Structural Elucidation of a Dimeric Impurity in the Process Development of Ceftolozane using LC/HRMS and 2D-NMR
Publication date: Available online 26 May 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Jing Liao, Huaming Sheng, Josep Saurí, Rong Xiang, Gary MartinAbstractCeftolozane is MSD’s 5th generation cephalosporin antibiotic with broad-spectrum gram-negative activity. While refining the synthetic route to the drug substance, a dimeric impurity was observed in the final active pharmaceutical ingredient (API) of ceftolozane. Through impurity enrichment and preparative isolation, the structure of the impurity was subsequently established through LC/HRMS, HRMSMS, H/D exchange and 2D-NMR studies...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 27, 2019 Category: Drugs & Pharmacology Source Type: research

Determination of epoxide impurity in sarpogrelate hydrochloride intermediate by UHPLC and column-switching liquid chromatography
In this study, we resolved the problem by using the most common UV method with two ideas: one was to improve the absolute sensitivity, and the other was to reduce matrix effects. Both ultra high-performance liquid chromatography (UHPLC with high sensitivity LightPipe™ flow cells) and column-switching liquid chromatography methods were developed and validated for the quantitative determination of epoxide impurity in sarpogrelate hydrochloride intermediates. The limits of detection (LODs) of the UHPLC and column-switching liquid chromatography methods were 0.09 ppm (0.09 μg/g) and 0.33 ppm (0.33 μg/g), and the re...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 26, 2019 Category: Drugs & Pharmacology Source Type: research

UHPLC-HRMS study of Anti-Alzheimer’s drug candidates: metabolism of 7-MEOTA-tryptophan hybrids hampers their passage into brain
Publication date: Available online 24 May 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): M. Mžik, J. Karasová-Žďárová, K. Chalupová, J Korábečný, V. Palička, V. ŠestákAbstractBeing among the top five causes of death in the developed world, Alzheimer’s disease represents a major socio-economic issue. We administered a single intramuscular dose of two new hybrid anti-Alzheimer’s compounds, with 7-methoxytacrine (7-MEOTA; acetylcholinesterase inhibitor) and tryptophan (inhibitor of amyloid accumulation) in their structure, to rat...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 26, 2019 Category: Drugs & Pharmacology Source Type: research

Analysis of Artemisia annua extracts and related products by high performance liquid chromatography-tandem mass spectrometry coupled to sample treatment miniaturisation
Publication date: Available online 23 May 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Michele Protti, Roberto Mandrioli, Manuela Mandrone, Concettina Cappadone, Giovanna Farruggia, Ilaria Chiocchio, Emil Malucelli, Gloria Isani, Ferruccio Poli, Laura MercoliniABSTRACTArtemisinin, the main antimalarial compound of Artemisia annua L., is currently attracting increasing interest for its antiproliferative properties, but its content is highly variable, depending on several genetic, environmental and processing conditions. Aim of the present study is to analyse the artemisinin content in different pl...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 25, 2019 Category: Drugs & Pharmacology Source Type: research

Size-tunable Au@Ag nanoparticles for colorimetric and SERS dual-mode sensing of palmatine in traditional Chinese medicine
Publication date: Available online 22 May 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Yaohui Gao, Ziwei Hu, Jiamin Wu, Zan Ning, Jingyi Jian, Ting Zhao, Xiaochen Liang, Xingjie Yang, Zi Yang, Qinyu Zhao, Jianping Wang, Zhigang Wang, Nicoleta Elena Dina, Ana Maria Raluca Gherman, Zhengjin Jiang, Haibo ZhouAbstractPalmatine is a protoberberine alkaloid separated from several plants and application as an anti-inflammatory and antibacterial agent in the therapy of gastrointestinal and genitourinary disorder. Thus, the fast quantification of palmatine is important in clinic medical assays. Herein, we...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 23, 2019 Category: Drugs & Pharmacology Source Type: research

Development and validation of a UPLC-MS/MS method for quantification of doxofylline and its metabolites in human plasma
Publication date: Available online 22 May 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Li-Na Fang, Ming-Qing Mao, Xiao-Hua Zhao, Ling Yang, Hui Jia, Shu-Yue XiaAbstractA sensitive and specific ultraperformance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed and validated for simultaneous determination of doxofylline and its two metabolites in human plasma. After protein precipitation with methanol, the chromatographic separation was carried out on an ACQUITY UPLC HSS T3 column, with acetonitrile and 0.1% formic acid in water as mobile phase at a flow rate of 0.30&...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 23, 2019 Category: Drugs & Pharmacology Source Type: research

Simultaneous determination of multiple compounds of Da-Huang-Xiao-Shi decoction in rat plasma by LC-MS/MS and its application in a pharmacokinetic study
In this study, we developed a rapid, sensitive, and accurate LC-MS/MS method to simultaneously determine multiple, potentially bioactive compounds of DHXSD, including five alkaloids (berberine, phellodendrine, palmatine, jatrorrhizine, and magnoflorine), five anthraquinones (rhein, aloe-emodin, emodin, chrysophanol, and physcion), two iridoid glycosides (geniposide and genipin 1-gentiobioside), and one iridoid aglycone (genipin) in rat plasma. Plasma samples collected from rats were treated immediately with 5% acetic acid to avoid the degradation of genipin. After protein precipitation with acetonitrile containing 5% aceti...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 23, 2019 Category: Drugs & Pharmacology Source Type: research

Tissue distribution study of Angelica dahurica cv. Yubaizhi in rat by ultra–performance liquid chromatography with tandem mass spectrometry
Publication date: Available online 22 May 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): You-Bo Zhang, Gai-Gai Deng, Tian-Xia Wang, Lu Liu, Xiu-Wei YangAbstractA sensitive and specific ultra–performance liquid chromatographic–tandem mass (UPLC–MS/MS) spectrometric method was established to investigate tissue distribution of fourteen coumarins of Angelica dahurica cv. Yubaizhi roots (ADYR) in rat tissues, including isoimperatorin (1), imperatorin (2), isooxypeucedanin (3), byakangelicin (4), oxypeucedanin hydrate (5), bergapten (6), 2''R–neobyakangelicol (7), phellopterin (8)...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 23, 2019 Category: Drugs & Pharmacology Source Type: research

An integrated strategy based on characteristic fragment filter supplemented by multivariate statistical analysis in multi-stage mass spectrometry chromatograms for the large-scale detection and identification of natural plant-derived components in rat: the rhubarb case
Publication date: Available online 22 May 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Yang Xu, Li Zhang, Qing Wang, Gan Luo, Xiaoyan GaoAbstractAn integrated strategy based on characteristic fragment filter (CFF) supplemented by multivariate statistical analysis (MSA) for MSn chromatograms [(CFF)s MSA] was proposed for the large-scale detection of natural plant-derived ingredients in vivo. To prove the practicability of this [(CFF)s MSA] strategy, rhubarb was taken as an example. First, representative authentic standards of homologous components contained in rhubarb were chosen, from which the f...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 23, 2019 Category: Drugs & Pharmacology Source Type: research

Serial hyphenation of dried spot, reversed phase liquid chromatography, hydrophilic interaction liquid chromatography, and tandem mass spectrometry towards direct chemical profiling of herbal medicine-derived liquid matrices, an application in Cistanche sinensis
Publication date: Available online 22 May 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Qingqing Song, Zhizi Zhou, Jun Li, Yan Cao, Yunfang Zhao, Shuangbing Deng, Haijun Qi, Yong Jiang, Yuelin Song, Pengfei TuAbstractInspired by dried blood spots (DBS), “dried spots of herbal medicines” (DSHM) concept was proposed here. In response to this superior sampling means, a new platform integrating dried spot, serially coupled reversed phase liquid chromatography and hydrophilic interaction liquid chromatography (RPLC-HILIC), and tandem mass spectrometry (MS/MS), was configured for directly, c...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 23, 2019 Category: Drugs & Pharmacology Source Type: research

Chemical profiling, antioxidant, enzyme inhibitory and molecular modelling studies on the leaves and stem bark extracts of three African medicinal plants
This study attempts for the first time to highlight the pharmacological and phytochemical profile of extracts prepared from leaves and stem barks of three African plants (Macaranga hurifolia Beille, Sterculia tragacantha Lindl. and Zanthoxylum gilletii (De Wild.) P. G. Waterman. The extracts were tested for antioxidant and enzyme inhibitory effects. Free radical scavenging, metal chelator, reducing power and phosphomolybdenum assays were performed to evaluate antioxidant effects. To identify enzyme inhibitory effects, cholinesterases (acetylcholinesterase (AChE) and butrylcholinesterase (BChE)), tyrosinase, α-amylase...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 23, 2019 Category: Drugs & Pharmacology Source Type: research

3D cloves bud like Gd doped ZnO strewn rGO hybrid for highly selective determination of l-dopa in the presence of carbidopa and ascorbic acid
Publication date: Available online 23 May 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): N. Dhanalakshmi, T. Priya, V. Karthikeyan, N. ThinakaranAbstractAn electrochemical sensor using three dimensional (3D) cloves bud like gadolinium doped ZnO nanoflowers strewn reduced graphene oxide (GZO@rGO) modified glassy carbon electrode was proposed for the sensitive and selective detection of l-dopa. The GZO@rGO nanocomposite was synthesized by hydrothermal method and characterized by a variety of analytical and spectroscopy techniques, viz. Field Emission Scanning Electron Microscopy, X-Ray Diffraction, F...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 23, 2019 Category: Drugs & Pharmacology Source Type: research

Investigation of the mechanism of incompatible herb pair Gansui-Gancao-induced hepatotoxicity and nephrotoxicity and the attenuated effect of Gansuibanxia Decoction by UHPLC-FT-ICR-MS-based plasma metabonomic analysis
Publication date: Available online 21 May 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Yue Cui, Roujia Wang, Ye Zhang, Ting Liu, Fei Han, Ruiyun Li, Nan Zhang, Yunli Zhao, Yu ZhiguoAbstractGansui-Gancao is one of the “eighteen incompatible herb pairs” which was recorded 2000 years ago according to TCM (Traditional Chinese Medicine) theory for their toxicity when using together. Nevertheless, Gansuibanxia decoction contained the herb pair have satisfactory effect on the treatment of cancerous ascites, pericardial effusion, etc. The present study aimed to investigate the mechanism of th...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 22, 2019 Category: Drugs & Pharmacology Source Type: research

Liquid chromatography-tandem mass spectrometric assay for the quantification of galunisertib in human plasma and the application in a pre-clinical study
This study describes the development and validation of a bioanalytical assay to quantify galunisertib in human plasma using HPLC-MS/MS. Stable isotope labelled galunisertib was added as internal standard and the analyte and internal standard were extracted from the matrix by protein precipitation using acetonitrile-methanol (50:50, v/v). Final extracts were injected onto a C18 column, gradient elution was applied for chromatographic separation and detection was performed using a triple quadrupole mass spectrometer operating in the positive ion mode. The assay was linear over the range 0.05-10 ng/mL, with acceptable ...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 22, 2019 Category: Drugs & Pharmacology Source Type: research

Validated LC-MS/MS method for simultaneous quantification of seven components of Naodesheng in rat serum after oral administration and its application to a pharmacokinetic study
Publication date: Available online 21 May 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Lan Luo, Jiazhen Kang, Weijun Zhao, Yue Qi, Shengwang LiangABSTRACTA simple, precise and reliable LC-MS/MS method was developed and validated for simultaneous quantification of vitexin, notoginsenoside R1, hydroxysafflor yellow A, ginsenoside Rd, puerarin, daidzein and senkyunolide I as components of Naodesheng (NDS) in rat serum. The Linearity ranges in rat serum were 0.045 to 4.5 μg/mL for vitexin, 0.0476 to 4.76 μg/mL for notoginsenoside R1, 0.0422 to 4.22 μg/mL for hydroxysaffl...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 22, 2019 Category: Drugs & Pharmacology Source Type: research

A validated size exclusion chromatography method coupled with fluorescence detection for rapid quantification of bevacizumab in ophthalmic formulations
Publication date: Available online 22 May 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Feras Jirjees, Karim Soliman, Yujing Wang, Rahul Sonawane, Ravi Sheshala, David Jones, Thakur Raghu Raj SinghAbstractBevacizumab is a full-length human monoclonal antibody used to treat various neovascular diseases such as wet age-related macular degeneration (AMD), diabetic eye disease and other problems of the retina. Monthly intravitreal injections of bevacizumab (Avastin®) are effective in the treatment of wet AMD. However, there is a growing demand in the development of sustained release ophthalmic for...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 22, 2019 Category: Drugs & Pharmacology Source Type: research

Analysis of the fingerprint profile of bioactive constituents of traditional Chinese medicinal materials derived from animal bile using the HPLC–ELSD and chemometric methods: An application of a reference scaleplate
Publication date: Available online 22 May 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Jing Xiong, Tian-jiao Zheng, Yan Shi, Feng Wei, Shuang-cheng Ma, Lan He, Si-cen Wang, Xin-she LiuAbstractTraditional Chinese medicinal materials derived from animal bile are widely applied in clinical therapy for thousands of years in several Southeast Asian countries. Although the constituents are similar, these crude drugs exhibit different pharmacological activities; bile acids are the main bioactive constituent. Depending on the source, the price of these crude drugs differs significantly. Therefore, a reli...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 22, 2019 Category: Drugs & Pharmacology Source Type: research

UIISScan 1.1: A Field Portable High-throughput Platform Tool for Biomedical and Agricultural Applications
Publication date: Available online 22 May 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Subhankar Mukherjee, Souvik Pal, Abhra Pal, Devdulal Ghosh, Subrata Sarkar, Sunil Bhand, Priyabrata Sarkar, Nabarun BhattacharyyaAbstractThe colorimetric sensing technology has evolved into an essential tool for high-throughput analysis including portability and cost-effectiveness among available biomedical and agricultural screening approach. In this endeavor, the objective of work is to focus on the development of a field-portable instrument based on an uniform illumination imaging system (UIIS), which will f...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 22, 2019 Category: Drugs & Pharmacology Source Type: research

Simultaneous determination of 15 BTEX hydroxyl biomarkers in urine by headspace solid-phase microextraction gas chromatography–mass spectrometry
Publication date: Available online 20 May 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Jeong-Eeh Lee, Hyun-Hee Lim, Ho-Sang ShinAbstractBenzene (B), toluene (T), ethylbenzene (E), o-, m- and p-xylene (o-, m-, p-X) are ubiquitous and frequently exposed to human throughout the environment. Previously published test methods for phenolic biomarkers are not sensitive enough to be detected in most general population groups and require a lot of labor. A simple and convenient headspace solid-phase microextraction (HS-SPME) gas chromatography–mass spectrometry method was described for the simultaneo...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 22, 2019 Category: Drugs & Pharmacology Source Type: research

Anti-diarrhea effects and Identification of Musca domestica larvae Low Molecular Weight Peptides (LMWP)
Publication date: Available online 20 May 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Fujiang Chu, Xiaobao Jin, Hongyan MaAbstractMusca domestica larvae have been used clinically to cure children malnutritional stagnation and low molecular weight peptides (LMWP) of Musca domestica larvae showed more useful bioactivities. But there is no report on anti-diarrhea effects and identification of the LWMP. The purposes of this study were clarifying the anti-diarrhea effects by regulating intestinal microecology and identification of LMWP. In anti-diarrhea test, diarrhea mice were administered LMWP by o...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 22, 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...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 22, 2019 Category: Drugs & Pharmacology Source Type: research

Rapid and sensitive LC-MS/MS method for simultaneous quantification of capsaicin and dihydrocapsaicin in microdialysis samples following dermal application
Publication date: Available online 18 May 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Ricardo Lorenzoni, Fabiano Barreto, Renata Vidor Contri, Bibiana Verlindo de Araújo, Adriana Raffin Pohlman, Teresa Dalla Costa, Silvia Stanisçuaski GuterresAbstractA bioanalytical LC-MS/MS method was developed and validated for the simultaneous quantification of capsaicin (CAPS) and dihydrocapsaicin (D-CAPS) in dermal microdialysis samples from rats. Capsaicinoids were separated by using a C18 column, with a mobile phase of water and acetonitrile, both with 0.1% of formic acid, eluted as a gradie...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 20, 2019 Category: Drugs & Pharmacology Source Type: research

Quantitative Amino Acids Profile of Monofloral Bee Pollens by Microwave Hydrolysis and Fluorimetric High Performance Liquid Chromatography
Publication date: Available online 18 May 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Thomas Themelis, Roberto Gotti, Serena Orlandini, Rita GattiAbstractBee pollen is an attractive resource in the field of alternative remedies and thanks to the content of carbohydrates, crude fibers, proteins and lipids must be considered as a supplementary food of high potential rate. In characterization of bee pollen with the aim to define its value in human nutrition, the amino acids profile is one of the most important attribute. In the present study, the determination of amino acids composition of differen...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 18, 2019 Category: Drugs & Pharmacology Source Type: research

Determination of benzonatate and its metabolite in human plasma by HPLC–MS/MS: A preliminary pharmacokinetic study in healthy Chinese volunteers after oral administration of benzonatate soft capsule
In this study, two sensitive high-performance liquid chromatography-tandem mass spectrometry (HPLC–MS/MS) methods were developed and fully validated for the determination of the original 4-(butylamino)benzoic acid (method B) and total 4-(butylamino)benzoic acid (containing the original 4-(butylamino)benzoic acid and 4-(butylamino)benzoic acid converted from benzonatate after collection, method A). For both methods, one-step protein precipitation by methanol was performed to extract analytes from the plasma samples. Chromatographic separation was done on an InfinityLab Poroshell 120 Phenyl Hexyl column (2.1 mm&...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 17, 2019 Category: Drugs & Pharmacology Source Type: research

Influence of different extraction techniques on the chemical profile and biological properties of Anthemis cotula L.: Multifunctional aspects for potential pharmaceutical applications
Publication date: Available online 15 May 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Stefania Sut, Stefano Dall’Acqua, Gokhan Zengin, Ismail Senkardes, Gizem Bulut, Aleksandra Cvetanović, Alena Stupar, Anamarija Mandić, Carene Picot-Allain, Ahmet Dogan, Kouadio Ibrahime Sinan, Fawzi MahomoodallyAbstractThe phytochemical composition of different extracts obtained from stinking chamomile (Anthemis cotula L.) was investigated. Ethanol was used as solvent and accelerated solvent extraction (ASE), microwave assisted extraction (MAE), maceration, soxhlet extraction (SE), and ultrasound assist...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 15, 2019 Category: Drugs & Pharmacology Source Type: research

Quality by Design oriented development of hydrophilic interaction liquid chromatography method for the analysis of amitriptyline and its impurities
In this study, for method optimization a Box-Behnken design was used to test the effect of acetonitrile content, buffer concentration and pH of water phase on critical system responses such as retention factor of impurity A, resolution between impurity B and impurity C, amitriptyline peak asymmetry factor and retention time of last eluted impurity F. The defined mathematical models and Monte Carlo simulations were used to identify the design space. For robustness testing, fractional factorial design was applied. Optimal chromatographic conditions were the analytical column ZORBAX NH2 (250 mm x 4.6&thin...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 15, 2019 Category: Drugs & Pharmacology Source Type: research

Metabolomics coupled with integrative pharmacology reveal the protective effect of FangjiHuangqi Decoction against adriamycin-induced rat nephropathy model
In this study, a NMR based metabolomics approach coupled with biochemical assay and Western Blot had been employed to study the protective effect of FHD against adriamycin-induced nephropathy using rat model. And we proposed a integrative pharmacology-based method, which combined chemical ingredients database building, target identification and network analysis. These were aimed to decipher the mechanisms of action for the FHD in NS treatment. Multivariate analysis revealed that 13 of 16 perturbed metabolites could be reversed by FHD, and the MetaboAnalyst analysis revealed that the anti-nephrotic syndrome effect of FHD wa...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 15, 2019 Category: Drugs & Pharmacology Source Type: research

Simultaneous determination of diethyl phthalate and its major metabolite, monoethyl phthalate, in rat plasma, urine, and various tissues collected from a toxicokinetic study by ultrahigh performance liquid chromatography-tandem mass spectrometry
This study describes the development of a novel and sensitive UPLC-MS/MS method for simultaneous determination of diethyl phthalate (DEP) and its major metabolite, monoethyl phthalate (MEP), in rat plasma, urine, and 11 different tissues collected from a toxicokinetic study. Analytes were separated using 0.1% (v/v) aqueous formic acid and acetonitrile containing 0.1% (v/v) formic acid as a mobile phase by gradient elution at a flow rate of 0.25 mL/min with a KINETEX core-shell C18 column (50 × 2.1 mm, 1.7 μm). Quantitation was performed on a triple quadrupole mass spectrometer em...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 15, 2019 Category: Drugs & Pharmacology Source Type: research

Study of Anopheles gambiae 3-hydroxykynurenine transaminase activity and inhibition by LC-MS/MS method
Publication date: Available online 13 May 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Rossana Canavesi, Riccardo Miggiano, Martina Stella, Ubaldina Galli, Franca Rossi, Menico Rizzi, Erika Del GrossoAbstractIn Anopheles gambiae, the most efficient vector of the malaria parasite Plasmodium falciparum, 3-hydroxykynurenine is endowed with a toxic potential. In adult mosquitoes, the excess of 3-hydroxykynurenine is removed by a specific transaminase (3-hydroxykynurenine transaminase, HKT) which converts the compound into the more stable xanthurenic acid. Interfering with 3-hydroxykynurenine metaboli...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 15, 2019 Category: Drugs & Pharmacology Source Type: research

Retrospective multivariate analysis of pharmaceutical preparations using 1H nuclear magnetic resonance (NMR) spectroscopy: Example of 990 heparin samples
In this study multivariate analysis was performed on a big dataset of 990 NMR heparin spectra recorded over six years (2012–2017) in our laboratory. Several steps of statistical analysis of accumulated data were used to differentiate samples according to animal origin (bovine, porcine and ovine heparin), purity grade (crude and purified heparin), distributing company as well as to estimate their closeness to the heparin reference sample (SST) provided by US Pharmacopeia. The projection of new samples on these models can automatically forecast of all mentioned qualitative heparin properties within one minute.NMR data ...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 15, 2019 Category: Drugs & Pharmacology Source Type: research

Development and validation of a sensitive LC–MS/MS method for determination of gefitinib and its major metabolites in human plasma and its application in non-small cell lung cancer patients
In this study, we established and validated a method for determining gefitinib and its main metabolites, M605211, M387783, M537194 and M523595 in patients with non-small cell lung cancer (NSCLC) by liquid chromatography–tandem mass spectrometry (LC–MS/MS) method. The mobile phase was water: acetonitrile (35:65, v/v) with 0.1% formic acid at a flow‐rate of 0.35 mL/min, within a 3 min run time. Gefitinib and its main metabolites were separated on a X-Terra RP18 column (50 × 2.1 mm, 3.5 μm) at 40 ℃ and subjected to mass analysis using positive electro-spray io...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 15, 2019 Category: Drugs & Pharmacology Source Type: research

The contamination of valsartan and other sartans, part 1: New findings
Publication date: Available online 11 May 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Fritz Sörgel, Martina Kinzig, Mona Abdel-Tawab, Clemens Bidmon, André Schreiber, Steffen Ermel, Jonas Wohlfart, Axel Besa, Oliver Scherf-Clavel, Ulrike HolzgrabeAbstractIn July 2018 one of the bestselling antihypertensive agents valsartan manufactured in China was found to be contaminated by the “probably carcinogenic” nitrosamine N-nitrosodimethylamine (NDMA), followed by the detection of N-nitrosodiethylamine (NDEA) by us and others soon after. Our work also revealed that two additiona...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 12, 2019 Category: Drugs & Pharmacology Source Type: research

Simultaneous quantitation of E0703, a novel radioprotective agent and its oxidative metabolite M1 in human plasma by UPLC–MS/MS, and application to clinical pharmacokinetics
In conclusion, the validated method is accurate, sensitive and high-throughput, and can be successfully implemented for subsequent clinical pharmacokinetic studies of E0703 and M1. (Source: Journal of Pharmaceutical and Biomedical Analysis)
Source: Journal of Pharmaceutical and Biomedical Analysis - May 11, 2019 Category: Drugs & Pharmacology Source Type: research

Application of SPME supported by ionic liquids for the determination of biogenic amines by MEKC in clinical practice
Publication date: Available online 11 May 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Natalia Kossakowska, Ilona Olędzka, Alicja Kowalik, Natalia Miękus, Piotr Kowalski, Alina Plenis, Ewa Bień, Aleksandra Kaczorowska, Małgorzata Anna Krawczyk, Elżbieta Adamkiewicz-Drożyńska, Tomasz BączekAbstractThe analysis of biogenic amines (BAs) and their metabolites is helpful for the diagnosis of central nervous system disorders and other neuroendocrine and cancer disturbances. In the study, a developed micellar electrokinetic chromatography method, coupled with diode array detection (MEKC-DAD), wa...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 11, 2019 Category: Drugs & Pharmacology Source Type: research

Simultaneous Determination of Several Flavonoids and Phenolic Compounds in Nineteen Different Cephalaria species by HPLC-MS/MS
Publication date: Available online 9 May 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Nazli Boke Sarikahya, Ahmet C. Goren, Suheyla KirmizigulAbstractCephalaria species in Turkey known as “Pelemir” and they have many different biological activities due to their wide range of chemical content. The main goal of this study is determine the flavonoids and phenolic acids in Cephalaria species using high-performance liquid chromatography coupled with tandem mass spectrometry (HPLC-MS/MS). This method was developed for quantitation of reported compounds using reverse phase Fortis C18 (150&th...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 10, 2019 Category: Drugs & Pharmacology Source Type: research

Isotopic dilution method for bile acid profiling reveals new sulfate glycine-conjugated dihydroxy bile acids and glucuronide bile acids in serum
Publication date: Available online 9 May 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Maria M. Ulaszewska, Andrea Mancini, Mar Garcia-Aloy, Massimo Del Bubba, Kieran Micheal Tuohy, Urska VrhovsekAbstractAn ultrahigh performance liquid chromatography tandem mass spectrometry method (UHPLC-MS/MS) was developed for the determination of 41 target and 8 additional bile acids isomers (BAs) in biological fluids. BAs were analysed by solid-phase extraction on 50 µL biofluid-aliquots, followed by a properly optimised 27 min-chromatographic run. The method provided high sensitivity (lim...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 10, 2019 Category: Drugs & Pharmacology Source Type: research

Monitoring of organophosphate and pyrethroid metabolites in human urine samples by an automated method (TurboFlowTM) coupled to ultra-high performance liquid chromatography-Orbitrap mass spectrometry
Publication date: Available online 10 May 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Marina López-García, Roberto Romero-González, Antonia Garrido FrenichAbstractThere is a growing concern to pesticide exposure in humans, being the organophosphate (OP), carbamate and pyrethroid the most commonly used insecticides. Therefore, a fast, simple and automated screening method based on ultra-high performance liquid chromatography coupled to Orbitrap high resolution mass spectrometry (UHPLC-Orbitrap-MS) has been developed to determine six OPs metabolites (3,5,6-trichloro-2-pyridino...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 10, 2019 Category: Drugs & Pharmacology Source Type: research

Oxidative degradation pathways of beclabuvir hydrochloride mediated by hydrogen peroxide and UV/Vis light
Publication date: Available online 8 May 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Qingmei Ye, Yande Huang, Stephen Grier, Scott A. MillerAbstractBeclabuvir hydrochloride (BCV) is a marketed product for the treatment of hepatitis C viral infection. It contains functional groups such as indole, tertiary amine and amides. Forced degradation studies of BCV revealed different degradation profiles under photo and hydrogen peroxide oxidative conditions. Under the photo-oxidative degradation conditions, the tertiary amine on the piperazine ring was oxidized to form the degradants as the hydroxyl and ...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 9, 2019 Category: Drugs & Pharmacology Source Type: research

Use of capillary electrophoresis for the determination of impurities in preparations of fluorine-18 labelled PET radiopharmaceuticals
Publication date: Available online 7 May 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Dmitrii Antuganov, Yulija Antuganova, Tatiana Zykova, Raisa KrasikovaAbstractFluorine-18 labelled radiotracers are the most common diagnostic agents employed in positron emission tomography (PET). Despite well-established quality control (QC) procedures, introduction of new synthetic methods demands continuous development of analytical methodology. Here we propose capillary electrophoresis (CE) as a simple, fast and cost-efficient analytical method, allowing for the evaluation of potentially toxic impurities, in...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 8, 2019 Category: Drugs & Pharmacology Source Type: research

Use of cysteine as a spectroscopic probe for determination of heme-scavenging capacity of serum proteins and whole human serum
Publication date: Available online 7 May 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Rémi Noé, Nina Bozinovic, Maxime Lecerf, Sébastien Lacroix-Desmazes, Jordan D. DimitrovAbstractHeme serves as a prosthetic group of numerous proteins involved in the oxidative metabolism. As result of various pathological conditions associated with hemolysis or tissue damage, large quantities of hemoproteins and heme can be released extracellularly. Extracellular heme has pronounced pathogenic effects in hemolytic diseases, mediated by its pro-oxidative and pro-inflammatory activities. The p...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 8, 2019 Category: Drugs & Pharmacology Source Type: research

Optimized flash extraction and UPLC-MS analysis on antioxidant compositions of Nitraria sibirica fruit
Publication date: Available online 7 May 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Qianbo Song, Xiao Xia, Chongmin Ji, Daofeng Chen, Yan LuAbstractThe fruit of Nitraria sibirica Pall. (N. sibirica) is a common folk medicine in the Northwest China and contains plentiful antioxidant compositions. In the study, a rapid flash extraction method (extracting for 3.3 min with 53% ethanol at the solvent-sample ratio of 34 mL/g) for the antioxidant compositions in N. sibirica fruit was optimized by response surface methodology. Twenty-seven compounds of the extract were recognized by ultra...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 8, 2019 Category: Drugs & Pharmacology Source Type: research

The qualitative and quantitative analyses of Gelsemium elegans
This study aimed to comprehensively assess the quality of G. elegans samples including different plant parts and origins using ultra high-performance liquid chromatography coupled with photo-diode array and quadrupole time-of-flight mass spectrometry (UHPLC-PDA-QTOF/MS) and high-performance liquid chromatography coupled with UV detector (HPLC-UV). Firstly, the UHPLC-PDA-QTOF/MS approach was developed for the characterization of alkaloids in G. elegans and understanding the differences between multiple groups of samples. Based on the exact mass information, the fragmentation characteristics and the retention time of compoun...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 8, 2019 Category: Drugs & Pharmacology Source Type: research

Editorial Board
Publication date: 15 July 2019Source: Journal of Pharmaceutical and Biomedical Analysis, Volume 171Author(s): (Source: Journal of Pharmaceutical and Biomedical Analysis)
Source: Journal of Pharmaceutical and Biomedical Analysis - May 8, 2019 Category: Drugs & Pharmacology Source Type: research

Development of simple isocratic HPLC methods for siRNA quantitation in lipid-based nanoparticles
Publication date: 5 August 2019Source: Journal of Pharmaceutical and Biomedical Analysis, Volume 172Author(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 conditi...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 8, 2019 Category: Drugs & Pharmacology Source Type: research

Tuning selectivity in cation-exchange chromatography applied for monoclonal antibody separations, part 2: evaluation of recent stationary phases
Publication date: Available online 5 May 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Amarande Murisier, Evelin Farsang, Krisztián Horváth, Matthew Lauber, Alain Beck, Davy Guillarme, Szabolcs FeketeAbstractIn this second part of the series, recently commercialized cation exchanger stationary phases were systematically investigated for their capabilities to separate therapeutic monoclonal antibodies. It was demonstrated that the different combinations of stationary and mobile phases result in diverse retention, selectivity and efficiency. Hence, the whole phase system (combination o...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 6, 2019 Category: Drugs & Pharmacology Source Type: research

Elucidation of the absolute configuration of a tadalafil analogue found as adulterant in a health supplement by mass spectrometry, chiroptical methods and NMR spectroscopy
Publication date: Available online 5 May 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Chee-Leong Kee, Lee-Cheng Chin, Nuan-Ping Cheah, Xiaowei Ge, Min-Yong LowAbstractThe chirality of a dipropylaminopretadalafil stereoisomer isolated from a health supplement has been studied. Under high resolution mass spectrometry (HRMS) study, this unknown compound seems to be one of the trans configuration tadalafil analogues i.e. (6S, 12aR) or (6R, 12aS), owing to the same precursor ion at m/z 492 with mass errors within ±2 ppm tolerance and very close retention times. Moreover, the MS2 fragment...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 6, 2019 Category: Drugs & Pharmacology Source Type: research

An immunosensing device based on inhibition of mediator's Faradaic process for early diagnosis of prostate cancer using bifunctional nanoplatform reinforced by carbon nanotube
In this study, a simple and lable-free voltammetric immunosensor was successfully developed for the ultrasensitive detection of prostate specific antigen (PSA). To do this, multiwalled carbon nanotube (MWCNT)/L-histidine functionalized reduced graphene oxide (His-rGO) was demonstrated as a bifunctional nanoplatform for covalently attaching thionine redox indicator and anti-PSA antibody (Ab). The MWCNT enhanced electrical conductivity and facilitated the electron transfer between thionine and the glassy carbon electrode. While, the presence of anti-PSA antibody blocked the electron transfer of thionine and decreased redox s...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 6, 2019 Category: Drugs & Pharmacology Source Type: research

Determination of Oligonucleotide Deamination by High Resolution Mass Spectrometry
Publication date: Available online 6 May 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Claus Rentel, Jaimie DaCosta, Stilianos Roussis, Jonathan Chan, Daniel Capaldi, Bao MaiAbstractA novel analytical approach capable of measuring deaminated degradation products of oligonucleotide therapeutics is described. The method employs high-resolution mass spectrometry to assess the shift in isotopic distribution that accompanies deamination. Isotopic Distribution Factors (IDF), derived directly from the peak heights of the isotopic pattern, are employed to measure deamination levels of as little as 0.5%. R...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 6, 2019 Category: Drugs & Pharmacology Source Type: research

A novel biostructure sorbent based on CysSB/MetSB@MWCNTs for separation of nickel and cobalt in biological samples by ultrasound assisted-dispersive ionic liquid-suspension solid phase micro extraction
Publication date: Available online 4 May 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Hamid Shirkhanloo, Zeynab Karamzadeh, Jamshid Rakhtshah, Negar Motakef KazemiAbstractAn efficient method based on CysSB/MetSB@MWCNTs as a novel bio structure material was used for determination/separation of nickel and cobalt (Ni and Co) in human samples by ultrasound assisted-dispersive ionic liquid-suspension solid phase micro extraction (USA-DIL-SSPME). In this procedure, CysSB/MetSB@MWCNTs suspended in 1-butyl-2,3-dimethylimidazolium hexafluorophosphate ([BDMIM][PF6]) and mixture dispersed to 10 mL of...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 5, 2019 Category: Drugs & Pharmacology Source Type: research

Development and validation of an absolute protein assay for the simultaneous quantification of fourteen CYP450s in human microsomes by HPLC-MS/MS-based targeted proteomics
Publication date: Available online 4 May 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Alexia Grangeon, Valerie Clermont, Azemi Barama, Fleur Gaudette, Jacques Turgeon, Veronique MichaudAbstractThe cytochrome P450 (CYP450) superfamily constitutes the major enzymatic system involved in drug metabolism. CYP450 s are highly expressed in the liver and other tissues and limited data on absolute characterization of CYP450 s in extra hepatic organs, such as the small intestine, are available. Our objective was to develop and validate an absolute quantification assay by HPLC-MS/MS-based targ...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 5, 2019 Category: Drugs & Pharmacology Source Type: research