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Journal of Pharmaceutical and Biomedical Analysis

Levan Megutnishvili, Nino Todua, Stephen Stein, Anzor Mikaia
A GC-MS method is described for the characterization of thebaol, a component of opium poppy. The method includes preliminary sample derivatization to TMS, TBDMS, TFA, PFP and HFB substituted products. Fragmentation of resulting derivatives is unique under electron ionization, and proceeds via consecutive loss of two radicals that violate the "even-electron rule". Peaks of [M-2CH3 ]+. and [M-C4 H9 -CH3 ]+. ions show maximum intensities in the spectra of trimethyl- and tert-butyldimethylsilyl-thebaols...
May 18, 2018: Journal of Pharmaceutical and Biomedical Analysis
Abeer H A Mohamed-Ahmed, Alastair Lockwood, Hala Fadda, Shivam Madaan, Peng T Khaw, Steve Brocchini, Kersti Karu
Ilomastat is a matrix metalloproteinase inhibitor (MMPi) that has shown the potential to inhibit scarring (fibrosis) by mediating healing after injury or surgery. A long lasting ocular implantable pharmaceutical formulation of ilomastat is being developed to mediate the healing process to prevent scarring after glaucoma filtration surgery. The ilomastat implant was coated with water permeable and biocompatible phosphoryl choline polymer (PC1059) displayed extended slow release of ilomastat in vitro and in vivo...
May 16, 2018: Journal of Pharmaceutical and Biomedical Analysis
S Raymundo, V V Muller, N B Andriguetti, M Tegner, A C Artmann, H M Kluck, M A Franzoi, R M M Vilela, G Schwartsmann, R Linden, M V Antunes
In this study, a LC-MS/MS method for the measurement of docetaxel in Dried Blood Spots (DBS) samples was developed and validated. Docetaxel was extracted from 8 mm DBS punch with a mixture of methanol and acetonitrile (9:1, v/v). The chromatographic separation occurred in an Acquity® C18 column (150 × 2.1 mm, 1.7 μm) eluted with a mixture of water and acetonitrile plus 0.1% formic acid (45:55, v/v). Total analytical run time was 7 min. The method was linear from 50 to 3000 ng ml-1 . Precision assays showed CV% < 9...
May 15, 2018: Journal of Pharmaceutical and Biomedical Analysis
Balasaheb B Chavan, Shristy Tiwari, Shankar G, Rakesh D Nimbalkar, Prabha Garg, Srinivas R, M V N Kumar Talluri
Palbociclib (PAB) is a CDK4/6 inhibitor and U. S Food and Drug Administration (FDA) granted regular approval for the treatment of hormone receptor (HR) positive, metastatic breast cancer in combination with an aromatase inhibitor in postmenopausal women. Metabolite identification is a crucial aspect during drug discovery and development as the drug metabolites may be pharmacologically active or possess toxicological activity. As there are no reports on the metabolism studies of the PAB, the present study focused on investigation of the in vitro and in vivo metabolic fate of the drug...
May 14, 2018: Journal of Pharmaceutical and Biomedical Analysis
Julian Hösl, André Gessner, Nahed El-Najjar
A simple and precise ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for the simultaneous analysis of five anti-infective agents used to treat severe infections [three antibiotics (daptomycin, moxifloxacin, ciprofloxacin) and two antifungals (isavuconazole, caspofungin)] in human plasma. Sample preparation was based on protein precipitation with ice cold methanol. All five agents were analyzed with the corresponding isotopically labeled internal standards. All analytes were detected in multiple reactions monitoring (MRM) using API 4000 triple-quadrupole mass spectrometer with electrospray (ESI) source operating in positive mode...
May 12, 2018: Journal of Pharmaceutical and Biomedical Analysis
Jeremy Carlier, Xingxing Diao, Marilyn A Huestis
Clandestine laboratories continue producing new synthetic cannabinoids that mimic and magnify natural cannabinoids effects to circumvent drug scheduling legislation. New synthetic cannabinoids are highly potent and responsible for many acute intoxications and deaths. Characterization of metabolic pathways is critical to identify metabolite markers whose detection can prove intake. BB-22 is a new potent synthetic cannabinoid whose toxicological and metabolic properties are currently unavailable. Analytical methods require constant updating and are challenging due to extensive synthetic cannabinoid metabolism and low marker concentrations...
May 7, 2018: Journal of Pharmaceutical and Biomedical Analysis
Long Yuan, Shenita Basdeo, Qin C Ji
BMS-986104 is a S1P1 R modulator drug candidate under development and has been evaluated in Phase I clinical trials. BMS-986104 functions as a prodrug and undergoes enzymatic transformations in vivo to form the pharmacologically active phosphate drug, BMS-986104-P. Here, we report approaches to overcome the stability, solubility and extraction challenges in developing a sensitive, accurate and rugged LC-MS/MS method for the simultaneous quantification of the phosphate drug and its prodrug in blood lysate. An effective stabilization strategy using a cocktail of phosphatase and kinase inhibitors was developed to ensure the stability of both analytes during sample collection, storage, and processing...
May 5, 2018: Journal of Pharmaceutical and Biomedical Analysis
Sara Tengattini, Francesca Rinaldi, Luciano Piubelli, Tom Kupfer, Benjamin Peters, Teodora Bavaro, Enrica Calleri, Gabriella Massolini, Caterina Temporini
One of the most popular enzymes used for the in vitro cleavage of fusion proteins is enterokinase (EK, E.C. EK cleaves with high specificity after the sequence Asp4 -Lys (DDDDK), which allows the fusion protein to preserve its native amino acid terminus without any additional unwanted cleavage residue from the recognition sequence. However, the complete removal of EK after protein cleavage is a critical step to ensure protein identity and stability. As enzyme immobilization increases stability and reusability of the biocatalyst while reducing operating costs and sample contamination, in this work we report the covalent immobilization of recombinant EK (rEK) on monolithic chromatographic supports with different binding chemistries for the development of a rEK-chromatographic-bioreactor...
May 4, 2018: Journal of Pharmaceutical and Biomedical Analysis
Mingya Ding, Zhen Li, Xie-An Yu, Dong Zhang, Jin Li, Hui Wang, Jun He, Xiu-Mei Gao, Yan-Xu Chang
This study aimed to clarify the difference between the effective compounds of raw and processed Farfarae flos using a network pharmacology-integrated metabolomics strategy. First, metabolomics data were obtained by ultra high-performance liquid chromatography-quadrupole-time of flight mass spectrometry (UHPLC-Q-TOF/MS). Then, metabolomics analysis was developed to screen for the influential compounds that were different between raw and processed Farfarae flos. Finally, a network pharmacology approach was applied to verify the activity of the screened compounds...
May 4, 2018: Journal of Pharmaceutical and Biomedical Analysis
Hamid Shirkhanloo, Sara Davari Ahranjani
A simple and applied method based on ultrasound assisted-Ionic liquid trap-micro solid phase extraction (USA-ILT-μSPE) was demonstrated for preconcentration/separation of lead (Pb) in human blood and urine samples. By proposed method, the amine-functionalized bimodal mesoporous silica nanoparticles (NH2 -UVM7 ) as solid phase sorbent was used for lead analysis in human biological samples at pH ≈ 7.0. After shaking/centrifuging of sample, the Pb (II) was extracted with NH2 -UVM7 without any chelating agents, trapped in ionic liquid phase and settled down in conical centrifuge tube as a residual solution [Pb→:NH2 -UVM7 ]...
May 4, 2018: Journal of Pharmaceutical and Biomedical Analysis
Bao Yang, Hui Li, Qing-Feng Ruan, Yuan-Yuan Xue, Di Cao, Xing-Hong Zhou, Shi-Qin Jiang, Tao Yi, Jing Jin, Zhong-Xiang Zhao
Ilex rotunda, in which triterpenoids and phenylpropanoids are major bioactive constituents, has been widely used in traditional Chinese medicines. In this study, a validated UPLC/Q-TOF-MS/MS method was developed to simultaneously identify and quantify the triterpenoids and phenylpropanoids in the stem bark, fruit, leaves, roots and stem xylem of this herbal medicine. A total of seventy triterpenoids and twelve phenylpropanoids were identified with the assistance of the modified mass defect filter and key product ion filter data processing strategies, and forty-eight of them were confirmed by reference substances...
May 3, 2018: Journal of Pharmaceutical and Biomedical Analysis
Jinfeng Chen, Jinlong Wang, Yingyuan Lu, Shaoyang Zhao, Qian Yu, Xuemei Wang, Pengfei Tu, Kewu Zeng, Yong Jiang
Neuroinflammation is a main factor in the pathogenesis of neurodegenerative diseases, such as Alzheimer disease. Our previous studies indicated that the modified Wuziyanzong Prescription (MWP) can suppress neuroinflammatory responses via nuclear factor-kappa B (NF-κB) and mitogen-activated protein kinases (MAPKs) signaling pathways. However, the anti-neuroinflammatory components of MWP remain unclear. Herein, a target-directed molecular docking fingerprint (TMDF) strategy, via integrating the chemical profiling and molecular docking approaches, was developed to identify the potential anti-neuroinflammatory components of MWP...
May 1, 2018: Journal of Pharmaceutical and Biomedical Analysis
Xin Huang, Xiaohui Lin, Lina Zhou, Benzhe Su
Feature relationships are complex and may contain important information. k top scoring pairs (k-TSP) studies feature relationships by the horizontal comparison. This study examines feature relationships and proposes vertical and horizontal k-TSP (VH-k-TSP) to identify the discriminative feature pairs by evaluating feature pairs based on the vertical and horizontal comparisons. Complexity is introduced to compute the discriminative abilities of feature pairs by means of these two comparisons. VH-k-TSP was compared with support vector machine-recursive feature elimination, relative simplicity-support vector machine, k-TSP and M-k-TSP on nine public genomics datasets...
May 1, 2018: Journal of Pharmaceutical and Biomedical Analysis
Mohammad Nabil Abo-Zeid, Samia M El-Gizawy, Noha N Atia, Salwa R El-Shaboury
Sofosbuvir (SOF) and daclatasvir (DCS) are newly discovered anti-hepatitis C drugs that have direct antiviral activity. A novel and simple high-performance thin-layer chromatography (HPTLC) method was designed for simultaneous determination of SOF and DCS in miscellaneous matrices. The method adopts coupling HPTLC with dual wavelength spectrodensitometry. Consequently, this enabled sensitive, specific and cost-effective determination of the SOF-DCS mixture. The developed HPTLC procedure is based on a simple liquid-liquid extraction, enrichment of the analytes and subsequent chromatographic separation with UV detection...
May 1, 2018: Journal of Pharmaceutical and Biomedical Analysis
Zhi-Lai Zhan, Ai-Ping Deng, Li-Ping Kang, Jin-Fu Tang, Tie-Gui Nan, Tong Chen, Ya-Li He, Lan-Ping Guo, Lu-Qi Huang
As a traditional processing method, sulfuring has been used in the processing of many traditional Chinese medicines (TCMs). Desulfuring, which has emerged in recent years, is a new method applied to sulfured herbs so they can comply with regulations regarding residual SO2 . Due to the chemical transformations and the residual SO2 in the herbs, both sulfuring and desulfuring have negative effects on the safety and therapeutic effects of TCMs, and Moutan Cortex is one of the TCMs most susceptible to these effects...
May 1, 2018: Journal of Pharmaceutical and Biomedical Analysis
Brian M Murphy, Tarik J Ozumerzifon, Charles S Henry, Mark Cornell Manning
Deamidation of asparagine (Asn) residues is one of the most common chemical degradation pathways observed in proteins. This reaction must be understood and controlled in therapeutic drug candidates, as chemical changes can affect their efficacy and safety. The analytical tools available for detection of deamidation reaction products, such as isoaspartic acid residues, are either chromatographic or electrophoretic, and require MS detection for absolute identification of peaks. High-throughput measurement of protein degradation has typically been limited to probing the target's physical state using spectroscopic techniques...
May 1, 2018: Journal of Pharmaceutical and Biomedical Analysis
Sandra Pimentel-Moral, Isabel Borrás-Linares, Jesús Lozano-Sánchez, David Arráez-Román, Antonio Martínez-Férez, Antonio Segura-Carretero
H. sabdariffa has demonstrated positive results against chronic diseases due to the presence of phytochemicals, mainly phenolic compounds. The extraction process of bioactive compounds increases the efficient collection of extracts with high bioactivity. Microwave-Assisted Extraction (MAE) constituted a "green technology" widely employed for plant matrix. In this work, the impact of temperature (50-150 °C), composition of extraction solvent (15-75% EtOH) and extraction time (5-20 min) on the extraction yield and individual compounds concentrations were evaluated...
May 1, 2018: Journal of Pharmaceutical and Biomedical Analysis
Takehito Inukai, Sanae Kaji, Hiroyuki Kataoka
Smoking not only increases the risk of lung cancer but is strongly related to the onset of cardiovascular disease. Particularly, passive smoking due to sidestream smoke is a critical public health problem. To assess active and passive exposure to tobacco smoke, we developed a simple and sensitive method, consisting of on-line in-tube solid phase microextraction (SPME) coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS), to determine nicotine and its metabolite cotinine in hair samples. These compounds were separated within 5 min using a Polar-RP80A column and detected in the positive ion mode by multiple reaction monitoring...
April 30, 2018: Journal of Pharmaceutical and Biomedical Analysis
Daniel Sironi, Jörg Rosenberg, Annette Bauer-Brandl, Martin Brandl
Here we report first experiences with the novel in vitro dissolution/permeation setup PermeaLoop™. It was designed to overcome current limitations of in vivo predictive dissolution testing of enabling formulations, such as lack of relevant absorptive drag to allow for meaningful interplay between dissolution and permeation, as it is occurring in vivo. We propose a novel setup with a high area-to-volume ratio and report as a model case the dissolution/permeation behavior of an enabling formulation of the poorly soluble and poorly permeable drug ABT-869...
April 28, 2018: Journal of Pharmaceutical and Biomedical Analysis
Naoual Kheyar-Kraouche, Andreia Bento da Silva, Ana Teresa Serra, Fatiha Bedjou, Maria R Bronze
Inula viscosa (I. viscosa) is a common Mediterranean plant, well known for its content on bioactive molecules. The chemical composition of an ethanolic extract from I. viscosa leaves, growing in Algeria, was analysed by liquid chromatography coupled to photodiode array detection and electrospray ionization mass spectrometry (LC-DAD-ESI-MS/MS) operating in negative and positive mode. The methodology used revealed the presence of 51 compounds from which 47 were putatively identified, including 11 phenolic acids, 23flavonoids, one lignan and 12 terpenoids...
April 27, 2018: Journal of Pharmaceutical and Biomedical Analysis
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