Tins, Bjoern Bengt Burckhardt, on behalf of the LENA consortiumAbstractWhile the role of plasma renin activity (PRA) in heart failure have been widely studied in adults, comprehensive data on pediatric heart failure remain lacking. This drawback is increasingly being addressed by academic research. Nevertheless, such pediatric investigations are commonly conducted only once due to ethical constraints. Therefore, the quality...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 29, 2019 Category: Drugs & Pharmacology Source Type: research

Measurement of NLG207 (formerly CRLX101) nanoparticle-bound and released camptothecin in human plasma
Publication date: Available online 27 December 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Keith T. Schmidt, Cody J. Peer, Alwin D.R. Huitema, Monique D. Williams, Susan Wroblewski, Jan H.M. Schellens, Ravi A. Madan, William D. FiggAbstractCamptothecin (CPT), a potent inhibitor of topoisomerase I and HIF-1α, failed to demonstrate utility as an anti-cancer agent in early clinical trial investigations, primarily due to limited clinical activity and significant toxicity attributable to unfavorable physicochemical properties (e.g. low plasma solubility, pH-labile lactone ring). NLG207 (formerl...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 28, 2019 Category: Drugs & Pharmacology Source Type: research

Toxicological effects of some antiparasitic drugs on equine liver glutathione S-Transferase enzyme activity
In this study, we report the effect of some benzimidazole drugs such as ricobendazole (RBZ), thiabendazole (TBZ), albendazole (ALBA) and oxfendazole (OFZ) on glutathione s-transferase (GST) enzyme activity. The kinetics studies, IC50 and Ki values of the tested drugs on GSTs enzyme activity were investigated. The obtained ranking of IC50 values were found to be approximately RBZ (53.31 μM, r2: 0.9778)
Source: Journal of Pharmaceutical and Biomedical Analysis - December 28, 2019 Category: Drugs & Pharmacology Source Type: research

Rapid and highly sensitive quantification of the anti-tuberculosis agents isoniazid, ethambutol, pyrazinamide, rifampicin and rifabutin in human plasma by UPLC-MS/MS
Publication date: Available online 26 December 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Lingjie Wu, Zhenjie Ye, Hui Liu, Hongliang Guo, Jing Lin, Ling Zheng, Nannan Chu, Xiaolong LiuAbstractWith the increased cases of multidrug- or rifampicin-resistant tuberculosis and co-infection with HIV globally, it is difficult to achieve ideal clinical responses because of poor drug absorption and drug-drug interactions. Herein, a bioanalytical UPLC-MS/MS method was developed and validated to quantify five anti-TB agents in human plasma samples for detecting blood drug concentrations to improve therapeu...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 28, 2019 Category: Drugs & Pharmacology Source Type: research

Chemical profiling of Coptis rootlet and screening of its bioactive compounds in inhibiting Staphylococcus aureus by UPLC-Q-TOF/MS
This study proved the utility of the Coptis rootlet, which is beneficial to the more comprehensive utilization of medicinal plant resources.Graphical Abstract (Source: Journal of Pharmaceutical and Biomedical Analysis)
Source: Journal of Pharmaceutical and Biomedical Analysis - December 28, 2019 Category: Drugs & Pharmacology Source Type: research

Metabolomics study to identify Plasma Biomarkers in Alzheimer Disease: ApoE genotype effect
In conclusion, ApoE4 genotype is associated with changes in lipid metabolomics profile in AD patients, and it could be relevant for the development of AD since early stages. (Source: Journal of Pharmaceutical and Biomedical Analysis)
Source: Journal of Pharmaceutical and Biomedical Analysis - December 28, 2019 Category: Drugs & Pharmacology Source Type: research

Recent developments of bioanalytical methods in determination of neurotransmitters in vivo
Publication date: Available online 24 December 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Joanna Matys, Barbara Gieroba, Krzysztof JóźwiakAbstractNeurotransmitters (NTs) constitute an important group of messenger molecules and their imbalance lead to various neurological disorders, making their analytical determination of great importance in both laboratory and clinical practice. Here we review the most recent progress in sample pretreatment and in vivo analysis for various NTs and metabolites focusing on two approaches: biosensors and SPME, which require small amounts of biological sam...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 25, 2019 Category: Drugs & Pharmacology Source Type: research

UPLC–MS/MS method for the simultaneous quantification of bictegravir and 13 others antiretroviral drugs plus cobicistat and ritonavir boosters in human plasma
Publication date: Available online 24 December 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Hélène Gouget, Gaëlle Noé, Aurélie Barrail-Tran, Valérie FurlanAbstractA sensitive and rapid ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method has been developed and validated for 14 antiretroviral drugs and 2 boosters in human plasma. Plasma (100 µL) was precipitated with a solution of acetonitrile containing labelled internal standards. The compounds were separated with a total chromatic run time of 6 min ...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 25, 2019 Category: Drugs & Pharmacology Source Type: research

Circulatory Glutamine/Glucose ratio for evaluating disease activity in Takayasu arteritis: A NMR based serum metabolomics study
Publication date: Available online 24 December 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Umesh Kumar, Avinash Jain, Anupam Guleria, Venkatesh Kumar R, Durga P Misra, Ruchika Goel, Debashish Danda, Ramnath Misra, Dinesh KumarAbstractQuantitative assessment of disease activity is important for effective care of patients with Takayasu arteritis (TA). Activated glutaminolysis and reduced glycolytic flux is the hallmark of active inflammation. Based on this, we hypothesize that the circulatory Glutamine/Glucose ratio (QGR) can serve as an indicant of active inflammation in TA. To probe this hypothe...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 25, 2019 Category: Drugs & Pharmacology Source Type: research

Metabolic profiling of chronic obstructive pulmonary disease model rats and the interventional effects of HuaTanJiangQi decoction using UHPLC-Q-TOF/MSE
Publication date: Available online 24 December 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Wei Fang, ChenHui Li, QingQing Wu, ZhaoMin Yao, Jie Wu, Peng Huang, DianLei Wang, ZeGeng LiAbstractThe occurrence of chronic obstructive pulmonary disease (COPD) will lead to physiological and pathological variations and endogenous metabolic disorders. A traditional Chinese medicine formula, HuaTanJiangQi decoction (HTJQ), exhibits an unambiguous therapeutic effect on COPD in China. Nevertheless, the mechanism of its therapeutic effect on COPD is not clear. With this purpose, pulmonary function, histopatho...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 25, 2019 Category: Drugs & Pharmacology Source Type: research

Simultaneous determination of di(2-ethylhexyl) phthalate and diisononylcyclohexane-1,2-dicarboxylate and their monoester metabolites in four labile blood products by liquid chromatography tandem mass spectrometry
Publication date: Available online 23 December 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Amandine Descat, Marie Lecoeur, Mostafa Kouach, Laurence Goossens, Aurélie Thelliez, Pascal Odou, Bertrand Decaudin, Jean-François GoossensAbstractDi(2-ethylhexyl) phthalate (DEHP) is a common plasticizer that is largely used for PVC blood bags. The migration of DEHP from medical devices into labile blood products (LBP) is a well-known situation. While DEHP has beneficial effects on the storage of red blood cells, it can have toxicological impact due to its potential reprotoxic effects (class...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 25, 2019 Category: Drugs & Pharmacology Source Type: research

Characterization of chemical profile and quantification of representative components of DanLou tablet, a traditional Chinese medicine prescription, by UHPLC-Q/TOF-MS combined with UHPLC-TQ-MS
Publication date: Available online 23 December 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Pei Lin, Qi Wang, Yuehe Liu, Zifei Qin, Hao Gao, Min Ye, Hongcai Shang, Xinsheng Yao, Zhihong YaoAbstractDanLou tablet (DLT), a famous traditional Chinese medicine prescription (TCMP) consisting of 10 herbal medicines, is extensively used for the treatment of angina pectoris and acute coronary syndrome in China. However, active chemical constituents responsible for the therapeutic effects still remains unclear, due to the fact that the complex composition in DLT have not been holistically clarified. Theref...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 25, 2019 Category: Drugs & Pharmacology Source Type: research

Metabolic and lipidomic characterization of malignant pleural effusion in human lung cancer
The objective of this study was to characterize the metabolic signatures in MPE of lung cancer, and identify potential metabolite biomarkers for diagnosis of MPE. MPE from lung cancer (n = 46) and BPE from tuberculosis patients (n = 32) were investigated by liquid chromatography-tandem mass spectrometry (LC-MS/MS)-based global metabolomic and lipidomic profiling. Multivariate partial least-square discriminative analysis models exhibited distinct metabolic profiles between MPE and BPE. A total of 25 ether lipids, including phosphatidylcholines (PC), lysophosphatidylcholines (LPC) and phosphatidyl...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 25, 2019 Category: Drugs & Pharmacology Source Type: research

LC-ESI-MS/MS Assay Development and Validation of a Novel Antidiabetic Peptide PSTi8 in Mice Plasma using SPE: an Application to Pharmacokinetics
Publication date: Available online 23 December 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Guru R. Valicherla, Mohammed Riyazuddin, Sudhir Shahi, Anand P. Gupta, Anees A. Syed, Athar Husain, Jiaur R. GayenAbstractPSTi8 is a 21 amino acid pancreastatin inhibitory peptide that demonstrated potent antidiabetic activity in insulin resistant rodent models. The goal of the current work is to establish and validate the LC-ESI-MS/MS bioanalytical assay of PSTi8 in mice plasma in order to unveil its pharmacokinetic (PK) behaviour for the first time. The MS detection of PSTi8 and diprotin A (internal stan...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 25, 2019 Category: Drugs & Pharmacology Source Type: research

Using HPLC to analyze (S)-oxiracetam and four related substances in the bulk drug of (S)-oxiracetam
Publication date: Available online 23 December 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Chao Wang, Hong Dong, Honghui Liu, Zhaoyi Sun, Ahu Yuan, Jinhui Wu, Yiqiao HuAbstract(S)-oxiracetam is undergoing clinical trials as an active ingredient in the racemic oxiracetam. Here, we report a specific analytical method for analyzing (S)-oxiracetam and four related impurities in the bulk drug of (S)-oxiracetam by using high-performance liquid chromatography (HPLC) system. The chromatographic system included a Capcell pak NH2 analytical column, a mobile phase containing acetonitrile-water (95:5, v/v; ...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 25, 2019 Category: Drugs & Pharmacology Source Type: research

Thermal shift assay: Strengths and weaknesses of the method to investigate the ligand-induced thermostabilization of soluble guanylyl cyclase
Publication date: Available online 23 December 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Christin Elgert, Anne Rühle, Peter Sandner, Sönke BehrendsAbstractThermal shift assay is a fluorescence dye based biochemical method to determine the melting point of a protein. It can be used to investigate the ligand-induced stabilization of proteins and helps to increase the likelihood of crystallization in biological samples. Dimeric proteins like soluble guanylyl cyclase (sGC) have specific structural and functional properties which may pose a challenge in thermal shift measurements. In this...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 25, 2019 Category: Drugs & Pharmacology Source Type: research

Spectrofluorimetric cytosensing of colorectal cancer cells using terbium-doped dendritic fibrous nano-silica functionalized by folic acid
Publication date: Available online 23 December 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Jafar Soleymani, Mohammad Hasanzadeh, Nasrin Shadjou, Mohammad Hossein Somi, Abolghasem JouybanAbstractA novel fluorescent probe for detection of HT 29 cancer cells was developed based on terbium-doped dendritic fibrous nanosilica functionalized by folic acid (Tb@KCC-1-NH2-FA). Using this probe, fluorescence signals was emitted by Tb@KCC-1-NH2-FA at 490 nm by applying 380 nm as excitation wavelength. The reported probe is based on the interaction between FA decorated on the surface of Tb@KCC...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 25, 2019 Category: Drugs & Pharmacology Source Type: research

Untargeted Metabolomics Reveals novel serum biomarker of Renal Damage in Rheumatoid Arthritis
Publication date: Available online 23 December 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Lili Song, Qingshen Yin, Mingqin Kang, Ningning Ma, Xin Li, Zhen Yang, Hua Jin, Mengya Lin, Pengwei Zhuang, Yanjun ZhangABSTRACTRheumatoid arthritis (RA) is a chronic progressive disease, it often involves kidney, lung, heart, and other systems.Renal damage is quite common in RA. Exploring of biomarkers of renal damage in the course of RA progression is of significant importance for disease diagnosis and treatment. We use type II Collagen-Induced Arthritis(CIA) Model. Serums were collected at the 4th, 6th,...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 25, 2019 Category: Drugs & Pharmacology Source Type: research

Optimized one-pot derivatization and enantioseparation of cysteine: application to the study of a dietary supplement
Publication date: Available online 23 December 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Lucia Pucciarini, Giorgio Saluti, Roberta Galarini, Andrea Carotti, Antonio Macchiarulo, Serge Rudaz, Roccaldo SardellaAbstractCysteine is a sulfur-containing amino acid which plays an outstanding role in many biological pathways in mammals. The analysis and quantification of native cysteine remains a critical issue due to its highly reactive thiol group evolving to the disulfide cystine derivative through oxidation reaction. Aimed at improving the derivative stability, cysteine was labelled with 4-fluoro-...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 25, 2019 Category: Drugs & Pharmacology Source Type: research

Drug-gut microbiota metabolic interactions: The case of UniPR1331, selective antagonist of the Eph-ephrin system, in mice
Publication date: Available online 23 December 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Francesca Ferlenghi, Riccardo Castelli, Laura Scalvini, Carmine Giorgio, Miriam Corrado, Massimiliano Tognolini, Marco Mor, Alessio Lodola, Federica VacondioAbstractThe interest on the role of gut microbiota in the biotransformation of drugs and xenobiotics has grown over the last decades and a deeper understanding of the mutual interactions is expected to help future improvements in the fields of drug development, toxicological risk assessment and precision medicine. In this paper, a microbiome drug metab...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 25, 2019 Category: Drugs & Pharmacology Source Type: research

The elution behavior of cyclosporine congeners in a developed HPLC system reflects the lipophilicity
Publication date: Available online 23 December 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Kumiko Sakai-Kato, Kohki YoshidaAbstractRecently, the development of cyclic peptide drugs has accelerated. To develop an analytical method to determine the physicochemical properties of these lipophilic drug candidates, we investigated the separation mechanism of cyclosporine congeners A, B, C, and D using HPLC with a column packed with 2-μm nonporous octadecylsilyl silica particles at high temperature. The four congeners were eluted with good repeatability in terms of retention time, peak area, and the...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 25, 2019 Category: Drugs & Pharmacology Source Type: research

Zirconium metal-organic framework assisted miniaturized solid phase extraction of phenylurea herbicides in natural products by ultra-high-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry
Publication date: Available online 23 December 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Qiu-Yan Wang, Juan Yang, Xin Dong, Yan Chen, Li-Hong Ye, Yu-Han Hu, Hui Zheng, Jun CaoAbstractThe zirconium metal-organic framework (Zr-MOF) was used as a novel and effective adsorbent material for the enrichment of five phenylurea herbicides (fenuron, monuron, diuron, linuron and pencycuron) in Dendrobii Officinalis Caulis, Salviae Miltiorrhizae Radix et Rhizoma and Hawthorn samples. The target analytes were determined by ultra-high-performance liquid chromatography coupled with quadrupole time-of-flight ...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 25, 2019 Category: Drugs & Pharmacology Source Type: research

Near infrared analysis of pharmaceutical powders with empirical target distribution optimization (ETDO)
Publication date: Available online 20 December 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Troels Pedersen, Jukka Rantanen, Kaisa Naelapää, Erik SkibstedAbstractNear infrared (NIR) spectroscopy is a well-established method for analysis of pharmaceutical products, and especially useful for process monitoring and control of continuous production due to high sample throughput. In this work, a previously established method called empirical target distribution optimization (ETDO) wherein reference sample values using information from model prediction of the calibration data was used as a to...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 21, 2019 Category: Drugs & Pharmacology Source Type: research

The role of solid state properties on the dissolution performance of flufenamic acid
Publication date: Available online 20 December 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Francesca Maestrelli, Patrizia Rossi, Paola Paoli, Enrico De Luca, Paola MuraAbstractFlufenamic acid is a nonsteroidal anti-inflammatory drug characterized by a low solubility and a variable oral bioavailability. Flufenamic acid is present in the commercial products in two polymorphic enantiotropic forms (Form I and III). Bioinequivalence was observed for commercial solid dosage forms due to the different dissolution rate of batches. Aim of this work is the full characterization of the solid state properti...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 21, 2019 Category: Drugs & Pharmacology Source Type: research

Relationship between cancer tissue derived and exhaled volatile organic compound from colorectal cancer patients. Preliminary results
In conclusion, these preliminary data suggest the involvement of the three compounds in CRC by encouraging further investigation.Graphical abstract (Source: Journal of Pharmaceutical and Biomedical Analysis)
Source: Journal of Pharmaceutical and Biomedical Analysis - December 21, 2019 Category: Drugs & Pharmacology Source Type: research

The relationship between serum clozapine concentrations and hematological parameters by a validated mass spectrometric method
ConclusionsThis LC-MS/MS method was rapid, simple, cost-effective and suitable for the routine clozapine monitoring. Furthermore, norclozapine and clozapine-N-oxide were also determined. Monitoring of metabolic and hematological parameters with clozapine levels is very important. However, the limitations of the study were that the method was not validated for norclozapine and clozapine-N-oxide, so the validation parameters were not evaluated for these two metabolites. (Source: Journal of Pharmaceutical and Biomedical Analysis)
Source: Journal of Pharmaceutical and Biomedical Analysis - December 21, 2019 Category: Drugs & Pharmacology Source Type: research

An enantiomeric quantitative LC-MS/MS method for tolvaptan and its monohydroxylates in human plasma using a reversed-phase separation procedure
In conclusion, the present method has an acceptable analytical performance level and can be helpful for characterization of the plasma 5R- and 5S-tolvaptan and their monohydroxylate enantiomers in heart failure patients.Graphical abstract (Source: Journal of Pharmaceutical and Biomedical Analysis)
Source: Journal of Pharmaceutical and Biomedical Analysis - December 21, 2019 Category: Drugs & Pharmacology Source Type: research

Identification of quality control markers in Suhuang antitussive capsule based on HPLC-PDA fingerprint and anti-inflammatory screening
The objective of this work is to identify the characteristic and active ingredients as the quality control markers for SH based on high performance liquid chromatography with photodiode array detector (HPLC-PDA) fingerprint and screening of anti-inflammatory components. Similarity analysis (SA), hierarchical clustering analysis (HCA) and principal component analysis (PCA) were used to evaluate 16 different batches of SH. 13 compounds accounting for 36% of the total components in the fingerprint were identified and semi-quantitatively analyzed, which anti-inflammatory activity was tested with the in vitro assay. The results...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 21, 2019 Category: Drugs & Pharmacology Source Type: research

Lifecycle management in pharmaceutical analysis: How to establish an efficient and relevant continued performance monitoring program
Publication date: Available online 19 December 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Joachim Ermer, Debora Aguiar, Annette Boden, Bei Ding, Daniel Obeng, Michael Rose, Julie VokrotAbstractIt is the objective of a systematic and holistic Quality-by-Design approach to demonstrate and ensure that an analytical procedure is fit for its intended purpose over its entire lifecycle. Such a lifecycle approach, as proposed for a new USP General Information Chapter includes the three stages Procedure Design and Development, Procedure Performance Qualification, and Continued Procedure Performance Veri...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 21, 2019 Category: Drugs & Pharmacology Source Type: research

pDNA conjugated with citrate capped silver nanoparticles towards ultrasensitive bio-assay of Haemophilus influenza in human biofluids
In this study, citrate capped silver nanoparticle was synthesized and employed for bioconjugation with pDNA toward target sequences detection. In this study, synthesized probe (SH-5'-AAT TTT CCA ACT TTT TCA CCT GCA T-3') of Haemophilus influenza was detected with great sensitivity and selectivity after hybridization with cDNA (5'-ATG CAG GTG AAA AAG TTG GAA AAT T-3'). Regarding to the obtained results, the low limit of quantification (LLOQ) of DNA sample was 1 ZM using 15 µL of probe and 200 µL of Cit/AgNPs. According to ultra-sensitivity of the fabricated optical DNA-based bio-assay, it ha...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 21, 2019 Category: Drugs & Pharmacology Source Type: research

Attenuated total reflection Fourier transform infrared spectroscopy based methods for identification of chromatography media formulations used in downstream processes
In this study, chromatographic media formulations used in downstream processes were investigated using attenuated total reflection Fourier transform infrared (ATR FT-IR) spectroscopy. Samples were measured both in original suspension form and after drying to examine the possibilities of a potential spectroscopic method without sample preparation. Principal component analysis (PCA) was employed to identify the spectral differences among the formulations with distinct support matrices and functional groups and soft independent modeling of class analogy (SIMCA) was performed to creating classification models for identificatio...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 21, 2019 Category: Drugs & Pharmacology Source Type: research

Boron and Nitrogen Codoped Carbon Dots as Fluorescence Sensor for Fe3+ with Improved Selectivity
In this study, we suspect that sp3 boron atom in phenylboronic acid group will be more compatible with Fe3+ to form coordination bonds, thereby increasing the selectivity to Fe3+. Hence, we designed and synthesized boron and nitrogen codoped carbon dots (BN-CDs) for detection of Fe3+ via a hydrothermal method using o-phenylenediamine (OPA) and 4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzylchloroformate as precursors. From the results, we found that BN-CDs had superior selectivity to Fe3+ in the presence of the other common interfering metal ions like Cu2+, Fe2+ and Pb2+. Besides, the obtained BN-CDs exhibited good w...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 21, 2019 Category: Drugs & Pharmacology Source Type: research

Method transfer of a near-infrared spectroscopic method for blend uniformity in a poorly flowing and hygroscopic blend
Publication date: Available online 20 December 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Bárbara B. Alvarado-Hernández, James V. Scicolone, Carlos Ortega-Zuniga, Andrés D. Román-Ospino, Yleana M. Colón, Efrain Aymat, Eric Sánchez, Fernando J. Muzzio, Rodolfo J. RomañachAbstractThe challenges in transferring and executing a near-infrared (NIR) spectroscopic method for croscarmellose (disintegrant) in binary blends for a continuous manufacturing (CM) process are presented. This work demonstrates the development of a NIR calibration model and its u...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 21, 2019 Category: Drugs & Pharmacology Source Type: research

Ketamine analogues: Comparative toxicokinetic in vitro–in vivo extrapolation and quantification of 2-fluorodeschloroketamine in forensic blood and hair samples
This study reports quantification of 2FDCK in whole blood samples and forensic hair and compares the following toxicokinetic parameters: unbound fraction (fu) and in vitro–in vivo-extrapolation (IVIVE) of hepatic clearance for ketamine, norketamine, 2FDCK, methoxetamine and deschloroketamine. The fu was investigated with ultrafiltration, while clearance studies were conducted at 1 µM with pooled human liver microsomes. Samples were analysed by liquid chromatography and mass spectrometry. For the first time, 2FDCK was determined in a concentration range between 0.005 and 0.48 mg/kg in blood samples. Segme...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 19, 2019 Category: Drugs & Pharmacology Source Type: research

Development of an on-line immobilized α-glucosidase microreactor coupled to liquid chromatography for screening of α-glucosidase inhibitors
Publication date: Available online 17 December 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Beibei Qiu, Yuqiong Shi, Luyun Yan, Xiangrong Wu, Jinhua Zhu, Dongbao Zhao, Zaved H. Khan, Xiuhua LiuAbstractIn order to rapidly screen α-glucosidase (α-GLU) inhibitors from Chinese herbs extract, an online screening method was developed by using enzymatic microreactors in combination with HPLC. A type of dodecahedral and porous material (ZIF-90) was synthesized at room temperature and employed as supports to construct enzymatic microreactor. The amount of α-glucosidase immobilized on ZIF...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 18, 2019 Category: Drugs & Pharmacology Source Type: research

Toxicological Effects of Some Antiparasitic Drugs on From Equine Liver Glutathione S-Transferase Enzyme Activity
In this study, we report the effect of some benzimidazole drugs such as ricobendazole (RBZ), thiabendazole (TBZ), albendazole (ALBA) and oxfendazole (OFZ) on glutathione s-transferase (GST) enzyme activity. The kinetics studies, IC50 and Ki values of the tested drugs on GSTs enzyme activity were investigated. The obtained ranking of IC50 values were found to be approximately RBZ (53.31 µM, r2: 0.9778)
Source: Journal of Pharmaceutical and Biomedical Analysis - December 18, 2019 Category: Drugs & Pharmacology Source Type: research

Determination of buprenorphine, naloxone and phase I and phase II metabolites in rat whole blood by LC-MS/MS
Publication date: Available online 16 December 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Camille Cohier, Sophie Salle, Anne Fontova, Bruno Mégarbane, Olivier RousselAbstractBuprenorphine and buprenorphine/naloxone combination are maintenance treatments used worldwide. However, since their marketing, despite ceiling respiratory effects, poisonings and fatalities have been attributed to buprenorphine misuse and overdose. Therefore, to better understand the mechanisms of buprenorphine-related toxicity in vivo, experimental investigations have been conducted, mainly in the rat. We developed...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 18, 2019 Category: Drugs & Pharmacology Source Type: research

Metabolic profiling of tyrosine kinase inhibitor nintedanib using metabolomics
This study provided a global view of nintedanib metabolism, which could be used to understand the mechanism of adverse effects related to nintedanib and its potential drug-drug interaction. (Source: Journal of Pharmaceutical and Biomedical Analysis)
Source: Journal of Pharmaceutical and Biomedical Analysis - December 18, 2019 Category: Drugs & Pharmacology Source Type: research

A novel UPLC/MS/MS method for rapid determination of murrayone in rat plasma and its pharmacokinetics
Publication date: Available online 16 December 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Shengyi Zhai, Xiaoxiao Deng, Chen Zhang, Yu Zhou, Huanzhang Xie, Zhou Jiang, Lee JiaAbstractMurraya paniculata (L.) is a traditional Chinese medicine (TCM) wildly grown in southeast China, and used for abortion in folk. Murrayone, a coumarin-containing compound extracted from M. paniculata, is the most bioactive substance in this species and is being developed as a novel cancer metastasis chemopreventive agent based on its unique pharmacological properties. In the present study, a novel rapid and sensitive...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 18, 2019 Category: Drugs & Pharmacology Source Type: research

Development, validation and application of LC–MS/MS method for quantification of amino acids, kynurenine and serotonin in human plasma
Publication date: 20 February 2020Source: Journal of Pharmaceutical and Biomedical Analysis, Volume 180Author(s): Dávid Virág, Márton Király, László Drahos, Andrea Edit Édes, Kinga Gecse, György Bagdy, Gabriella Juhász, István Antal, Imre Klebovich, Borbála Dalmadi Kiss, Krisztina LudányiAbstractAltered serotonergic neurotransmission is a key factor in several neurologic and psychiatric disorders such as migraine. Human and animal studies suggest that chronically low interictal serotonin levels of plasma and brain may facilitate increased act...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 16, 2019 Category: Drugs & Pharmacology Source Type: research

Development and validation of an LC-MS/MS method for the quantification of goserelin in a Pheroid® formulation simulated intestinal fluid
Publication date: Available online 12 December 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): John Takyi-Williams, Linnè Erasmus, Rose Hayeshi, Anne GroblerAbstractThe purpose of this reported study was to develop and validate an LC-MS/MS method for the quantification of goserelin in a Pheroid® formulation simulated intestinal fluid. Biopharmaceuticals are formulated in drug delivery systems to improve their gastrointestinal stability. Goserelin, a peptide drug was formulated in Pheroid® delivery system and its gastrointestinal stability assessed using simulated intestinal fluid, whi...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 13, 2019 Category: Drugs & Pharmacology Source Type: research

Development and validation of an LC-MS/MS method for the quantitative analysis of the anti-influenza agent camphecene in rat plasma and its application to study the blood-to-plasma distribution of the agent
Publication date: Available online 10 December 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Alina A. Okhina, Artem D. Rogachev, Olga I. Yarovaya, Mikhail V. Khvostov, Tatyana G. Tolstikova, Andrey G. Pokrovsky, Veniamin A. Khazanov, Nariman F. SalakhutdinovAbstractA method of quantitative determination of camphecene, a new anti-influenza agent, in rat blood plasma based on LC-MS/MS was developed, validated and used to study the distribution of the agent between blood cells and blood plasma. The method was validated according to FDA and EMA recommendations in terms of selectivity, linearity, accur...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 12, 2019 Category: Drugs & Pharmacology Source Type: research

Development of a Mass Spectrometry-Based Pseudotargeted Metabolomics strategy to analyze Hormone-Stimulated Gastric Cancer Cells
Publication date: Available online 10 December 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Juan Li, Qingli Wang, Yichao Zheng, Piao Zhou, Xia Xu, Xueqi Liu, Longfei Zhao, Hongmin LiuAbstractGastric cancer (GC) is the third most common cause of cancer death worldwide, and the incidence of GC is higher in males than females. To investigate the gastric cellular response to hormone therapy, we developed a cell pseudotargeted metabolomics method based on liquid chromatography-hybrid triple quadrupole linear ion trap mass spectrometry (LC-QTRAP MS). Chromatographic separation, sample analysis and meta...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 12, 2019 Category: Drugs & Pharmacology Source Type: research