A systematic investigation on free phenolic acids and flavonoids profiles of commonly consumed edible flowers in China
Publication date: Available online 4 May 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Jingyun Zheng, Maninder Meenu, Baojun XuAbstractEdible flowers of ornamental plants are non-toxic flowers that have been used since ancient times for their nutritional and health benefits. These health benefits are attributed to their phytochemicals such as phenolic acids and flavonoids. These phytochemicals exert positive health effects on chronic diseases such as cancer, inflammation, and diabetes. This research paper is focused on the systematic investigation of free phenolic acids and flavonoids (including a...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 5, 2019 Category: Drugs & Pharmacology Source Type: research

Diablo Ubiquitination Analysis by Sandwich Immunoassay
Publication date: Available online 3 May 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Arcan Guven, Wenfang S. Wu, Saurabh Patil, Karthiga Gokul, Poornima Tekumalla, Shefali Sharma, Anne Diers, Stephane Gesta, Vivek Vishnudas, Rangaprasad Sarangarajan, Mark D. Kellogg, Niven R. Narain, Michael A. KiebishAbstractUbiquitin plays an essential role in modulating protein functions, and deregulation of the ubiquitin system leads to the development of a variety of human diseases. E3 Ubiquitin ligases that mediate ubiquitination and degradation of caspases prevent apoptosis, and as such belong to the fami...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 5, 2019 Category: Drugs & Pharmacology Source Type: research

Pharmacokinetics and tissue distribution evaluation of α-asaronol and its main metabolite in rats by HPLC method
Publication date: Available online 3 May 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Ying Sun, Yajun Bai, Min Zeng, Xufei Chen, Jing Xie, Bin Li, Xirui He, Yujun Bai, Pu Jia, Xue Meng, Jing Liang, Shixiang Wang, Tai-Ping Fan, Biao Wu, Xiaohui ZhengAbstractα-Asaronol is one of trace metabolites of α-asarone formed in vivo and in vitro and exhibits good anticonvulsant activities with low neurotoxicity. The present study was mainly to describe the pharmacokinetics and tissue distribution of α-asaronol and its metabolite E-2,4,5-trimethoxy cinnamic acid (E-2,4,5-TMCA), in rat after...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 5, 2019 Category: Drugs & Pharmacology Source Type: research

Development of a novel LC–MS/MS method for quantitation of triticonazole enantiomers in rat plasma and tissues and application to study on toxicokinetics and tissue distribution
In this study, a chiral analytical method of LC–MS/MS was developed and validated for the assay of triticonazole enantiomers in rat plasma and tissues. There were no endogenous interferences in the blank plasma and tissues of rats. R-(−)- and S-(+)-triticonazole peaks were separated entirely. The calibration curves were linear from 25 to 2500 ng/mL of each enantiomer. The accuracy, precision, and stability met the requirements of bioanalysis. Therefore, this method is enantioselective, accurate, precise, sensitive and reliable, and has been successfully applied to analyze R-(−)- and S-(+)-triticona...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 3, 2019 Category: Drugs & Pharmacology Source Type: research

Characterization of TPN171 metabolism in humans via ultra-performance liquid chromatography/quadrupole time-of-flight mass spectrometry
This study aimed to establish a rapid and reliable method based on ultra-performance liquid chromatography/quadrupole time-of-flight mass spectrometry for the characterization of TPN171 metabolites in human plasma, urine and stool samples. A total of 17 metabolites, including 14 from phase I and 3 from phase II metabolic reactions, were identified and characterized. TPN171 was found to be the predominant component in all plasma, urine and stool samples. Seven proposed metabolites were validated by comparing with synthetic reference standards. N-demethylation, O-depropylation, N-oxidation and dehydrogenation were demonstrat...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 2, 2019 Category: Drugs & Pharmacology Source Type: research

Identification of recombinant human insulin and biosynthetic insulin analogues by multiplexed targeted unlabeled mass spectrometry of proteotypic tryptic peptides
Publication date: Available online 1 May 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Rani J. Qasem, Anas S. Aldawsari, Faisal E. Almutairi, Abdullah S AlsadoonAbstractDirect qualitative methods that allow the rapid screening and identification of insulin products during early stages of the drug development process and those already in the market can be of great utility for manufacturers and regulatory agencies and the recent scientific literature describes several methods. Herein, a qualitative proteomic method is presented for the identification of recombinant human insulin and all marketed bio...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 2, 2019 Category: Drugs & Pharmacology Source Type: research

In vitro studies on the metabolism of saikogenins and the detection of their metabolites in authentic biosamples
Publication date: Available online 30 April 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Yunwen Xue, Jingjing Liu, Ruijia Fu, Lei Gao, Xuping Yang, Zunjian Zhang, Rui SongAbstractSaikosaponins are the representative bioactive ingredient in the Radix Bupleuri. Previous studies have reported that saikosaponins are prone to losing their glycones and being converted to corresponding prosaikogenins and saikogenins by intestinal bacteria. However, the microsomal cytochrome P450-mediated metabolism of these deglycosylated metabolites is still unknown. This research performed in vitro studies of five sai...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 2, 2019 Category: Drugs & Pharmacology Source Type: research

Real-time analysis of living animals and rapid screening of human fluid samples using remote sampling electrospray ionization mass spectrometry
In this report, we demonstrate a real-time analysis of a living mouse liver and an automatic analysis of 138 serum samples using this new technique. (Source: Journal of Pharmaceutical and Biomedical Analysis)
Source: Journal of Pharmaceutical and Biomedical Analysis - May 2, 2019 Category: Drugs & Pharmacology Source Type: research

Non-enzymatic sensing of dopamine by localized surface plasmon resonance using carbon dots-functionalized gold nanoparticles
Publication date: Available online 30 April 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Mojtaba Amiri, Shayessteh Dadfarnia, Ali Mohammad Haji Shabani, Sodeh SadjadiAbstractA highly selective, sensitive, and rapid colorimetric sensor for the determination of dopamine (DA) was developed using the color change of S-doped carbon dots functionalized gold nanoparticles (S-CDs@Au NPs). The base of the method is the formation of a complex between the amine groups of dopamine with carboxylic groups of S-CDs@Au NPs followed by their aggregation with Fe3+ ions which acts as the linkers causing a red shift...
Source: Journal of Pharmaceutical and Biomedical Analysis - April 30, 2019 Category: Drugs & Pharmacology Source Type: research

Study of possible association between endometriosis and phthalate and bisphenol A by biomarkers analysis
Publication date: Available online 28 April 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Miriany Avelino Moreira Fernandez, Zenilda Lourdes Cardeal, Márcia Mendonça Carneiro, Leiliane Coelho AndréAbstractEndocrine disrupting chemicals (EDCs) such as phthalates and bisphenol A (BPA) are substances that may interfere with the actions of endogenous hormones and may be associated with estrogen-related diseases such as endometriosis. This paper describes a case-control study to evaluate the relationship between endometriosis and phthalates and BPA exposure, through biomarkers anal...
Source: Journal of Pharmaceutical and Biomedical Analysis - April 29, 2019 Category: Drugs & Pharmacology Source Type: research

A rapid and eco-friendly method for determination of the main components of gamma-oryzanol in equestrian dietary and nutritional supplements by liquid chromatography – tandem mass spectrometry
Publication date: Available online 28 April 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Emilia Waraksa, Konrad Kowalski, Ewa Kłodzińska, Rafał Rola, Jarosław Ciekot, Wojciech Filipiak, Tomasz Bieńkowski, Jacek NamieśnikAbstractGamma-oryzanol (GO) has gained special attention in the equine sports industry in recent years due to its touted properties, including the fact that it may cause anabolic effects on muscle growth and reduce fatigue. Many manufactures offer supplements containing GO as a naturally occurring anabolic substance; however, some producers do not declare its presence in pro...
Source: Journal of Pharmaceutical and Biomedical Analysis - April 29, 2019 Category: Drugs & Pharmacology Source Type: research

Development of a Simple Isocratic HPLC Method for siRNA Quantitation in Lipid-based Nanoparticles
Publication date: Available online 27 April 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Zongyun Huang, William P. FishAbstractThis paper describes the development of simple and user-friendly HPLC methods that can quantitate the amount of small interfering RNA (siRNA) in lipid-based nanoparticle (LNP) formulations. The methods have been used as alternative chromatographic approaches to the size exclusion chromatography in order to perform “fit for purpose” analysis such as determining the amount of released siRNA from LNP formulations as a part of in-vitro release testing. Two HPLC co...
Source: Journal of Pharmaceutical and Biomedical Analysis - April 29, 2019 Category: Drugs & Pharmacology Source Type: research

Pharmacokinetics and metabolism of H3B-6545, a selective estrogen receptor covalent antagonist, in dog plasma by liquid chromatography combined with electrospray ionization tandem mass spectrometry
Publication date: Available online 26 April 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Yingying Ge, Yongjie Zhang, Xiaonan Li, Yongsheng Yu, Qingwang LiuAbstractThe present study aimed at developing a simple and sensitive LC-MS/MS assay for the determination of H3B-6545 in dog plasma. The plasma samples were processed with acetonitrile and subsequently separated on a ZORBAX SB-C18 column (50 mm × 4.6 mm, 5 μm), using 0.1% formic acid in water and acetonitrile as mobile phase, at a flow rate of 0.4 mL/min. Mass detection was obtained using selec...
Source: Journal of Pharmaceutical and Biomedical Analysis - April 27, 2019 Category: Drugs & Pharmacology Source Type: research

Studies of Pharmacokinetics in Beagle Dogs and Drug-drug Interaction Potential of a Novel Selective ZAK Inhibitor 3h for Hypertrophic Cardiomyopathy Treatment
Publication date: Available online 26 April 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Weifan Jiang, Lan Ding, Tianming Dai, Jiayin Guo, Renke Dai, Yu ChangAbstractOverexpression of leucine-zipper and sterile-α motif kinase (ZAK) in heart has been closely associated with the development of hypertrophic cardiomyopathy (HCM). N-(3-(1H-pyrazolo[3,4-b]pyridin-5-yl)ethynyl) benzene-sulfonamides, novel highly selective ZAK inhibitors, had exhibited reasonable orally therapeutic effects on HCM in spontaneous hypertensive rat models. In the present study, a rapid and sensitive HPLC-MS/MS method f...
Source: Journal of Pharmaceutical and Biomedical Analysis - April 27, 2019 Category: Drugs & Pharmacology Source Type: research

Screening of Amaryllidaceae alkaloids in bulbs and tissue cultures of Narcissus papyraceus and four varieties of N. tazetta
Publication date: Available online 24 April 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Ameneh Tarakeme, Majid Azizi, Vahid Rowshan, Hassan Salehi, Rosella Spina, François Dupire, Hossein Arouie, Dominique Laurain-MattarAbstractNarcissus spp. are an economically important crop for medicines in relation with the alkaloids production, mainly galanthamine, an acetylcholinesterase inhibitor used for the treatment of Alzheimer’s disease. In this article an extensively study of the phytochemistry of both bulbs of different species and varieties of Narcissus grown in Iran and in vitro cult...
Source: Journal of Pharmaceutical and Biomedical Analysis - April 26, 2019 Category: Drugs & Pharmacology Source Type: research

A new diosgenin sensor based on molecularly imprinted polymer of para aminobenzoic acid selected by computer-aided design
Publication date: Available online 24 April 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Fatemeh Ganjeizadeh Rohani, Alireza Mohadesi, Mehdi AnsariAbstractA novel electropolymerized molecularly imprinted polymer (MIP) film, based on diosgenin on a glassy carbon electrode (GCE), has been synthesized. Based on density functional theory (DFT), para-aminobenzoic acid (pABA), which is a green substance, was selected from five functional monomers by Gaussian software for MIP production, to be the suitable monomer. The MIP’s synthesis conditions were optimized, and the imprinting effect was confir...
Source: Journal of Pharmaceutical and Biomedical Analysis - April 24, 2019 Category: Drugs & Pharmacology Source Type: research

Validation and uncertainty estimation for trace amounts determination of 25 drugs used in hospital chemotherapy compounding units
Publication date: Available online 22 April 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Nicolas Guichard, Serge Rudaz, Pascal Bonnabry, Sandrine Fleury-SouverainAbstractThe validation and uncertainty assessment of the analytical method developed for the simultaneous determination of 25 anticancer drugs commonly handled in hospital pharmacy was reported. Selected compounds were 5-fluorouracil, cytarabine, fludarabine phosphate, ganciclovir, gemcitabine, dacarbazine, methotrexate, pemetrexed, busulfan, raltitrexed, etoposide phosphate, topotecan, ifosfamide, cyclophosphamide, irinotecan, doxorubic...
Source: Journal of Pharmaceutical and Biomedical Analysis - April 23, 2019 Category: Drugs & Pharmacology Source Type: research

Quantitation of paclitaxel, and its 6-alpha-OH and 3-para-OH metabolites in human plasma by LC–MS/MS
Publication date: 5 August 2019Source: Journal of Pharmaceutical and Biomedical Analysis, Volume 172Author(s): Susan M. Christner, Robert A. Parise, Percy S. Ivy, Hussein Tawbi, Edward Chu, Jan H. BeumerAbstractWe have developed a high performance liquid chromatography mass spectrometry method for quantitating paclitaxel and its 6-alpha−OH and 3-para−OH metabolites in 0.1 mL human plasma. After MTBE liquid-liquid extraction, chromatographic separation was achieved with a Phenomenex synergy polar reverse phase (4 μm, 2 mm × 50 mm) column and a gradient of 0.1% f...
Source: Journal of Pharmaceutical and Biomedical Analysis - April 23, 2019 Category: Drugs & Pharmacology Source Type: research

Development and validation of a highly sensitive LC–MS/MS method for in vitro measurement of histamine concentration
In this study, a bioanalytical LC–MS/MS method was developed and validated to quantify histamine in the leukocyte suspension from human peripheral blood. The method used pre-column derivatization with phenylisothiocyanate (PITC) and the resulting phenylthiocarbamyl (PTC) histamine was analyzed by positive-ion electrospray ionization using the multiple reaction monitoring mode. Chromatographic separation was achieved using an Imtakt-HT C18 column (2.1 mm × 50 mm, 3.0 μm), with a flow rate of 0.35 mL/min, 2 μL injection, and gradient elution with a mixture of...
Source: Journal of Pharmaceutical and Biomedical Analysis - April 23, 2019 Category: Drugs & Pharmacology Source Type: research

Development of a novel LC-MS/MS method for quantitation of triticonazole enantiomers in rat plasma and tissues and application to study on toxicokinetics and tissue distribution
In this study, a chiral analytical method of LC-MS/MS was developed and validated for the assay of triticonazole enantiomers in rat plasma and tissues. There were no endogenous interferences in the blank plasma and tissues of rats. R-(-)- and S-(+)-triticonazole peaks were separated entirely. The calibration curves were linear from 25 to 2500 ng/mL of each enantiomer. The accuracy, precision, and stability met the requirements of bioanalysis. Therefore, this method is enantioselective, accurate, precise, sensitive and reliable, and has been successfully applied to analyze R-(-)- and S-(+)-triticonazole in rat plasma...
Source: Journal of Pharmaceutical and Biomedical Analysis - April 21, 2019 Category: Drugs & Pharmacology Source Type: research

Comparative pharmacokinetic study on phenolic acids and flavonoids in spinal cord injury rats plasma by UPLC-MS/MS after single and combined oral administration of danshen and huangqin extract
Publication date: Available online 20 April 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Lixin Zhang, Xifang Liu, Hao Yang, Rui Zhao, Ciucui Liu, Rui Zhang, Qian ZhangAbstractChinese medicinal herbs danshen and huangqin have attracted attention in spinal cord injury (SCI) treatment. Purpose of this study was to investigate and compare the pharmacokinetic characteristics of 4 phenolic acids and 4 flavonoids in SCI rat plasma after orally administrate danshen, huangqin and combined extract of these two herbs (CDH). Thus, a rapid and sensitive ultra performance liquid chromatography-tandem mass spec...
Source: Journal of Pharmaceutical and Biomedical Analysis - April 21, 2019 Category: Drugs & Pharmacology Source Type: research

Development and validation of an LC-MS/MS method for the analysis of ivermectin in plasma, whole blood, and dried blood spots using a fully automatic extraction system
Publication date: 5 August 2019Source: Journal of Pharmaceutical and Biomedical Analysis, Volume 172Author(s): Urs Duthaler, Claudia Suenderhauf, Stefan Gaugler, Beatrice Vetter, Stephan Krähenbühl, Felix HammannAbstractIvermectin is deployed in mass drug administration (MDA) campaigns to control parasitic diseases in the tropics, with billions of treatments having been administered in the last three decades. Simple blood sampling tools, like the dried blood spots (DBS) technique, are needed to monitor treatments in such challenging settings. Thus, we developed a fully automated method for the analysis of ivermec...
Source: Journal of Pharmaceutical and Biomedical Analysis - April 21, 2019 Category: Drugs & Pharmacology Source Type: research

Selective modification of skin barrier lipids
This study assess the effect of Ac on skin barrier lipids in-depth. Synchrotron based Fourier-transform infrared microspectroscopy (FTIR), which is used to study SC lipid organization, revealed a more ordered lipid organization after Ac treatment. In vitro experiments using Franz cells, which were selected to follow the SC barrier function capability, demonstrated that Ac-treated skin retained caffeine and ibuprofen on the SC with very low permeation of both compounds into the deeper skin layers. In vitro transepidermal water loss (TEWL) measurements revealed the ability of Ac to induce a less water permeated skin. Althoug...
Source: Journal of Pharmaceutical and Biomedical Analysis - April 20, 2019 Category: Drugs & Pharmacology Source Type: research

Development and validation of a UPLC-MS/MS analytical method for dofetilide in mouse plasma and urine, and its application to pharmacokinetic study
Publication date: Available online 19 April 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Muhammad Erfan Uddin, Xinxin Sun, Kevin M. Huang, Shuiying Hu, Cynthia A. Carnes, Alex Sparreboom, Qiang FuAbstractA novel method using UPLC with tandem mass-spectrometric detection (UPLC-MS/MS) with positive electrospray ionization was developed for the detection of the antiarrhythmic drug, dofetilide, in mouse plasma and urine. Protein precipitation was performed on 10 µL of plasma and 2 µL of urine samples using dofetilide-D4 as an internal standard, and separation of the analyte ...
Source: Journal of Pharmaceutical and Biomedical Analysis - April 20, 2019 Category: Drugs & Pharmacology Source Type: research

A qHNMR method for simultaneous quantification of terpenoids from Ferula ovina (Boiss.) Boiss roots
Publication date: Available online 19 April 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Faegheh Farhadi, Saba Soltani, Satar Saberi, Mehrdad IranshahiAbstractFerula ovina (Boiss.) Boiss is one of the most important endemic medicinal plants in Iran, which has three main terpenoid compounds including ferutinin, stylosin and tschimgine. Ferutinin is the strongest natural phytoestrogen that has agonistic activity on estrogen receptors, particularly α-receptors. To determine the amount of ferutinin in F. ovina roots, we firstly used HPLC-UV method. In the HPLC method, the resolution of ferutini...
Source: Journal of Pharmaceutical and Biomedical Analysis - April 20, 2019 Category: Drugs & Pharmacology Source Type: research

Development and validation of a multiplexed drug level assay in support of combination biologics therapy clinical studies
Publication date: 15 July 2019Source: Journal of Pharmaceutical and Biomedical Analysis, Volume 171Author(s): Huaping Tang, Ketal Shah, Thomas Steinmetz, Anson Abraham, Hans Jensen, Andrew Bouton, Kasia Marullo, Shuangping ShiAbstractClinical development of biotherapeutics for combination therapy requires monitoring the concentrations of both drugs in biological samples. Traditionally, two assays are required to measure drug levels one at a time, which poses challenges in sample management, data reporting, and cost. The Meso Scale Discovery (MSD®) U-PLEX™ platform provides a simple and flexible way to create cust...
Source: Journal of Pharmaceutical and Biomedical Analysis - April 20, 2019 Category: Drugs & Pharmacology Source Type: research

A simple and sensitive LC-MS/MS method for quantification of Bepridil in rat plasma and its application to pharmacokinetic studies
Publication date: Available online 18 April 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Bhavesh D. Patel, Nageswararao P, Rajesh Alamanda, Ajit R. Gadekar, Amol A. Raje, Rakshit AmetaAbstractBepridil is potent inhibitor of Na+, K+ and Ca+ channel in cardiomyocytes. It has demonstrated strong antianginal effect with type I antiarrhythmic and with minimum antihypertensive therapeutic effect. Till date, a specific LC-MS/MS method to quantify Bepridil concentrations in biological matrix have not been reported yet.. In current study, a highly sensitive, specific and simple LC-MS/MS method for quantif...
Source: Journal of Pharmaceutical and Biomedical Analysis - April 20, 2019 Category: Drugs & Pharmacology Source Type: research

Quantification of the tyrosine kinase inhibitor erlotinib in human scalp hair by liquid chromatography-tandem mass spectrometry: pitfalls for clinical application
In conclusion, a reliable and robust LC-MS/MS method was developed to quantify erlotinib in hair, however, clinical and in vitro evaluations showed that the method is not suitable for monitoring long term erlotinib exposure. The pitfalls of this application outweigh the current benefits. (Source: Journal of Pharmaceutical and Biomedical Analysis)
Source: Journal of Pharmaceutical and Biomedical Analysis - April 18, 2019 Category: Drugs & Pharmacology Source Type: research

Salting out assisted liquid-liquid extraction for liquid chromatography tandem-mass spectrometry determination of amphetamine-like stimulants in meconium
Publication date: Available online 17 April 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Alžběta Nemeškalová, Miroslava Bursová, David Sýkora, Martin Kuchař, Radomír Čabala, Tomáš HložekAbstractIn the last decade there has been a dramatic increase in the availability and abuse of synthetic cathinones – new amphetamine-like stimulants. Even though their abuse during pregnancy could have serious adverse effects on the fetus, cathinones are not readily included in neonatal toxicological screenings. Meconium (first neonatal stool) is the spe...
Source: Journal of Pharmaceutical and Biomedical Analysis - April 18, 2019 Category: Drugs & Pharmacology Source Type: research

Novel chiral metal organic frameworks functionalized composites for facile preparation of optically pure propranolol hydrochlorides
Publication date: Available online 16 April 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Xue Ma, Wenrui Du, Yan Li, Chenfeng Hua, Ajuan Yu, Wuduo Zhao, Shusheng Zhang, Fuwei XieABSTRACTTwo novel sorbents based on polydopamine (PDA)-coated magnetic graphite oxide-metal organic frameworks nanoparticles [Cu(L-mal)(bpy)]·H2O (MGO-CuLBH) and [Cu(D-mal)(bpy)]·H2O (MGO-CuDBH) possessing of both magnetic property and excellent enantioselective ability were prepared and characterized. Solutions of racemic propranolol hydrochloride (Rac-PRO) were chosen to investigate the enantioselective per...
Source: Journal of Pharmaceutical and Biomedical Analysis - April 17, 2019 Category: Drugs & Pharmacology Source Type: research

Pharmacokinetic Properties of Enantiomerically Pure GluN2B Selective NMDA Receptor Antagonists with 3-Benzazepine Scaffold
Publication date: Available online 16 April 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Frederik Börgel, Fabian Galla, Kirstin Lehmkuhl, Dirk Schepmann, Simon M. Ametamey, Bernhard WünschAbstractRecently, the eutomers of highly potent GluN2B selective NMDA receptor antagonists with 3-benzazepine scaffold were identified. Herein, pharmacokinetic properties regarding lipophilicity, plasma protein binding (PPB) and metabolism are analyzed. The logD7.4 values of 1.68 for phenol 1 and 2.46 for methyl ether 2 are in a very good range for CNS agents. A very similar logD7.4 value was recorded ...
Source: Journal of Pharmaceutical and Biomedical Analysis - April 17, 2019 Category: Drugs & Pharmacology Source Type: research

The contamination of valsartan and other sartans, Part 2: Untargeted Screening reveals contamination with amides additionally to known nitrosamine impurities
Publication date: Available online 16 April 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Oliver Scherf-Clavel, Martina Kinzig, Axel Besa, André Schreiber, Clemens Bidmon, Mona Abdel-Tawab, Jonas Wohlfart, Fritz Sörgel, Ulrike HolzgrabeAbstractThe recent incidences of contaminated valsartan drug products gave rise to review the suitability of current impurity profiling workflows implemented at authorities and pharmaceutical companies. The major drawback of targeted impurity profiling, where a considerable amount of prior knowledge about possible contaminants is necessary, is the fact t...
Source: Journal of Pharmaceutical and Biomedical Analysis - April 17, 2019 Category: Drugs & Pharmacology Source Type: research

Simultaneous determination of curcumin, tetrahydrocurcumin, quercetin, and paeoniflorin by UHPLC-MS/MS in rat plasma and its application to a pharmacokinetic study
In this study, a rapid, sensitive, and reliable ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method was developed and validated for the simultaneous determination of CUR, tetrahydrocurcumin (THC), QR, and PF in rat plasma by using tinidazole as the internal standard (IS). A liquid-liquid extraction method with ethyl acetate was used to pre-treat the plasma samples. Chromatographic separation was conducted on a C18 column with isocratic elution using acetonitrile and 0.1% formic acid water solution (80:20, v/v) as the mobile phase at the flow rate of 0.3 mL/min. A TSQ Quantum Ac...
Source: Journal of Pharmaceutical and Biomedical Analysis - April 17, 2019 Category: Drugs & Pharmacology Source Type: research

The application of combined 1H NMR-based metabolomics and transcriptomics techniques to explore phenolic acid biosynthesis in Salvia miltiorrhiza Bunge
Publication date: Available online 17 April 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Xia Liu, Mengxia Jin, Min Zhang, Tianqi Li, Shanshan Sun, Jinyue Zhang, Jungui Dai, Yinghong WangAbstractSalvia miltiorrhiza Bunge is a traditional Chinese medicine, and its water-soluble phenolic acid active compounds have very important medicinal value; however, the synthesis pathways of the main active ingredients remain unknown. Here, we employed nuclear magnetic resonance (NMR)-based metabolomics and transcriptomics techniques to study the biosynthesis mechanism of salvianolic acids. High-performance liq...
Source: Journal of Pharmaceutical and Biomedical Analysis - April 17, 2019 Category: Drugs & Pharmacology Source Type: research

Analysis of hydroxy-cocaine metabolites as evidence of cocaine consumption: identification by parent ion search and quantitation by uhplc–ms/ms in hair sample
Publication date: Available online 15 April 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Mauro Minoli, Sara Casati, Ilaria Angeli, Alessandro Ravelli, Paola Rota, Pietro Allevi, Marica OrioliAbstractOver the last decade, hair analysis has become a routine procedure in most forensic laboratories and, complementary to blood and urine, hair is a unique biological matrix which gives the opportunity to establish a temporal consumption profile. Despite hair is widely used to identify drug use, environmental contamination continues to represent a challenging factor of this procedure, especially for coca...
Source: Journal of Pharmaceutical and Biomedical Analysis - April 17, 2019 Category: Drugs & Pharmacology Source Type: research

Multi-class determination of steroid hormones and antibiotics in fatty hotpot ingredients by pressurized liquid extraction and liquid chromatography–tandem mass spectrometry
Publication date: Available online 15 April 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Mengting Wang, Yang Wang, Bin Peng, Na Zhao, Jing Zhao, Zhili Xiong, Longshan ZhaoAbstractDue to the misuse of hormones and antibiotics resulting in drug residues in meat products, serious concerns have arisen regarding to the potential risks for human health. In this paper, a simple and efficient method was developed to simultaneously quantify six steroid hormones and six antibiotics in fatty foods by combining pressurized liquid extraction (PLE) with ultra-high performance liquid chromatography-tandem mass ...
Source: Journal of Pharmaceutical and Biomedical Analysis - April 17, 2019 Category: Drugs & Pharmacology Source Type: research

Quantitation of paclitaxel, and its 6-alpha-OH and 3-para-OH metabolites in human plasma by LC-MS/MS
Publication date: Available online 15 April 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Susan M. Christner, Robert A. Parise, Percy S. Ivy, Hussein Tawbi, Edward Chu, Jan H. BeumerAbstractWe have developed a high performance liquid chromatography mass spectrometry method for quantitating paclitaxel and its 6-alpha-OH and 3-para-OH metabolites in 0.1 mL human plasma. After MTBE liquid-liquid extraction, chromatographic separation was achieved with a Phenomenex synergy polar reverse phase (4 µm, 2 mm x 50 mm) column and a gradient of 0.1% formic acid...
Source: Journal of Pharmaceutical and Biomedical Analysis - April 17, 2019 Category: Drugs & Pharmacology Source Type: research

Development and validation of a LC-MS/MS method for the analysis of ivermectin in plasma, whole blood, and dried blood spots using a fully automatic extraction system
Publication date: Available online 16 April 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Urs Duthaler, Claudia Suenderhauf, Stefan Gaugler, Beatrice Vetter, Stephan Krähenbühl, Felix HammannAbstractIvermectin is deployed in mass drug administration (MDA) campaigns to control parasitic diseases in the tropics, with billions of treatments having been administered in the last three decades. Simple blood sampling tools, like the dried blood spots (DBS) technique, are needed to monitor treatments in such challenging settings. Thus, we developed a fully automated method for the analysis of iv...
Source: Journal of Pharmaceutical and Biomedical Analysis - April 17, 2019 Category: Drugs & Pharmacology Source Type: research

Belizatinib: Novel reactive intermediates and bioactivation pathways characterized by LC–MS/MS
Publication date: 15 July 2019Source: Journal of Pharmaceutical and Biomedical Analysis, Volume 171Author(s): Mohamed W. Attwa, Adnan A. Kadi, Hany W. DarwishAbstractBelizatinib (BZB; TSR-011) is a next-generation anaplastic lymphoma kinase inhibitor that also inhibits tropomyosin-related kinases A/B/C. In this in-vitro study, we examined the formation of reactive metabolites from BZB using rat liver microsomes or human liver microsomes in the presence of a trapping agent (potassium cyanide) to generate iminium reactive intermediates. Identification of the in vitro BZB metabolites indicated that the major in-vitro metaboli...
Source: Journal of Pharmaceutical and Biomedical Analysis - April 17, 2019 Category: Drugs & Pharmacology Source Type: research

Study of the in vitro metabolic profile of a new α2-adrenergic agonist in rat and human liver microsomes by using liquid chromatography-multiple-stage mass spectrometry and nuclear magnetic resonance
Publication date: Available online 14 April 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Josiane de O. Cardoso, Bianca F. da Silva, Tiago Venâncio, Marina G. da Rocha Pitta, Ivan da R. Pitta, Rosângela G. Peccinini, Regina V. OliveiraAbstractA potent synthetic α2-adrenergic agonist called PT-31, (3-(2-chloro-6-fluorobenzyl)-imidazolidine-2,4-dione), was recently detected as a potential drug to be used as an adjuvant drug to treat chronic pain. The excellent pharmacological property of PT-31 highlights the importance in elucidating its metabolism, which could provide valuable inf...
Source: Journal of Pharmaceutical and Biomedical Analysis - April 16, 2019 Category: Drugs & Pharmacology Source Type: research

An optimized analytical method for cellular targeted quantification of primary metabolites in tricarboxylic acid cycle and glycolysis using gas chromatography-tandem mass spectrometry and its application in three kinds of hepatic cell lines
In this study, we established a repeatable gas chromatography-tandem mass spectrometry (GC-MS/MS) method with selected reaction monitoring (SRM) mode for simultaneous quantification of several primary metabolites in these two pathways, including glucose, 3-phosphoglycerate, phosphoenolpyruvate (PEP), pyruvate, lactate, citrate, cis-aconitate, isocitrate, α-ketoglutarate, succinate, fumarate and malate. There are many solvents to extract the metabolites in these two pathways, however, which one is more effective still remains unclear. Sample pretreatment was optimized for solvent types and volumes to advance the extra...
Source: Journal of Pharmaceutical and Biomedical Analysis - April 14, 2019 Category: Drugs & Pharmacology Source Type: research

Degradation studies of ibrutinib under stress conditions: characterisation and structural elucidation of novel degradants
Publication date: Available online 12 April 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Soujanya Vajjha, Vijay Bommuluri, KVK Mohan P, Chidananda Swamy Rumalla, Raju Doddipalla, Muralidharan Kaliyaperumal, Raghu Babu KorupoluAbstractThe aim of the research work is to study the degradation behaviour of Ibrutinib (IBN) which is performed under different stress conditions according to International Conference on Harmonization guidelines (ICH). The study included monitoring degradation of the Ibrutinib drug under acidic, base, oxidation, thermal and photolytic conditions followed by isolation and ch...
Source: Journal of Pharmaceutical and Biomedical Analysis - April 14, 2019 Category: Drugs & Pharmacology Source Type: research

Development and validation of a highly sensitive LC-MS/MS method for in vitro measurement of histamine concentration
In this study, a bioanalytical LC-MS/MS method was developed and validated to quantify histamine in the leukocyte suspension from human peripheral blood. The method used pre-column derivatization with phenylisothiocyanate (PITC) and the resulting phenylthiocarbamyl (PTC) histamine was analyzed by positive-ion electrospray ionization using the multiple reaction monitoring mode. Chromatographic separation was achieved using an Imtakt-HT C18 column (2.1 mm × 50 mm, 3.0 μm), with a flow rate of 0.35 mL/min, 2 μL injection, and gradient elution with a mixture of aceto...
Source: Journal of Pharmaceutical and Biomedical Analysis - April 14, 2019 Category: Drugs & Pharmacology Source Type: research

DeFvelopment and Validation of a Multiplexed Drug Level Assay in Support of Combination Biologics Therapy Clinical Studies
Publication date: Available online 13 April 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Huaping Tang, Ketal Shah, Thomas Steinmetz, Anson Abraham, Hans Jensen, Andrew Bouton, Kasia Marullo, Shuangping ShiAbstractClinical development of biotherapeutics for combination therapy requires monitoring the concentrations of both drugs in biological samples. Traditionally, two assays are required to measure drug levels one at a time, which poses challenges in sample management, data reporting, and cost. The Meso Scale Discovery (MSD®) U-PLEXTM platform provides a simple and flexible way to create cus...
Source: Journal of Pharmaceutical and Biomedical Analysis - April 14, 2019 Category: Drugs & Pharmacology Source Type: research

Measurement of ultra-trace level of intact oxytocin in plasma using SALLE combined with nano-LC-MS
In this study, we developed an efficient salt-out assisted liquid-liquid extraction (SALLE) to treat plasma, and then analyzed the samples using nano-LC-MS to quantify intact oxytocin (OT) in human and rat plasmas. Our results showed that the use of SALLE (Isopropanol/K2HPO4 (4 M)) allows efficient removal of various disrupters, including proteins, inorganic salts, and lipids, which helps avoid the risk of blocked capillary columns and matrix effects. Moreover, instant SALLE can reduce the possible binding between OT and proteins, thus allowing high repeatability of OT extraction from the original plasma. This combi...
Source: Journal of Pharmaceutical and Biomedical Analysis - April 14, 2019 Category: Drugs & Pharmacology Source Type: research

A new strategy for extraction and depuration of pantoprazole in rat plasma: vortex assisted dispersive micro-solid-phase extraction employing metal organic framework MIL-101(Cr) as sorbent followed by dispersive liquid-liquid microextraction based on solidification of a floating organic droplet
Publication date: Available online 11 April 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Qianqian Cai, Tianyu Zhao, Lianjun Zhang, Pan Zhao, Yajie Zhu, Haiyan Xu, Xiaohong HouAbstractDispersive micro-solid-phase extraction (DMSPE) combined with dispersive liquid-liquid microextraction based on the solidification of a floating organic droplet (DLLME-SFO) was successfully developed for extraction and depuration of pantoprazole in rat plasma. The remarkable metal organic framework (MOF), MIL-101(Cr) was used as DMSPE adsorbent. The detection of pantoprazole was performed by convenient HPLC-UV. In th...
Source: Journal of Pharmaceutical and Biomedical Analysis - April 12, 2019 Category: Drugs & Pharmacology Source Type: research

Reply to “Requirements for accurate 1H NMR quantification of mineral oil hydrocarbons (paraffins) for pharmaceutical or cosmetic use”
Publication date: Available online 10 April 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Jonas Urlaub, Jochen Norwig, Curd Schollmayer, Ulrike Holzgrabe (Source: Journal of Pharmaceutical and Biomedical Analysis)
Source: Journal of Pharmaceutical and Biomedical Analysis - April 11, 2019 Category: Drugs & Pharmacology Source Type: research

Comparison of isotope pattern deconvolution and calibration curve quantification methods for the determination of estrone and 17β-estradiol in human serum
Publication date: Available online 9 April 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): J. Pitarch-Motellón, N. Fabregat-Cabello, C. Le Goff, A.F. Roig-Navarro, J.V. Sancho-Llopis, E. CavalierAbstractA Liquid Chromatography coupled to tandem mass spectrometry (LC-MS/MS) based method have been developed for the determination of the main estrogen compounds –estrone (E1) and 17β-estradiol (E2)– in human serum. Two isotope dilution mass spectrometry (IDMS) quantification procedures have been used: a classical calibration curve-based method were compared to a recently developed...
Source: Journal of Pharmaceutical and Biomedical Analysis - April 10, 2019 Category: Drugs & Pharmacology Source Type: research

Pharmaceutical and preclinical evaluation of Advax adjuvant as a dose-sparing strategy for ant venom immunotherapy
Publication date: Available online 9 April 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Troy Wanandy, Yoshikazu Honda-Okubo, Noel W. Davies, Hayley E. Rose, Robert J. Heddle, Simon G.A. Brown, Richard Woodman, Nikolai Petrovsky, Michael D. WieseAbstractA major challenge in broader clinical application of Jack Jumper ant venom immunotherapy (JJA VIT) is the scarcity of ant venom which needs to be manually harvested from wild ants. Adjuvants are commonly used for antigen sparing in other vaccines, and thereby could potentially have major benefits to extend JJA supplies if they were to similarly enh...
Source: Journal of Pharmaceutical and Biomedical Analysis - April 10, 2019 Category: Drugs & Pharmacology Source Type: research

Rapid quantitative analysis of ginkgo flavonoids using paper spray mass spectrometry
Publication date: Available online 10 April 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Wei Zhou, Zihui Yang, Si Huang, Zhengfa Fang, Bo Chen, Ming MaAbstractIn this work, a method for the rapid and reliable analysis of ginkgo flavonoids was developed by using paper spray mass spectrometry (PS-MS) assisted by microwave-assisted hydrolysis (MAH). Kaempferol-D4, quercetin-D5, and isorhamnetin-D3 were used as internal standards (IS). Samples analyses were completed by simply treating with extraction, MAH, dilution, and quantitative analysis by PS-MS. Because of the absence of HPLC separation, the P...
Source: Journal of Pharmaceutical and Biomedical Analysis - April 10, 2019 Category: Drugs & Pharmacology Source Type: research