Enhancing online protein isolation as intact species from soy flour samples by actively modulated two-dimensional liquid chromatography (2D-LC)
In this study, an enhanced fully automated approach is described for the protein isolation from soy flour samples by two-dimensional liquid chromatography with active modulation interface. The use of two multi-port switching valves is proposed to on-line connect the first to the second dimension column, thus overcoming the problems associated with the re-mixing effects and incompatibility of eluent composition and pH. A 5-cm long C4 analytical column installed in the interface device allows to focus the proteins coming from the first column (size exclusion chromatography), before their selective elution in the second colum...
Source: Journal of Pharmaceutical and Biomedical Analysis - November 8, 2019 Category: Drugs & Pharmacology Source Type: research

Stability in clinical use and stress testing of meropenem antibiotic by direct infusion ESI-Q-TOF: Quantitative method and identification of degradation products
Publication date: Available online 6 November 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Fábio de Souza Barbosa, Leonardo Capra Pezzi, Marisa Tsao, Sandra Manoela Dias Macedo, Tiago Franco de Oliveira, Elfrides E.S. Schapoval, Andreas S.L. MendezAbstractAn ESI-MS/MS method through direct infusion was validated for quantitative analysis of meropenem powder for injection. The validation parameters were established in a rapid analysis of 30 s. Drug stability was studied through the submission to stress testing, resulting on four degradation products. Under hydrolytic conditions, in a...
Source: Journal of Pharmaceutical and Biomedical Analysis - November 7, 2019 Category: Drugs & Pharmacology Source Type: research

Determination and pharmacokinetic study of skimmin by UHPLC-MS/MS in rat plasma
This study will be beneficial in better understanding the pharmacological properties and the further development of skimmin.Graphical abstract (Source: Journal of Pharmaceutical and Biomedical Analysis)
Source: Journal of Pharmaceutical and Biomedical Analysis - November 7, 2019 Category: Drugs & Pharmacology Source Type: research

Pharmacokinetics and pharmacodynamics analysis of XQ-1H and its combination therapy with clopidogrel on cerebral ischemic reperfusion injury in rats
In this study, we established an UPLC-MS/MS spectrometry method for the determination of XQ-1H and investigated the pharmacokinetic effect of clopidogrel on XQ-1H in rats subjected to middle cerebral artery occlusion (MCAO). Meanwhile, the anti-apoptotic and neuroprotective effects of XQ-1H and its combination with clopidogrel were also studied. The results revealed that XQ-1H and its combination with clopidogrel abridged brain infarct volume, cerebral edema and alleviated neurological dysfunction caused by cerebral ischemic reperfusion injury. Further study demonstrated that XQ-1H combined with clopidogrel lessened TUNEL ...
Source: Journal of Pharmaceutical and Biomedical Analysis - November 7, 2019 Category: Drugs & Pharmacology Source Type: research

Improving diagnosis of genitourinary cancers: Biomarker discovery strategies through mass spectrometry-based metabolomics
Publication date: 30 January 2020Source: Journal of Pharmaceutical and Biomedical Analysis, Volume 178Author(s): Malena Manzi, Gabriel Riquelme, Nicolás Zabalegui, María Eugenia MongeAbstractThe genitourinary oncology field needs integration of results from basic science, epidemiological studies, clinical and translational research to improve the current methods for diagnosis. MS-based metabolomics can be transformative for disease diagnosis and contribute to global health parity. Metabolite panels are promising to translate metabolomic findings into the clinics, changing the current diagnosis paradigm based ...
Source: Journal of Pharmaceutical and Biomedical Analysis - November 7, 2019 Category: Drugs & Pharmacology Source Type: research

Development of a sensitive LC-MS/MS method for quantification of linezolid and its primary metabolites in human serum
In this study, we established the first liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the simultaneous quantification of LZD and its main metabolites in human serum. Proteins in serum samples were precipitated with acetonitrile containing a deuterated internal standard. Chromatographic separation of analytes was performed with Waters X-bridge column (C18, 150 x 4.6 mm, 3.5 μm) at 25 °C and subjected to mass analysis using positive electro-spray ionization. The mobile phase A was water with 0.1% formic acid, and mobile phase B was acetonitrile with 0.1% formic...
Source: Journal of Pharmaceutical and Biomedical Analysis - November 7, 2019 Category: Drugs & Pharmacology Source Type: research

Enantioselective separation of Novel Psychoactive Substances using a Lux® AMP 3 μm column and HPLC-UV
Publication date: Available online 5 November 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(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 s...
Source: Journal of Pharmaceutical and Biomedical Analysis - November 7, 2019 Category: Drugs & Pharmacology Source Type: research

A Double Surrogate Approach for the Quantitation of 2-Hydroxyglutarate – an Oncometabolite in Human Brain Tumors via LC-MS/MS
Publication date: Available online 4 November 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Feng Yin, Jennifer Keller, Dennis Kraus, Heidi Mangus, Fumin Li, Guowen LiuAbstractWe are reporting a validated LC-MS/MS assay for the quantitation of 2-Hydroxyglutarate (2-HG), an endogenous oncometabolite, in human brain tumors. To address the challenges of endogenous levels of 2-HG in biological matrix and the limited availability of human brain tumors, a surrogate analyte in conjunction with a surrogate matrix approach was used (stable isotope labeled 2-HG in monkey brain homogenate). Human brain tumor ...
Source: Journal of Pharmaceutical and Biomedical Analysis - November 6, 2019 Category: Drugs & Pharmacology Source Type: research

Synthesis and Characterization of Reishi Mushroom-mediated Green Synthesis of Silver Nanoparticles for the Biochemical Applications
In this study, silver nanoparticles (Ag NPs) were synthesized using reishi mushroom (Ganoderma lucidum) extract. Different analytical techniques including X-ray Photoelectron Spectroscopy (XPS), X-ray diffraction (XRD), transmission electron microscopy (TEM), UV–vis spectroscopy, and Fourier Transform Infrared Spectrophotometer (FTIR) were used for the characterization of Ag NPs. Uv-Vis spectrum exhibited a broad absorption peak between 400-460 nm which indicates the existence of Ag NPs. TEM images showed Ag NPs are spherical with a diameter range of 15-22 nm. In addition, it is shown that Ag NPs form a...
Source: Journal of Pharmaceutical and Biomedical Analysis - November 6, 2019 Category: Drugs & Pharmacology Source Type: research

Identification of UDP-glucuronosyltransferases involved in the metabolism of silymarin flavonolignans
This study was designed to identify UDP-glucuronosyltransferases (UGTs) involved in the glucuronidation of six silymarin flavonolignans, namely silybin A, silybin B, isosilybin A, isosilybin B, silychristin, and silydianin. UHPLC-MS analyses showed that all of the tested compounds, both individually and in silymarin, were glucuronidated by human liver microsomes, and that glucuronidation was the main metabolic transformation in human hepatocytes. Further, each compound was glucuronidated by multiple recombinant human UGT enzymes. UGTs 1A1, 1A3, 1A8 and 1A9 were able to conjugate all of the tested flavonolignans, and some o...
Source: Journal of Pharmaceutical and Biomedical Analysis - November 6, 2019 Category: Drugs & Pharmacology Source Type: research

Simultaneous determination of elbasvir and grazoprevir in fixed-dose combination and mass spectral characterization of each degradation product by UHPLC-ESI-QTOF-MS/MS
Publication date: Available online 3 November 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Liqin Chen, Junli Chen, Mingqiu Lu, Andreas StämpfliAbstractZepatier® (Elbasvir and Grazoprevir) is a novel two-drug, fixed-dose combination product containing elbasvir and grazoprevir used for the treatment of chronic hepatitis C virus infection. Various forced degradation studies of the two drugs had been conducted in order to identify significant degradation products and establish the degradation pathway induced by thermal, photolytic, acid/base hydrolytic and/or oxidative stress conditions. A r...
Source: Journal of Pharmaceutical and Biomedical Analysis - November 4, 2019 Category: Drugs & Pharmacology Source Type: research

Why should the pharmaceutical industry claim for the implementation of second-order chemometric models - a critical review
Publication date: Available online 4 November 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Silvana E. Vignaduzzo, Rubén M. Maggio, Alejandro C. OlivieriAbstractToday, pharmaceutical products are submitted to a large number of analytical tests, planned to either ensure or construct their quality. The official methods of analysis used to perform these determinations are very different in nature, but almost all demand the intensive use of reagents and manpower as major drawbacks. Thus, analytical development is continuously evolving to find fast and smart approaches. First-order chemometric m...
Source: Journal of Pharmaceutical and Biomedical Analysis - November 4, 2019 Category: Drugs & Pharmacology Source Type: research

Interaction of novel Aurora kinase inhibitor MK-0457 with human serum albumin: Insights into the dynamic behavior, binding mechanism, conformation and esterase activity of human serum albumin
This study is beneficial for understanding the biological action of MK-0457, providing additional information about the feasibility of its transport and accumulation in blood plasma.Graphical abstractIn-vitro assessment of the binding properties of MK-0457, a novel Aurora kinase inhibitor, with human serum albumin: computer simulations in combination with multi-spectroscopic, esterase activity and microscopic studies. (Source: Journal of Pharmaceutical and Biomedical Analysis)
Source: Journal of Pharmaceutical and Biomedical Analysis - November 4, 2019 Category: Drugs & Pharmacology Source Type: research

Biogenic Platinum Nanoparticles using Black Cumin Seed and Their Potential Usage as Antimicrobial and Anticancer Agent
Publication date: Available online 2 November 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Aysenur Aygun, Fulya Gülbagca, Lutfiye Yildiz Ozer, Buket Ustaoglu, Yasemin Celik Altunoglu, Mehmet Cengiz Baloglu, Mehmet Nuri Atalar, Mehmet Hakkı Alma, Fatih SenAbstractHerein, the biogenic platinum nanoparticles (Pt NPs) were synthesized by using black cumin seed (Nigella sativa L.) extract as a reducing agent. The biogenic platinum nanoparticles synthesized by black cumin seed extract was characterized in detail by Transmission Electron Microscopy (TEM), UV-Vis spectrophotometer, X-ray diffractio...
Source: Journal of Pharmaceutical and Biomedical Analysis - November 4, 2019 Category: Drugs & Pharmacology Source Type: research

Development of a mass spectrometric screening assay for hepatitis B virus entry inhibitors
Publication date: Available online 3 November 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Byoungsook Goh, Jieun Choi, Jung-Ah Kang, Sung-Gyoo Park, Jiwon Seo, Tae-Young KimAbstractSodium taurocholate cotransporting polypeptide (NTCP) involved in bile acid transport in the liver is an entry receptor of hepatitis B virus (HBV). In the present study, we introduce a mass spectrometric screening assay for targeting HBV entry inhibitors that can reduce NTCP transporter activity by employing taurocholic acid (TCA) labeled with stable isotope (2,2,4,4-d4-TCA, d4-TCA) and NTCP-overexpressing human liver ...
Source: Journal of Pharmaceutical and Biomedical Analysis - November 4, 2019 Category: Drugs & Pharmacology Source Type: research

Metabolic impact of partial hepatectomy in the non-alcoholic steatohepatitis animal model of methionine-choline deficient diet
The objective of the present study was to gain deeper knowledge about the metabolic processes involved in the NASH animal model, and particularly in the effect of PH by using metabolomics. For achieving such information, twelve 8-week-old male C57BL/6 J mice, fed commercial chow (control diet) or methionine and choline-Deficient diet (MCD) for three weeks were subjected to PH and sacrificed 2 weeks later. Livers were removed and submitted to metabolic profiling analysis through RP-LC/MS (qTOF), GC/MS (qTOF) and CE/MS(TOF). More than 3000 different features were detected and repeated measurements one-way ANOVA analys...
Source: Journal of Pharmaceutical and Biomedical Analysis - November 2, 2019 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 ic...
Source: Journal of Pharmaceutical and Biomedical Analysis - November 2, 2019 Category: Drugs & Pharmacology Source Type: research

A novel and sensitive HILIC-CAD method for glucosamine quantification in plasma and its application to a human pharmacokinetic study
Publication date: Available online 31 October 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Chhavi Asthana, Gregory M. Peterson, Madhur D. Shastri, Rahul P. PatelAbstractThe clinical effect of glucosamine, the most widely used supplement in patients with osteoarthritis, on joint pain and function improvement, is reported to be inconsistent. Inter-patient variability in the pharmacokinetics of glucosamine, especially its oral absorption, could contribute to the inconsistent clinical outcomes. To test this hypothesis, a novel but simple Hydrophilic Interaction Liquid Chromatography coupled with Char...
Source: Journal of Pharmaceutical and Biomedical Analysis - November 2, 2019 Category: Drugs & Pharmacology Source Type: research

Biomedical analysis of New Psychoactive Substances (NPS) of natural origin
Publication date: Available online 30 October 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Alfredo Fabrizio Lo Faro, Annagiulia Di Trana, Nunzia La Maida, Adriano Tagliabracci, Raffaele Giorgetti, Francesco Paolo BusardòAbstractNew psychoactive substances (NPS) can be divided into two main groups: synthetic molecules and active principles of natural origin. With respect to this latter group, a wide range of alkaloids contained in plants, mainly from Asia and South America, can be included in the class of NPS of natural origin. The majority NPS of natural origin presents stimulant and/or ha...
Source: Journal of Pharmaceutical and Biomedical Analysis - October 31, 2019 Category: Drugs & Pharmacology Source Type: research

Post-column infused internal standard assisted lipidomics profiling strategy and its application on phosphatidylcholine research
Publication date: Available online 30 October 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Hsiao-Wei Liao, Ching-Hua Kuo, Hsi-Chun Chao, Guan-Yuan ChenAbstractVarious lipidomics studies have revealed the potential of using phospholipids as disease biomarkers for conditions such as Alzheimer’s disease, cancer, and sepsis. Establishing accurate quantification methods for targeted phospholipid analysis is important for making these potential markers more clinically relevant. Although a stable isotope labelled-internal standard method can provide good quantification accuracy for endogenous meta...
Source: Journal of Pharmaceutical and Biomedical Analysis - October 31, 2019 Category: Drugs & Pharmacology Source Type: research

The occurrence and exposure risk assessment of psychoactive drug residues and metabolites in aquatic environment
Publication date: Available online 31 October 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): D.P. Masemola, E.N. Nxumalo, H. Nyoni, TTI Nkambule, B.B Mamba, T.A.M. MsagatiAbstractIncreased use of psychoactive drugs and their continuous release into the aquatic environment threatens the aquatic life, human and animal’s life. As such this study was aimed at investigating the occurrence and the associated exposure human health risks of psychoactive drugs residues. The psychoactive drugs investigated include amphetamine, methylphenidate, heroin, cocaine and metabolites included are mainly morphin...
Source: Journal of Pharmaceutical and Biomedical Analysis - October 31, 2019 Category: Drugs & Pharmacology Source Type: research

An electrochemical signal-on apta-cyto-sensor for quantitation of circulating human MDA-MB-231 breast cancer cells by transduction of electro-deposited non-spherical nanoparticles of gold
Publication date: Available online 28 October 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): S. Akhtartavan, M. Karimi, N. Sattarahmady, H. HeliAbstractA highly simple, sensitive, specific and low-cost electrochemical apta-cyto-sensor for determination of circulating human MDA-MB-231 breast cancer cells was fabricated. Non-spherical nanoparticles of gold were electro-deposited in the presence of ethosuximide as a shape directing and size controlling agent. The nanoparticles had dimensions ranging 50-150 nm, and covered the underlying surface with a roughness factor of 8.03. The Non-spherical...
Source: Journal of Pharmaceutical and Biomedical Analysis - October 30, 2019 Category: Drugs & Pharmacology Source Type: research

Detection and comparison of phenolic compounds in different extracts of black currant leaves by Liquid Chromatography coupled with High-Resolution ESI-LTQ-Orbitrap MS and High-Sensitivity ESI-Qtrap MS
Publication date: Available online 28 October 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Gilda D’Urso, Paola Montoro, Sonia PiacenteAbstractLiquid preparations such as tinctures and infusion derived from Ribes nigrum L. (black currant) leaves are widely used in Europe. Despite the various uses reported for the infusion and hydroalcoholic extracts of the leaves of this species, their chemical profile has not yet been defined. In the present study, the infusion, hydroalcholic and methanolic extracts prepared from R. nigrum leaves were analyzed. LC-MS analyses of these extracts allowed the c...
Source: Journal of Pharmaceutical and Biomedical Analysis - October 30, 2019 Category: Drugs & Pharmacology Source Type: research

A New High-Performance Liquid Chromatography–Tandem Mass Spectrometry Method for the Determination of Sunitinib and N-desethyl sunitinib in Human Plasma: Light-Induced Isomerism Overtaking Towards Therapeutic Drug Monitoring in Clinical Routine
Publication date: Available online 25 October 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Elena Marangon, Mauro Buzzo, Bianca Posocco, Sara Gagno, Martina Zanchetta, Valentina Iacuzzi, Ariana Soledad Poetto, Michela Guardascione, Luciana Giodini, Giuseppe ToffoliAbstractSunitinib is approved for advanced renal cell cancer, imatinib-resistant or -intolerant gastrointestinal stromal tumors and pancreatic neuroendocrine cancers. It is prescribed at a fixed dose but its plasma exposure shows large inter-individual variations. Taking into account the narrow therapeutic window and the positive exposur...
Source: Journal of Pharmaceutical and Biomedical Analysis - October 26, 2019 Category: Drugs & Pharmacology Source Type: research

Determination of total and free voriconazole in human plasma: application to pharmacokinetic study and therapeutic monitoring
Publication date: Available online 25 October 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Matylda Resztak, Katarzyna Kosicka, Paulina Zalewska, Justyna Krawiec, Franciszek K. GłówkaAbstractVoriconazole (VCZ) is highly efficient in the treatment of invasive fungal infections. However, the therapy requires the monitoring of VCZ plasma concentration, due to a narrow therapeutic index and large inter-individual variability of pharmacokinetics of VCZ, which often exhibits nonlinearity. Total plasma concentration of VCZ does not always provide sufficient information, especially in hemato-oncol...
Source: Journal of Pharmaceutical and Biomedical Analysis - October 26, 2019 Category: Drugs & Pharmacology Source Type: research

Exclusion of unsuitable CNS drug candidates based on their physicochemical properties and unbound fractions in biomatrices for brain microdialysis investigations
Publication date: Available online 25 October 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Qianwen Wang, Tianjing Ren, Jiajia Zhao, Chun-Ho Wong, H.Y. Edwin Chan, Zhong ZuoAbstractMicrodialysis has been the only direct method of continuously measuring the unbound drug concentrations in extracellular fluid at a specific brain region with respect to time in the same animal. However, not every compound is suitable for microdialysis system as demonstrated by their inconsistent “by gain” and “by loss” in-vitro microdialysis probe recoveries leading to over- or under- estimated ...
Source: Journal of Pharmaceutical and Biomedical Analysis - October 26, 2019 Category: Drugs & Pharmacology Source Type: research

Quantitative, real-time in vivo tracking of magnetic nanoparticles using multispectral optoacoustic tomography (MSOT) imaging
Publication date: Available online 25 October 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Tareq Anani, Andrew Brannen, Peter Panizzi, Evert C. Duin, Allan E. DavidAbstractThe goal of this work was to demonstrate real-time tracking of in vivo nanoparticle concentrations utilizing multispectral optoacoustic tomography (MSOT). Combining the high contrast of optical imaging with the high resolution of ultrasound imaging, MSOT was utilized for non-invasive, real-time tomographic imaging of particles in mice and the results calibrated against analysis of tissue samples with electron paramagnetic reson...
Source: Journal of Pharmaceutical and Biomedical Analysis - October 26, 2019 Category: Drugs & Pharmacology Source Type: research

Editorial Board
Publication date: 5 January 2020Source: Journal of Pharmaceutical and Biomedical Analysis, Volume 177Author(s): (Source: Journal of Pharmaceutical and Biomedical Analysis)
Source: Journal of Pharmaceutical and Biomedical Analysis - October 26, 2019 Category: Drugs & Pharmacology Source Type: research

Simultaneous Quantitative LC-MS Method of Ketamine, Midazolam and their Metabolites (Dehydronorketamine, Norketamine and 1Hydroxymidazolam) for its Application in Patients on Extracorporeal Membrane Oxygenation (ECMO) Therapy
Publication date: Available online 24 October 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Ankit Rochani, Edwin Lam, Julian Tanjuakio, Hitoshi Hirose, Walter K. Kraft, Gagan KaushalAbstractKetamine (Ket) and midazolam (MDZ) are commonly administered drugs in the intensive care setting for analgesia and sedation. Ket and MDZ are metabolized to dehydro-norketamine (DHNK), nor-ketamine (NK) and 1-hydroxy midazolam (1HMDZ). Limited studies evaluating their pharmacokinetics exists in patients on extracorporeal membrane oxygenation (ECMO) therapy. Therefore, we developed a quantitative, high-performanc...
Source: Journal of Pharmaceutical and Biomedical Analysis - October 26, 2019 Category: Drugs & Pharmacology Source Type: research

UHPLC-MS/MS method for the quantification of aloin-A in rat plasma and its application to a pharmacokinetic study
Publication date: Available online 25 October 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Chao Niu, Weijian Ye, Xiao Cui, Jia Sun, Shuyi Xiao, Gen Chen, Shihui Bao, Ruijie ChenAbstractAloin-A (also known as barbaloin), the main bioactive anthraquinone-C-glycoside of Aloe species, exhibits various beneficial pharmacological effects. However, the determination and pharmacokinetic study of aloin-A in rat plasma need to be improved and systematically demonstrated. In the present study, a simple, robust and sensitive ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) ...
Source: Journal of Pharmaceutical and Biomedical Analysis - October 26, 2019 Category: Drugs & Pharmacology Source Type: research

Labeled substance P as a neuropeptide reporter substance for enzyme activity
Publication date: Available online 24 October 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Ulrich Schreiber, Christian Engl, Malte Bayer, Simone KönigAbstractRecently, we developed a bradykinin reporter assay and demonstrated the differing protease activity in Complex Regional Pain Syndrome patients vs. controls. In order to further characterize CRPS pathophysiology, the neuropeptide substance P was evaluated as possible reporter substance, here. It was labeled with a chromophore at the lysine residue and generated two major fragments following incubation with serum (amino acid residues 3-8 ...
Source: Journal of Pharmaceutical and Biomedical Analysis - October 24, 2019 Category: Drugs & Pharmacology Source Type: research

Optimization of a liquid chromatography method for the analysis of related substances in daclatasvir tablets using design of experiments integrated with the steepest ascent method and Monte Carlo simulation
Publication date: Available online 22 October 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Trupti Tol, Harshad Tawde, Savita Gorad, Avinash Jagdale, Amol Kulkarni, Avinash Kasbale, Anita Desai, Gautam SamantaAbstractAnalytical method for the determination of related substances (RS) in Daclatasvir tablets was optimised using quality by design (QbD) approach. Seven degradants (each more than 1.0%) generated during oxidation study, adversely affected the selectivity of the method. Coelution of the degradant peaks with API and known impurities, suggested failure in developing a stability indicating m...
Source: Journal of Pharmaceutical and Biomedical Analysis - October 24, 2019 Category: Drugs & Pharmacology Source Type: research

Pharmacokinetic and Metabolic Profiling Studies of sennoside B by UPLC-MS/MS and UPLC-Q-TOF-MS
This study aimed to obtain the metabolic and pharmacokinetic data of sennoside B. The metabolic profiles of sennoside B were obtained from rat plasma, urine, bile and feces by an ultra-performance liquid chromatography quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF-MS). As a result, 14 metabolites were structurally identified and the proposed metabolic pathways of sennoside B included hydrolysis to aglycones, release of rhein-type anthrone, and extensive conjugation. As the only compound detected in the plasma samples after intravenous and intragastric administrations, the prototype was selected as the plasma mark...
Source: Journal of Pharmaceutical and Biomedical Analysis - October 23, 2019 Category: Drugs & Pharmacology Source Type: research

Permeability and transport mechanism of trihexyphenidyl hydrochloride in Caco-2 cell monolayer model with a validated UPLC-MS/MS method
Publication date: Available online 21 October 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Chengcan Lu, Kejia Fu, Kangna Cao, Jiali Wei, Jing Zhou, Di Zhao, Ning Li, Yang Lu, Xijing Chen, Yongjie ZhangAbstractA rapid and sensitive ultra-high-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was applied to investigate the permeability characteristics and transport mechanism of trihexyphenidyl hydrochloride (TH) in D-hanks with the Caco-2 cells model. Analytes were separated using an Zorbax Extend-Agilent C18 (1.8 µm, 4.6 × 30 mm)...
Source: Journal of Pharmaceutical and Biomedical Analysis - October 23, 2019 Category: Drugs & Pharmacology Source Type: research

Benchtop NMR spectroscopy in the analysis of substandard and falsified medicines as well as illegal drugs
Publication date: Available online 21 October 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Peter H.J. Keizers, Frank Bakker, José Ferreira, Paul F.K. Wackers, Dion van Kollenburg, Eva van der Aa, Amy van BeersAbstractSubstandard and falsified medical products may cause harm to patients and fail to treat the diseases or conditions for which they were intended. It is therefore required to have analytical methods available to assess medical product quality. Benchtop NMR spectroscopy provides a generic, inherently quantitative, analytical method capable of separating specific signals from thos...
Source: Journal of Pharmaceutical and Biomedical Analysis - October 23, 2019 Category: Drugs & Pharmacology Source Type: research

HPLC–MS/MS method for the determination and pharmacokinetic study of six compounds against rheumatoid arthritis in rat plasma after oral administration of the extract of Caulophyllum robustum Maxim
Publication date: Available online 21 October 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Yuyan Guo, Shaowa lü, Bingyou Yang, Guoyu Li, Wenbao Ma, Qiaoxin Guo, Qiuhong Wang, Haixue KuangAbstractCaulophyllum robustum Maxim (CRM) is a well-known traditional Chinese medicine (TCM) mainly present in the northeast, northwest and southwest regions of China, which is belong to the family Berberidaceae. The roots and rhizomes of CRM have been used as a famous TCM for the treatment of rheumatoid arthritis (RA). The selective, sensitive and accurate high-performance liquid chromatography-electrospray...
Source: Journal of Pharmaceutical and Biomedical Analysis - October 21, 2019 Category: Drugs & Pharmacology Source Type: research

Effect of light, oxygen and temperature on the stability of artepillin C and p-coumaric acid from Brazilian green propolis
Publication date: Available online 19 October 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Caroline Arruda, Victor Pena Ribeiro, Marília Oliveira Almeida, Jennyfer Andrea Aldana Mejía, Rosana Casoti, Jairo Kenupp BastosAbstractBrazilian Green Propolis (BGP) is an important bee product, which displays important biological activities, making it valuable in the international market. The major prenylated phenolic compound in BPG is (E)-artepillin C, along with its precursor (E)-p-coumaric acid, both contributing to the biological effects of BGP. Taking that into account, it was evaluate...
Source: Journal of Pharmaceutical and Biomedical Analysis - October 21, 2019 Category: Drugs & Pharmacology Source Type: research

Paper-based immunosensor with competitive assay for cortisol detection
Publication date: Available online 19 October 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Amara Apilux, Sirirat Rengpipat, Wilasinee Suwanjang, Orawon ChilapakulAbstractThe measurement of cortisol (stress hormone) is important for diagnosis and monitoring of stress-related diseases. A paper-based immunosensor with a competitive assay was developed for quick and easy detection of cortisol levels in serum. The paper-based sensor was fabricated using a simple and cheap wax printing method. Cortisol conjugated-BSA was immobilized on the paper’s surface in the detection zone for the competitive...
Source: Journal of Pharmaceutical and Biomedical Analysis - October 21, 2019 Category: Drugs & Pharmacology Source Type: research

Pharmacopeial specifications and analytical data from post-marketing quality sampling and testing programs: a perspective beyond out-of-specification results
Publication date: Available online 18 October 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Edvaldo Oliveira Neves, Paloma Michelle de Sales, Damaris SilveiraAbstractEnsuring that marketed medicines meet acceptable standards (safety, quality, and efficacy) involves aspects of product development, compliance with good manufacturing practices, and monitoring and testing of these products already on the market. Pharmacopeias are one of the main tools used by regulatory authorities in the analytical testing for quality assessment; there are almost 60 pharmacopeias in the world. Thus, this research eva...
Source: Journal of Pharmaceutical and Biomedical Analysis - October 20, 2019 Category: Drugs & Pharmacology Source Type: research

Solid-state analysis of amorphous solid dispersions: why dsc and xrpd may not be regarded as stand-alone techniques
Publication date: Available online 18 October 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Sien Dedroog, Timothy Pas, Bjorn Vergauwen, Christophe Huygens, Guy Van den MooterAbstractAmorphous solid dispersions (ASDs) are single-phase amorphous systems, where drug molecules are molecularly dispersed (dissolved) in a polymer matrix. The molecular dispersion of the drug molecules is responsible for their improved dissolution properties. Unambiguously establishing the phase behaviour of the ASDs is of utmost importance. In this paper, we focused on the complementary nature of (modulated) differential ...
Source: Journal of Pharmaceutical and Biomedical Analysis - October 20, 2019 Category: Drugs & Pharmacology Source Type: research

Comparative Study on Metabolic Profiling and Excretion in Rat Bile Between Combination of Notoginseng Total Saponins and Safflower Total Flavonoids and Its Individual Extracts by LC-MS/MS
In conclusion, the compatibility of SF and NS could reduce the bile excretion of the CNS-derived compounds, which may be one of the reasons for the enhancement of anti-myocardial ischemia after combination.Graphical abstract (Source: Journal of Pharmaceutical and Biomedical Analysis)
Source: Journal of Pharmaceutical and Biomedical Analysis - October 18, 2019 Category: Drugs & Pharmacology Source Type: research

Chromatographic tools for plant-derived recombinant antibodies purification and characterization
Publication date: Available online 14 October 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Caterina Temporini, Raffaella Colombo, Enrica Calleri, Sara Tengattini, Francesca Rinaldi, Gabriella MassoliniAbstractIn the last two decades, plants became an interesting alternative for the production of recombinant proteins for human therapy and several antibodies expressed in plants have reached the clinical development stage. Plants are capable of post-translational modifications (PTMs) necessary for protein activity and pharmacokinetics, such as glycosylation. However, there are important kingdom-spec...
Source: Journal of Pharmaceutical and Biomedical Analysis - October 15, 2019 Category: Drugs & Pharmacology Source Type: research

Simultaneous determination of donepezil, 6-O-desmethyl donepezil and spinosin in beagle dog plasma using liquid chromatography‒tandem mass spectrometry and its application to a drug-drug interaction study
Publication date: Available online 13 October 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Chae Bin Lee, Jee Sun Min, Soon Uk Chae, Hye Min Kim, Jun Hee Jang, In Ho Jung, Yu Fen Zheng, Jong Hoon Ryu, Soo Kyung BaeABSTRACTSpinosin, which is traditionally used for sedation and sleep disorders, has recently shown potential effects in alleviating memory loss. As spinosin is the main bioactive component in a standardized dried 50% ethanol extract of the seeds of Zizyphus jujuba var. spinosa, a Phase Ⅱb clinical trial is ongoing, in Korea for the combination of the above extract formulated in a table...
Source: Journal of Pharmaceutical and Biomedical Analysis - October 15, 2019 Category: Drugs & Pharmacology Source Type: research

Separation Methods hyphenated to Mass Spectrometry for the Characterization of the Protein Glycosylation at the Intact Level
Publication date: Available online 13 October 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Julien Camperi, Valerie Pichon, Nathalie DelaunayAbstractGlycosylation is one of the most common post-translational modifications of proteins that affects their biological activity, solubility, and half-life. Therefore, its characterization is of great interest in proteomic, particularly from a diagnostic and therapeutic point of view. However, the number and type of glycosylation sites, the degree of site occupancy and the different possible structures of glycans can lead to a very large number of isoforms...
Source: Journal of Pharmaceutical and Biomedical Analysis - October 15, 2019 Category: Drugs & Pharmacology Source Type: research

Metabolite distribution and correlation studies of Ziziphus jujuba and Ziziphus nummularia using LC-ESI-MS/MS
Publication date: Available online 11 October 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Muhammad Noman Khan, Faraz Ul Haq, Saeedur Rahman, Arslan Ali, Syed Ghulam MusharrafAbstractZiziphus jujuba and Ziziphus nummularia are two important species of the genus Ziziphus. Both plants offer great commercial value and are consumed as food around the world and used for their medicinal values such as anti-inflammatory, antioxidant and hepatoprotective activities. Comprehensive chemical profiling of Z. jujuba and Z. nummularia was done through identification of major metabolites using HPLC-QTOF-MS/MS a...
Source: Journal of Pharmaceutical and Biomedical Analysis - October 12, 2019 Category: Drugs & Pharmacology Source Type: research

Typing and determination of SNP functional gene based on highly selective and signal-amplified fluorescence double-probe with the help of ExoIII nuclease and magnetic bead
Publication date: Available online 11 October 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Chun-Yan Min, Lu-Qian Wu, Ting-ting Qian, Noor Ul Ain, Wen-Juan Liu, Xiao-Ning Wu, Chen Zhang, Zhe Chen, Hong-Ping XieAbstractWe have developed a fluorescence double-probe detection system with signal amplification for simple typing and determination of single nucleotide polymorphism (SNP) functional gene based on non-sequence dependence of ExoIII nuclease on dsDNA and rapid separation of magnetic bead. Matched detected gene can cyclically release abundant fluorescence-labeled ssDNA from the probe and the c...
Source: Journal of Pharmaceutical and Biomedical Analysis - October 12, 2019 Category: Drugs & Pharmacology Source Type: research

Advanced sensing technologies of phenolic compounds for pharmaceutical and biomedical analysis
Publication date: Available online 11 October 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Liya Ge, Shao-Ping Li, Grzegorz LisakAbstractPhenolic compounds are bioactive natural products of considerable interest in pharmaceuticals and biomedicines. Due to their bioactive functions, phenolic compounds have received increasing attention in recent years. Therefore, it is necessary to develop new and advanced analytical methods for determination of phenolic compounds in relation to pharmaceutical and biomedical applications. However, in majority, their detection has been largely conducted by sensitive...
Source: Journal of Pharmaceutical and Biomedical Analysis - October 12, 2019 Category: Drugs & Pharmacology Source Type: research

NMR Reveals an Undeclared Constituent in Custom Synthetic Peptides
This report shows how NMR analysis uncovered the unanticipated presence of substantial amounts of mannitol (20 and 43% w/w) as undeclared constituent in two custom synthetic peptides, DR and DRVYI, that were sourced commercially. Quantitative 1H NMR (qHNMR) readily detected the contaminant, even on a 60 MHz benchtop instrument, and quantified the highly polar UV-transparent adulterant. Quantum-mechanical 1H iterative Full Spin Analysis (HiFSA) achieved unambiguous identification of both the mannitol and the peptides and confirmed the quantitative results.The cases show that experimental verification supersedes trust...
Source: Journal of Pharmaceutical and Biomedical Analysis - October 11, 2019 Category: Drugs & Pharmacology Source Type: research

Detection of wheat allergens using 2D Western blot and mass spectrometry
ConclusionsThe present study allowed the identification of different protein areas specific to these studied groups. The protein spots of interest were identified by UHPLC-MS/MS. It has been possible to establish a link between a specific symptomatology and the newly identified responsible allergens. (Source: Journal of Pharmaceutical and Biomedical Analysis)
Source: Journal of Pharmaceutical and Biomedical Analysis - October 11, 2019 Category: Drugs & Pharmacology Source Type: research

Combinatory high-resolution microdissection/ultra performance liquid chromatographic–mass spectrometry approach for small tissue volume analysis of rat brain glycogen
Publication date: 30 January 2020Source: Journal of Pharmaceutical and Biomedical Analysis, Volume 178Author(s): Khaggeswar Bheemanapally, Mostafa M.H. Ibrahim, Karen P. BriskiAbstractCyto-architectural diversity of brain structures emphasizes need for analytical tools for discriminative investigation of distinctive neural structures. Glycogen is the major energy reserve in the brain. There is speculation that brain utilization of this fuel source may affect detection of hypoglycemia. To evaluate sex-specific regulation of glycogen mass and mobilization in the glucose-sensory ventromedial hypothalamic nucleus (VMN), curren...
Source: Journal of Pharmaceutical and Biomedical Analysis - October 11, 2019 Category: Drugs & Pharmacology Source Type: research