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Journal of Pharmaceutical and Biomedical Analysis

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https://www.readbyqxmd.com/read/29154197/investigation-of-the-effect-of-blood-hematocrit-and-lipid-content-on-the-blood-volume-deposited-by-a-disposable-dried-blood-spot-collection-device
#1
N Spooner, A Olatunji, K Webbley
When using dried blood spot (DBS) sampling for the quantitative bioanalysis of circulating concentrations of drugs, metabolites and endogenous analytes, it is important that a fixed volume of blood is deposited to overcome the issues associated with blood hematocrit (HCT) and homogeneity. The volumetric performance of the KTH DBS collection device was tested with radiolabelled [(14)C]-diclofenac. It was demonstrated that the device deposits a fixed volume of blood (13.5μL) regardless of the HCT (25-65%), or lipid content of the blood sample...
November 14, 2017: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/29145099/degradation-kinetics-study-of-1-palmitoyl-2-linoleoyl-3-acetyl-rac-glycerol-plag-by-a-validated-stability-indicating-rp-hplc-method
#2
Kyeong Soo Kim, Eun Su Yang, Dong Shik Kim, Dong Wuk Kim, Chul Soon Yong, Jong Oh Kim, Sung Giu Jin, Han-Gon Choi
The chemical stability of 1-palmitoyl-2-linoleoyl-3-acetyl-rac-glycerol (PLAG), a therapeutic agent for neutropenia, was investigated using a validated stability-indicating reversed phase high-performance liquid chromatographic (RP-HPLC) method. The forced degradation of PLAG was carried out under the stress conditions of hydrolysis (alkaline, acidic and various pH buffers), oxidation, photolysis and heat. A simple, sensitive, specific, robust, precise and accurate RP-HPLC method was developed and validated for evaluating the degradation kinetics of PLAG...
November 13, 2017: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/29154196/analysis-of-potential-genotoxic-impurities-in-rabeprazole-active-pharmaceutical-ingredient-via-liquid-chromatography-tandem-mass-spectrometry-following-quality-by-design-principles-for-method-development
#3
Katerina Iliou, Anđelija Malenović, Yannis L Loukas, Yannis Dotsikas
A novel Liquid Chromatography-tandem mass spectrometry (LC-MS/MS) method is presented for the quantitative determination of two potential genotoxic impurities (PGIs) in rabeprazole active pharmaceutical ingredient (API). In order to overcome the analytical challenges in the trace analysis of PGIs, a development procedure supported by Quality-by-Design (QbD) principles was evaluated. The efficient separation between rabeprazole and the two PGIs in the shortest analysis time was set as the defined analytical target profile (ATP) and to this purpose utilization of a switching valve allowed the flow to be sent to waste when rabeprazole was eluted...
November 12, 2017: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/29145098/a-novel-simplified-strategy-of-relative-quantification-n-glycan-quantitative-glycomics-using-electrospray-ionization-mass-spectrometry-through-the-stable-isotopic-labeling-by-transglycosylation-reaction-of-mutant-enzyme-endo-m-n175q
#4
Qing Shi, Ryugo Hashimoto, Tadamune Otsubo, Kiyoshi Ikeda, Kenichiro Todoroki, Hajime Mizuno, Dongri Jin, Toshimasa Toyo'oka, Zhe Jiang, Jun Zhe Min
The lack of a highly sensitive and simple method for the quantitative analysis of glycan has impeded the exploration of protein glycosylation patterns (glycomics), evaluation of antibody drug stability, and screening of disease glycan biomarkers. In this study, we describe a novel and simplified quantitative glycomics strategy. Quantitation by mutant enzyme reaction stable isotope labeling (QMERSIL) to label the N-glycans with either a nondeuterated (d0-) or deuterated (d8-) 4-(2,4-Dinitro-5-piperazin-1-yl-phenyl)-1,1-dimethyl-piperazin-1-ium (MPDPZ)-Boc-asparaginyl-N-acetyl-d-glucosamine (Boc-Asn-GlcNAc) acceptor of a positive charge structure through the glycosynthase (Endo-M-N175Q) transglycosylation reaction with mass spectrometry facilitates comparative glycomics...
November 12, 2017: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/29145096/sulfaguanidine-cocrystals-synthesis-structural-characterization-and-their-antibacterial-and-hemolytic-analysis
#5
Syed Sibte Asghar Abidi, Yasser Azim, Shahper Nazeer Khan, Asad U Khan
Sulfaguanidine (SG), belongs to the class of sulfonamide drug used as an effective antibiotic. In the present work, using crystal engineering approach two novel cocrystals of SG were synthesized (SG-TBA and SG-PT) with thiobarbutaric acid (TBA) and 1,10-phenanthroline (PT), characterized by solid state techniques viz., powder X-ray diffraction (PXRD), fourier transform infrared spectroscopy (FT-IR), differential scanning calorimetry (DSC) and the crystal structures were determined by single crystal X-ray diffraction studies...
November 11, 2017: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/29136591/direct-comparison-of-low-and-mid-frequency-raman-spectroscopy-for-quantitative-solid-state-pharmaceutical-analysis
#6
Tiina Lipiäinen, Sara J Fraser-Miller, Keith C Gordon, Clare J Strachan
This study considers the potential of low-frequency (terahertz) Raman spectroscopy in the quantitative analysis of ternary mixtures of solid-state forms. Direct comparison between low-frequency and mid-frequency spectral regions for quantitative analysis of crystal form mixtures, without confounding sampling and instrumental variations, is reported for the first time. Piroxicam was used as a model drug, and the low-frequency spectra of piroxicam forms β, α2 and monohydrate are presented for the first time...
November 11, 2017: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/29145097/lc-esi-ms-ms-determination-of-defactinib-a-novel-fak-inhibitor-in-mice-plasma-and-its-application-to-a-pharmacokinetic-study-in-mice
#7
Gurulingappa Hallur, Natarajan Tamizharasan, Suresh P Sulochana, Neeraj Kumar Saini, Mohd Zainuddin, Ramesh Mullangi
A sensitive, specific, selective and rapid LC-ESI-MS/MS method has been developed and validated for the quantification of defactinib in mice plasma using (13)C3,(15)N-tofacitinib as an internal standard (I.S.). Sample preparation was accomplished through a liquid-liquid extraction process. Baseline chromatographic resolution of defactinib and the I.S. was achieved on an Atlantis dC18 column using an isocratic mobile phase comprising 0.2% formic acid in water and acetonitrile (25:75, v/v) delivered at a flow rate of 0...
November 10, 2017: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/29132113/fluorometric-detection-of-protein-ligand-engagement-the-case-of-phosphodiesterase5
#8
Giulia Di Rocco, Ilaria Martinelli, Salvatore Pacifico, Remo Guerrini, Elena Cichero, Paola Fossa, Silvia Franchini, Silvia Cardarelli, Mauro Giorgi, Marco Sola, Glauco Ponterini
Phosphodiesterases (PDEs) regulate the intracellular levels of cAMP and cGMP. The great clinical success of the PDE5 inhibitors, Sildenafil (Viagra), Vardenafil (Levitra) and Tadalafil (Cialis) has led to an increasing interest for this class of enzymes. Recent studies have shown a correlation between tumor growth and PDE5 overexpression, making PDE5-selective inhibitors promising candidates for cancer treatment. The search for such inhibitors rests today on radioactive assays. In this work, we exploit the conserved catalytic domain of the enzyme and propose a faster and safer method for detecting the binding of ligands and evaluate their affinities...
November 10, 2017: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/29132111/characterization-of-global-metabolic-profile-of-rhodiola-crenulata-after-oral-administration-in-rat-plasma-urine-bile-and-feces-based-on-uhplc-ft-icr-ms
#9
Yanting Li, Yangyang Zhao, Xintong Li, Tianfeng Liu, Xiwei Jiang, Fei Han
Rhodiola crenulata has been widely used as a health food, antifatigue and antidepressant in China and many other countries for centuries. However, to date the metabolism of it in vivo still remains unclear. In this study, UHPLC-FT-ICR MS was used to analyze the major components and their metabolites in rats after oral administration of Rhodiola crenulata for the first time. A total of 179 constituents, including 37 prototype compounds and 142 metabolites (89 phase I metabolites and 53 phase II metabolites) were tentatively identified...
November 10, 2017: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/29154110/authentication-of-eleutherococcus-and-rhodiola-herbal-supplement-products-in-the-united-kingdom
#10
Markus Ruhsam, Peter M Hollingsworth
Siberian ginseng (Eleutherococcus senticosus, Araliaceae) and roseroot (Rhodiola rosea, Rosaceae) are popular herbal supplements which have been shown to improve resilience to conditions such as stress and exhaustion. Using DNA barcoding methods we tested 25 Siberian ginseng and 14 roseroot products which are widely available to UK customers to test whether the herbal ingredient stated on the label is also in the product. All Siberian ginseng supplements contained E. senticosus, however, 36% also contained an Eleutherococcus species other than E...
November 9, 2017: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/29149702/an-hplc-tandem-mass-spectrometry-for-quantification-of-et-26-hcl-and-its-major-metabolite-in-plasma-and-application-to-a-pharmacokinetic-study-in-rats
#11
Xu Chen, Wensheng Zhang, Sandy Rios, Miriam B Morkos, Xiaoli Ye, Gen Li, Xuehua Jiang, Zhijun Wang, Ling Wang
ET-26-HCl is a new analog of etomidate, a short-acting anesthetic drug, with less adrenal cortex inhibition. The pharmacokinetics of ET-26-HCl in rats needs to be determined for future clinical trials in human subjects. In order to facilitate the pharmacokinetic study, a liquid chromatography based tandem mass spectrometric (HPLC-MS/MS) method was developed and validated for quantification of ET-26-HCl and its major metabolite, ET-26-acid. These two compounds and gabapentin (internal standard) were extracted using a protein precipitation method with methanol and detected by Multiple Reaction Monitoring of m/z transition of 275...
November 8, 2017: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/29132112/raman-spectroscopy-as-a-pat-for-pharmaceutical-blending-advantages-and-disadvantages
#12
Daniela Riolo, Alessandro Piazza, Ciro Cottini, Margherita Serafini, Emilio Lutero, Erika Cuoghi, Lorena Gasparini, Debora Botturi, Iari Gabriel Marino, Irene Aliatis, Danilo Bersani, Pier Paolo Lottici
Raman spectroscopy has been positively evaluated as a tool for the in-line and real-time monitoring of powder blending processes and it has been proved to be effective in the determination of the endpoint of the mixing, showing its potential role as process analytical technology (PAT). The aim of this study is to show advantages and disadvantages of Raman spectroscopy with respect to the most traditional HPLC analysis. The spectroscopic results, obtained directly on raw powders, sampled from a two-axis blender in real case conditions, were compared with the chromatographic data obtained on the same samples...
November 8, 2017: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/29132110/comprehensive-phospholipid-and-sphingomyelin-profiling-of-different-brain-regions-in-mouse-model-of-anxiety-disorder-using-online-two-dimensional-hilic-rp-lc-ms-method
#13
Róbert Berkecz, Ferenc Tömösi, Tímea Körmöczi, Viktor Szegedi, János Horváth, Tamás Janáky
A novel online system including two-dimensional liquid chromatography coupled to high-resolution mass spectrometry (2D-LC/MS) was developed and applied for comprehensive phospholipid (PL) and sphingomyelin (SM) profiling of dorsal hippocampus (DHPC), ventral (VHPC) and prefrontal cortex (PFC) brain regions in a mouse model of anxiety disorder. In the first dimension, lipid classes were distinguished by hydrophilic interaction liquid chromatography (HILIC), while the second dimensional separation of individual PL and SM species was achieved by reversed-phase (RP) chromatography...
November 8, 2017: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/29128829/identification-of-the-binding-between-three-fluoronucleoside-analogues-and-fat-mass-and-obesity-associated-protein-by-isothermal-titration-calorimetry-and-spectroscopic-techniques
#14
Zhigang Li, Zechun Wang, Ning Wang, Xinxin Han, Wenquan Yu, Ruiyong Wang, Junbiao Chang
In this work, the interactions between fat mass and obesity-associated (FTO) protein and three fluoronucleoside analogues (three-member-ring compound (1a), five-member-ring compound (1b) and six-member-ring compound (1c)) have been investigated by fluorescence, ultraviolet-visible absorption spectroscopy, isothermal titration calorimetric (ITC) and molecular modeling. Analysis of fluorescence data showed that the binding between three analogues and FTO occurred via a static quenching mechanism. Both ITC and fluorescence results indicated that 1b is the strongest quencher...
November 8, 2017: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/29127907/synthesis-of-carbon-quantum-dots-doped-dummy-molecularly-imprinted-polymer-monolithic-column-for-selective-enrichment-and-analysis-of-aflatoxin-b1-in-peanut
#15
Guohuan Liang, Haiyun Zhai, Lu Huang, Xuecai Tan, Qing Zhou, Xiao Yu, Haidan Lin
In this study, a novel method was proposed to sensitively determine aflatoxin B1 (AFB1) in peanut sample by using a carbon quantum dots-coated dummy molecularly imprinted polymer (CDs-DMIP) monolithic column for pretreatment coupled with high performance liquid chromatography-fluorescence detection (HPLC-FLD). The CDs-DMIP monolithic column was prepared by in-situ polymerization in a water bath using 5,7-dimethoxycoumarin as dummy template molecule. The CDs-DMIP monolithic column was applied to determine AFB1 by HPLC-FLD...
November 8, 2017: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/29127905/dissolution-studies-of-metamizole-sodium-and-pseudoephedrine-sulphate-dosage-forms-comparison-and-correlation-of-electronic-tongue-results-with-reference-studies
#16
Małgorzata Wesoły, Marcin Zabadaj, Krzysztof Cal, Patrycja Ciosek-Skibińska, Wojciech Wróblewski
This work reports a critical evaluation of the results of the release of active substances (APIs) from novel pharmaceutical formulations provided by an electronic tongue system (ET). Detailed dissolution studies of modified-release granules used in pharmacotherapy containing metamizole sodium and pseudoephedrine sulphate were carried out. The impact of the dissolution-modifying excipients (carmellose sodium and hypromellose) on the dissolution process as well as on the outcomes of the sensor array of ion-selective electrodes was investigated...
November 8, 2017: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/29127904/pharmacokinetics-and-brain-uptake-study-of-novel-ampa-receptor-antagonist-perampanel-in-sd-rats-using-a-validated-uhplc-qtof-ms-method
#17
David Paul, Lingesh Allakonda, Amit Sahu, Shruti Surendran, Nanjappan Satheeshkumar
Perampanel (PER) is a novel AMPA receptor antagonist for antiepileptic therapy and is prospective for the treatment of other neurological disorders. A highly sensitive and rapid UHPLC-QTOF-MS method was developed for the quantification of PER in plasma/brain homogenate of SD rat with alogliptin as an internal standard (IS). Chromatographic separation was carried out on an Acquity UPLC HSS Cyano column (100mm×2.1mm, 1.8μm) using gradient mobile phase consisting of 0.1% formic acid and acetonitrile at a flow rate of 0...
November 8, 2017: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/29128830/metabolism-of-the-synthetic-cannabinoid-5f-py-pica-by-human-and-rat-hepatocytes-and-identification-of-biliary-analytical-targets-by-directional-efflux-in-sandwich-cultured-rat-hepatocytes-using-uhplc-hr-ms-ms
#18
Marie Mardal, Pieter Annaert, Carolina Noble, Marlies Oorts, Kristian Linnet
Analytical strategies for detecting drugs in biological samples rely on information on metabolism and elimination. 5F-PY-PICA belongs to the group of synthetic cannabinoids that are known to undergo excretion into the bile. The aims of this study were the in vitro identification of metabolites of 5F-PY-PICA and to determine which analytical targets are excreted into the bile and urine. Metabolites identified after incubation of 5F-PY-PICA with pooled human liver microsomes (pHLM), pooled human hepatocytes (pHH), or suspended and sandwich-cultured rat hepatocytes (SCRH)...
November 7, 2017: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/29127908/development-and-validation-of-a-stability-indicating-hplc-uv-method-for-the-determination-of-triamcinolone-acetonide-and-its-degradation-products-in-an-ointment-formulation
#19
A J P van Heugten, W de Boer, W S de Vries, C M A Markesteijn, H Vromans
A stability indicating high performance liquid chromatography method has been developed for the determination of triamcinolone acetonide (TCA) and its main degradation products in ointment formulations. The method, based on extensive stress testing using metal salts, azobisisobutyronitrile, acid, base and peroxide, showed that TCA undergoes oxidative degradation. All degradation products were identified using HPLC mass spectrometry. Separation and quantification was achieved using an Altima C18 RP18 HP column (250×4...
November 7, 2017: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/29154109/development-and-validation-of-a-sensitive-and-rapid-uhplc-ms-ms-method-for-the-simultaneous-quantification-of-the-common-active-and-inactive-metabolites-of-vicagrel-and-clopidogrel-in-human-plasma
#20
Cai Liu, Youming Lu, Hongbin Sun, Jin Yang, Yongqiang Liu, Xiaojuan Lai, Yanchun Gong, Xuefang Liu, Yongguo Li, Yifan Zhang, Xiaoyan Chen, Dafang Zhong
Vicagrel, an analog of clopidogrel, is a novel thienopyridine P2Y12 antagonist in clinical development in China for the treatment of acute coronary syndromes. Vicagrel and clopidogrel are prodrugs requiring metabolic activation to produce a pharmacologically active thiol metabolite (H4) in vivo. The formation of H4 from vicagrel in humans is promising more efficient and consistent than that from clopidogrel. After oral dosing of vicagrel or clopidogrel to humans, the active thiol metabolite H4 and two inactive metabolites closely related to H4 formation (the thiol metabolite H3 and the S-methylated metabolite SM3) were observed in plasma; SM3 was the most abundant drug-related component of vicagrel in circulation...
November 6, 2017: Journal of Pharmaceutical and Biomedical Analysis
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