Simultaneous determination of alkaloids dicentrine and sinomenine in Stephania epigeae by 1H NMR spectroscopy
Publication date: Available online 6 August 2018Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Jian-Wei Dong, Xue-Jiao Li, Le Cai, Jun-You Shi, Yu-Feng Li, Cui Yang, Zhen-Jie LiAbstractStephania epigaea Lo is an important herbal medicine used as antiphlogistic and analgesic drugs. Its major components are dicentrine (1) and sinomenine (2). In the present study, a rapid, accurate, and precise method for simultaneous quantitation of dicentrine (1) and sinomenine (2) in S. epigeae using 1H NMR spectra was developed. The deuterated solvent of DMSO-d6 enabled satisfactory separation of the signals to be int...
Source: Journal of Pharmaceutical and Biomedical Analysis - August 7, 2018 Category: Drugs & Pharmacology Source Type: research

Diffusion-ordered spectroscopy on a benchtop spectrometer for drug analysis
Publication date: Available online 6 August 2018Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Gaëtan Assemat, Boris Gouilleux, Dylan Bouillaud, Jonathan Farjon, Véronique Gilard, Patrick Giraudeau, Myriam Malet-MartinoAbstractThe first reported two-dimensional diffusion-ordered spectroscopy (DOSY) experiments were recorded at low field (LF) on a benchtop NMR spectrometer using the BPP-STE-LED (bipolar pulse pair-stimulated echo sequence with a longitudinal eddy current delay) pulse sequence which limits phase anomalies and baseline discrepancies. A LF DOSY map was first obtained from a sol...
Source: Journal of Pharmaceutical and Biomedical Analysis - August 7, 2018 Category: Drugs & Pharmacology Source Type: research

Recent developments in green membrane-based extraction techniques for pharmaceutical and biomedical analysis
Publication date: Available online 6 August 2018Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Hadi Tabani, Saeed Nojavan, Michal Alexovič, Ján SaboAbstractMonitoring of target analytes (e.g., pharmaceuticals, endogenous compounds) present in biological samples usually requires a preliminary step toward analyte isolation from surrounding matrix and enrichment for trace analysis. Evident developments have been recently made to introduce novel “green” analytical approaches (which keep the requirements of Green Analytical Chemistry – GAC) being effective, economical, eco-friendly...
Source: Journal of Pharmaceutical and Biomedical Analysis - August 7, 2018 Category: Drugs & Pharmacology Source Type: research

Analytical methods for the study of bioactive compounds from medicinally used Echinacea species
Publication date: Available online 6 August 2018Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Renato Bruni, Virginia Brighenti, Lindsay K. Caesar, Davide Bertelli, Nadja B. Cech, Federica PellatiAbstractEchinacea purpurea (L.) Moench, Echinacea angustifolia DC. var. angustifolia and Echinacea pallida (Nutt.) Nutt. are frequently used as medicinal plants and their preparations are among the most widely used herbal medicines. The extracts from these species have shown a highly complex chemical composition, including polar compounds (caffeic acid derivatives, CADs), non-polar compounds (alkylamides and a...
Source: Journal of Pharmaceutical and Biomedical Analysis - August 7, 2018 Category: Drugs & Pharmacology Source Type: research

Study of the interaction of broad-spectrum antimicrobial drug sitafloxacin with human serum albumin using spectroscopic methods, molecular docking, and molecular dynamics simulation
This study are useful for further drug development, in vivo toxicity studies, and can provide guidance for the clinical application of STFX to study its pharmacokinetic properties.Graphical abstract (Source: Journal of Pharmaceutical and Biomedical Analysis)
Source: Journal of Pharmaceutical and Biomedical Analysis - August 4, 2018 Category: Drugs & Pharmacology Source Type: research

Simultaneous optimization of mobile phase composition and pH using retention modeling and experimental design
Publication date: Available online 2 August 2018Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Norbert Rácz, Imre Molnár, Arnold Zöldhegyi, Hans-Jürgen Rieger, Róbert KormányAbstractChromatographic methods are progressing continuously. Increasing sample complexity and safety expectations lead to higher regulatory demands, hence challenges in liquid chromatography analysis are rising, even today, when faster and faster chromatographic systems are extensively employed and become widely accessible for successful method development.The goal of this study was to investi...
Source: Journal of Pharmaceutical and Biomedical Analysis - August 3, 2018 Category: Drugs & Pharmacology Source Type: research

Development of a double-antibody sandwich ELISA for rapid detection to C-peptide in human urine
Publication date: Available online 2 August 2018Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Rui Lv, Yingshan Chen, Nana Xia, Yuxin Liang, Qiyi He, Minyou Li, Zongxian Qi, Yeyu Lu, Suqing ZhaoAbstractC-peptide level is recognized as an important indicator of diabetes diagnosis. A sensitive and specific double-antibody sandwich enzyme-linked immunosorbent assay for the detection of C-peptide based on double antibody sandwich method was studied in this paper. The rabbit and hen were innunized with PLL-C-peptide and BSA-C-peptide respectively to obtain specific Yolk antibody (IgY) and polyclonal antibod...
Source: Journal of Pharmaceutical and Biomedical Analysis - August 3, 2018 Category: Drugs & Pharmacology Source Type: research

Effects of Dibutyl phthalate and Di(2-ethylhexyl) phthalate with their metabolites on CYP2C9*1 and CYP2C19*1 activities in vitro
In this study, recombinant CYP2C9*1 and CYP2C19*1 microsomes were used to investigate the effects of phthalates and their metabolites on corresponding enzyme activities in vitro. 2-100 μM substrate of enzyme was incubated with series concentration of phthalates for 30 min at 37 °C. The metabolic products were detected using ultra-high performance liquid chromatography (UHPLC) and ultra-high performance liquid chromatography-mass spectrometry (UHPLC-MS/MS) methods. The results showed dibutyl phthalate (DBP) significantly inhibited CYP2C9*1 with an activity inhibition rate of 67.3% and half-maxima...
Source: Journal of Pharmaceutical and Biomedical Analysis - August 3, 2018 Category: Drugs & Pharmacology Source Type: research

An attempt to characterize the human Chorionic Gonadotropin protein by reversed phase liquid chromatography coupled with high-resolution mass spectrometry at the intact level
Publication date: Available online 2 August 2018Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Julien Camperi, Audrey Combes, Jean Guibourdenche, Davy Guillarme, Valerie Pichon, Thierry Fournier, Nathalie DelaunayAbstractFor the first time, the human Chorionic Gonadotropin (hCG) hormone at the intact level was characterized by reversed phase liquid chromatography (RPLC) coupled with high resolution mass spectrometry (HRMS). This heterodimeric protein is specific to human pregnancy, consists in an α and a β subunit, so-called hCGα and hCGβ, respectively, and has 8 glycosylation sit...
Source: Journal of Pharmaceutical and Biomedical Analysis - August 3, 2018 Category: Drugs & Pharmacology Source Type: research

Multiresidue determination of 21 pharmaceuticals in crayfish (Procambarus Clarkii) using enzymatic microwave-assisted liquid extraction and ultrahigh-performance liquid chromatography - triple quadrupole mass spectrometry analysis
Publication date: Available online 2 August 2018Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Julia Kazakova, Rut Fernández-Torres, María Ramos-Payán, Miguel Ángel Bello-LópezAbstractIn this paper, a multiresidue enzymatic-microwave assisted extraction prior to ultrahigh performance liquid chromatography and triple quadrupole mass spectrometry analysis has been developed for the determination of 21 pharmaceuticals in crayfish (Procambarus Clarkii) samples. The analysed compounds corresponding to 6 therapeutic families were: fluoroquinolones (ciprofloxacin, danofloxac...
Source: Journal of Pharmaceutical and Biomedical Analysis - August 3, 2018 Category: Drugs & Pharmacology Source Type: research

Ultrahigh-Performance Liquid Chromatography-Tandem Mass Spectrometry (UHPLC-MS/MS) Assay for Simultaneous Quantifications of CZ48, Lactone-stabilized Camptothecin, and Camptothecin and Their Pharmacokinetic and Biliary Evaluations in Rats
In this study, a UHPLC-MS/MS method was developed and validated to simultaneously quantify CZ48 and CPT in rat plasma and bile. Detection was performed using the API 3200 Q Trap triple quadrupole mass spectrometer in a positive ion mode. Chromatographic separation was achieved on Waters ACQUITY UPLC BEH Shield RP18 column with a gradient elution at a flow rate of 0.45 ml/min, using mobile phases of 0.1% acetic acid in water (A) and 0.1% acetic acid in acetonitrile (B). The method was linear at the concentration ranges of 0.98 (LLOQ) – 1,000 ng/ml of CZ48 and CPT in rat plasma and 3.9 (LLOQ) – 1,00...
Source: Journal of Pharmaceutical and Biomedical Analysis - August 3, 2018 Category: Drugs & Pharmacology Source Type: research

Simultaneous quantification of cannabinoids tetrahydrocannabinol, cannabidiol and CB1 receptor antagonist in rat plasma: An application to characterize pharmacokinetics after passive cannabis smoke inhalation and co-administration of rimonabant
Publication date: 25 October 2018Source: Journal of Pharmaceutical and Biomedical Analysis, Volume 160Author(s): Abhigyan Ravula, Hardik Chandasana, Barry Setlow, Marcelo Febo, Adriaan W. Bruijnzeel, Hartmut DerendorfAbstractA highly sensitive and selective liquid chromatography-tandem mass spectrometry method for the determination of tetrahydrocannabinol (THC), cannabidiol, and rimonabant in rat plasma was developed. Analytes and the internal standard were extracted from plasma using a combination of protein precipitation followed by liquid-liquid extraction. Chromatographic separation was done using Waters Symmetry C18, ...
Source: Journal of Pharmaceutical and Biomedical Analysis - August 3, 2018 Category: Drugs & Pharmacology Source Type: research

Immobilized enzyme-based analytical tools in the -omics era: recent advances
Publication date: Available online 31 July 2018Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Marina Naldi, Anna Tramarin, Manuela BartoliniAbstractProtein analysis is a field under rapid development mainly thanks to technological advances which have granted miniaturization of analytical devices, automation and higher detection sensitivity. The interest in the field has paralleled the expansion of the -omics era, laying down the bases for the current proteomic and glycomic applications. Advances in protein sample transformation prior to analysis have led to limitation in sample consumption and contamin...
Source: Journal of Pharmaceutical and Biomedical Analysis - August 1, 2018 Category: Drugs & Pharmacology Source Type: research

Phytochemical profile of Euphorbia peplus L. collected in Central Italy and NMR semi-quantitative analysis of the diterpenoid fraction
Publication date: Available online 31 July 2018Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Claudio Frezza, Alessandro Venditti, Fabio Sciubba, Pierpaolo Tomai, Marika Antonetti, Marco Franceschin, Maria Enrica Di Cocco, Alessandra Gentili, Maurizio Delfini, Mauro Serafini, Armandodoriano BiancoAbstractIn this work, the phytochemical profile of the ethanolic extract of Euphorbia peplus L. collected in Central Italy, was reported. This specimen had never been studied before and the analysis was accomplished by means of Column Chromatography for the separation procedure and by means of NMR Spectroscopy...
Source: Journal of Pharmaceutical and Biomedical Analysis - August 1, 2018 Category: Drugs & Pharmacology Source Type: research

Volatile component interaction effects on compatibility of Cyperi Rhizoma and Angelicae Sinensis Radix or Chuanxiong Rhizoma by UPLC-MS/MS and response surface analysis
Publication date: Available online 31 July 2018Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Pei Liu, Er-xin Shang, Yue Zhu, Da-wei Qian, Jin-ao DuanABSTRACTCyperi Rhizoma (Xiangfu) combined with either Angelicae Sinensis Radix (Danggui) or Chuanxiong Rhizoma (Chuanxiong) are herb pairs that are commonly used in clinical settings. To illustrate the herb–herb interactions that occur when extracts from these herbs are obtained together, ultra-high-performance liquid chromatography coupled with triple quadrupole electrospray tandem mass spectrometry and response surface analysis were used. Volatile...
Source: Journal of Pharmaceutical and Biomedical Analysis - August 1, 2018 Category: Drugs & Pharmacology Source Type: research

Quantitation of Residual Host Cell DNA in Protamine Sulfate Drug Product by qPCR Assay
Publication date: Available online 31 July 2018Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Cynthia Sommers, Barry Rosenzweig, Lida Oum, Karol Thompson, David A. KeireAbstractProtamine sulfate (PS) is an FDA approved drug used to reverse heparin-induced anticoagulation in patients. Protamine sulfate is a mixture of primarily four ~4 kDa arginine-rich cationic polypeptide chains derived from chum (Oncorhynchus keta) salmon sperm. Because the presence of residual host cell salmon DNA (resDNA) in PS drug product can pose safety concerns, processing steps during PS manufacturing are designed to ta...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 31, 2018 Category: Drugs & Pharmacology Source Type: research

Risk-based approach for method development in pharmaceutical quality control context: A critical review
Publication date: Available online 30 July 2018Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Riccardo Deidda, Serena Orlandini, Philippe Hubert, Cédric HubertAbstractPharmaceutical regulatory bodies increasingly require the implementation of systematic approaches in pharmaceutical product development. Quality control methods play a key role in the control strategy of drugs manufacturing to assure their quality. A risk-based approach in the analytical method development is strongly recommended to ensure that the method performances fit the purpose of the method during its entire life-cycle. In t...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 31, 2018 Category: Drugs & Pharmacology Source Type: research

Quantitative Analysis of a Pharmaceutical Formulation: Performance Comparison of Different Handheld Near-Infrared Spectrometers
Publication date: Available online 30 July 2018Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Hui Yan, Heinz W. SieslerAbstractNotwithstanding the first developments of miniaturized vibrational spectrometers more than a decade ago, only recently real handheld near-infrared (NIR) spectrometers (
Source: Journal of Pharmaceutical and Biomedical Analysis - July 31, 2018 Category: Drugs & Pharmacology Source Type: research

Investigating the utility of minimized sample preparation and high-resolution mass spectrometry for quantification of monoclonal antibody drugs
In this study, we investigate the capabilities of high-resolution MS instruments for circumventing the complex sample preparation currently needed for sensitive LC–MS/MS-based quantification of mAbs. Employing a simple one-step sample pre-treatment workflow, we compare the ability of three different LC–MS platforms for absolute quantification of a representative monoclonal antibody Rendomab-B1 in serum and plasma. The samples are subjected to protein precipitation with methanol, followed by pellet digestion with trypsin prior to LC–MS analysis. AQUA peptides based on two surrogate mAb peptides selected fr...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 31, 2018 Category: Drugs & Pharmacology Source Type: research

UHPLC-MS/MS method for determination of atorvastatin calcium in human plasma: Application to a pharmacokinetic study based on healthy volunteers with specific genotype
Publication date: Available online 30 July 2018Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Binbin Xia, Yali Li, Yatong Zhang, Ming Xue, Xiaorong Li, Pingxiang Xu, Tao Xia, Shicai ChenAbstractA rapid, selective and sensitive ultra high performance liquid chromatography coupled with tandem triple quaternary mass spectrometry (UHPLC-MS/MS) method was developed and validated for the quantitative determination of atorvastatin calcium (AC) in human plasma. Separation of AC and rosuvastatin calcium (internal standard, IS) were achieved on a Dikma Leapsil C18 reversed phase column (100 ×&thinsp...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 30, 2018 Category: Drugs & Pharmacology Source Type: research

Development and validation of a rapid ultra-high performance liquid chromatography diode array detector method for Verbena officinalis L
This study presents a fast and validated ultra-high performance liquid chromatography diode array detector (UHPLC-DAD) method for the simultaneous determination of the major compounds in Verbena officinalis L. (Verbenaceae), a medicinal plant listed in the European, British, and, Chinese Pharmacopoeias. In order to get reference substances, nine compounds, belonging to iridoids, flavonoids, and phenylpropanoid glycosides, were isolated from the herb extract. Two of them, namely cistanoside D and leucosceptoside A, were found in this plant species for the first time. Chromatographic separation was achieved in less than 7&th...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 28, 2018 Category: Drugs & Pharmacology Source Type: research

Characterization of polydisperse macrogols and macrogol-based excipients via HPLC and charged aerosol detection
Publication date: Available online 27 July 2018Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Christiane Theiss, Ulrike HolzgrabeAbstractMacrogol-based emulsifiers and their respective precursor substances, i.e. macrogols (PEG), fatty acids (FA), and fatty alcohols (FAA), are widely used excipients which are usually characterized by a series of tests described within the European Pharmacopoeia (Ph. Eur.). Examples are bulk parameters such as the hydroxyl value, the peroxide value, and the determination of fatty acids composition by gas chromatography. The choice of tests depends on the emulsifier consi...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 28, 2018 Category: Drugs & Pharmacology Source Type: research

Metabolite profiling of “green” extracts of Corylus avellana leaves by 1H NMR spectroscopy and multivariate statistical analysis
Publication date: Available online 26 July 2018Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Antonietta Cerulli, Milena Masullo, Paola Montoro, Jan Hošek, Cosimo Pizza, Sonia PiacenteAbstractCorylus avellana L. (Betulaceae) leaves, consumed as infusion, are used in traditional medicine, for the treatment of hemorrhoids, varicose veins, phlebitis, and edema due to their astringent, vasoprotective, and antiedema properties. In previous works we reported from the leaves of Corylus avellana cv. “Tonda di Giffoni” diarylheptanoid derivatives, a class of plant secondary metabolites with a...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 27, 2018 Category: Drugs & Pharmacology Source Type: research

Evaluation of free thyroxine determination based on one-step fluorometric immunoassay technique and the suboptimal concordance with two-step immunoassay
Publication date: Available online 26 July 2018Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Radhouene Doggui, Rahma Mahjoub, Wassef Lotfi Aissa, Imen Tounsi, Zeineb Allagui, Zmorda Cherif, Sihem Haj Sassi, Sinda Ennigrou, Dhiaeddine Edriss, Jalila El Ati, Amina BibiAbstractFree thyroxine (FT4) quantification is continuing to be a concern. The purpose of the following study was to evaluate the analytical performance of Tosoh AIA900 based on a one-step technique and its comparison to Access 2 (two-step technique) over different clinical contexts (euthyroid, thyroid disorders, uncontrolled diabetes, ren...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 27, 2018 Category: Drugs & Pharmacology Source Type: research

Identification and structure elucidation of a new degradation impurity in the multi-component tablets of amlodipine besylate
Publication date: Available online 26 July 2018Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Petr Gibala, Michal Douša, Aneta Kalužíková, Marcela Tkadlecová, Martin Štefko, Stanislav Kalášek, Jiří BřicháčAbstractNew unknown impurity at m/z 421.15 was observed during the accelerated stability analysis (40 °C/75% relative humidity) in the multi-component tablets of amlodipine besylate by reversed-phase ultra-high performance liquid chromatography–mass spectrometry (UHPLC-MS). UHPLC-MS and nuclear magnetic resonance (NMR)...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 26, 2018 Category: Drugs & Pharmacology Source Type: research

LC–MS/MS reveals the formation of iminium and quinone methide reactive intermediates in entrectinib metabolism: In vivo and in vitro metabolic investigation
Publication date: 25 October 2018Source: Journal of Pharmaceutical and Biomedical Analysis, Volume 160Author(s): Mohamed W. Attwa, Adnan A. Kadi, Haitham Alrabiah, Hany W. DarwishAbstractEntrectinib (RXDX-101) is orally available inhibitor of the tyrosine kinases including tropomyosin receptor kinases (Trk) A–C, C-ros oncogene 1 (ROS1) and anaplastic lymphoma kinase (ALK), with potential antineoplastic activity. Entrectinib (ENB) granted breakthrough designation by FDA for NTRK + Solid tumors. In vitro metabolism of ENB generates quinone methide and iminium reactive intermediates that were captured by p...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 26, 2018 Category: Drugs & Pharmacology Source Type: research

Simultaneous determination of ten nonsteroidal anti-inflammatory drugs from drinking water, surface water and wastewater using micro UHPLC-MS/MS with on-line SPE system
Publication date: Available online 18 July 2018Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Zoltán Márta, Balázs Bobály, Jenő Fekete, Balázs Magda, Tímea Imre, Pál Tamás SzabóAbstractA simple, accurate and sensitive micro UHPLC-MS/MS method was developed and validated for the simultaneous determination of 10 nonsteroidal anti-inflammatory drugs (NSAIDs) from different environmental matrices. The micro LC ‒ on-line SPE method described in this study allowed to determine the selected drugs at ultra-trace levels without the most commonly ...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 25, 2018 Category: Drugs & Pharmacology Source Type: research

Validated stability indicating assay method of olaparib: LC-ESI-Q-TOF-MS/MS and NMR studies for characterization of its new hydrolytic and oxidative forced degradation products
Publication date: Available online 18 July 2018Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Thummar Mohit, Bhoopendra S. Kuswah, S. Gananadhamu, Bulbake Upendra, Gour Jitendra, Khan WahidAbstractOlaparib (OLA) is a poly ADP ribose polymerase (PARP) enzyme inhibitor used to treat prostate, ovarian and breast cancer. The drug substance OLA was subjected to forced degradation as per ICH prescribed guidelines. It was degraded in hydrolytic (acidic and basic) and oxidative stress conditions and yielded four degradation products (DPs) while it remained stable in neutral hydrolytic, dry heat and photolytic ...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 25, 2018 Category: Drugs & Pharmacology Source Type: research

Metabolic fingerprinting in breast cancer stages through 1H NMR spectroscopy-based metabolomic analysis of plasma
Publication date: Available online 18 July 2018Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Shankar Suman, Raj Kumar Sharma, Vijay Kumar, Neeraj Sinha, Yogeshwer ShuklaAbstractBreast cancer (BC) is one of the most common malignancies among women worldwide, which is indeed associated with metabolic reprogramming. However, BC is a very complex and heterogeneous diseases can relate with the changes in metabolic profiles during BC progression. Hence, investigating the metabolic alterations during BC stage progression may reveal the deregulated pathways and useful metabolic signatures of BC. To demonstrat...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 25, 2018 Category: Drugs & Pharmacology Source Type: research

Simultaneous quantification of the cannabinoids tetrahydrocannabinol and cannabidiol and the CB1 receptor antagonist in rat plasma: An application to characterize pharmacokinetics after passive cannabis smoke inhalation and co-administration of rimonabant
Publication date: Available online 19 July 2018Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Abhigyan Ravula, Hardik Chandasana, Barry Setlow, Marcelo Febo, Adriaan W. Bruijnzeel, Hartmut DerendorfAbstractA highly sensitive and selective liquid chromatography-tandem mass spectrometry method for the determination of tetrahydrocannabinol (THC), cannabidiol, and rimonabant in rat plasma was developed. Analytes and the internal standard were extracted from plasma using a combination of protein precipitation followed by liquid-liquid extraction. Chromatographic separation was done using Waters Symmetry C18...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 25, 2018 Category: Drugs & Pharmacology Source Type: research

Potential of Near Infrared Spectroscopy and Pattern Recognition for Rapid Discrimination and Quantification of Gleditsia Sinensis Thorn Powder with Adulterants
In this study Fourier transform near-infrared spectroscopy (FT-NIR) combined with chemical pattern recognition techniques was explored for the first time to discriminate and quantify of cheaper materials (BRM and BRR) in GST. The Savitzkye-Golay (SG) smoothing, vector normalization (VN), min max normalization (MMN), first derivative (1 st D) and second derivative (2nd D) methods were used to pre-process the raw FT-NIR spectra. Successive projections algorithm was adopted to select the characteristic variables and linear discriminate analysis (LDA), support vector machine (SVM), as while as back propagation neural network...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 25, 2018 Category: Drugs & Pharmacology Source Type: research

Metabolic profiling of the anti-tumor drug regorafenib in mice
This study provided a global view of regorafenib metabolism and its potential side-effects.Graphical Abstract (Source: Journal of Pharmaceutical and Biomedical Analysis)
Source: Journal of Pharmaceutical and Biomedical Analysis - July 25, 2018 Category: Drugs & Pharmacology Source Type: research

Combination of phase-solubility method and capillary zone electrophoresis to determine binding constants of cyclodextrins with practically water-insoluble compounds
Publication date: Available online 21 July 2018Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Viktoria V. Sursyakova, Nikolai G. Maksimov, Vladimir A. Levdansky, Anatoly I. RubayloAbstractThe combined method based on phase-solubility technique and capillary zone electrophoresis (PS-CZE) was suggested for the determination of binding (stability) constants of cyclodextrins (CD) complexes with water-insoluble organic compounds that have no or weak UV chromophores. In this method, the insoluble compounds are agitated at the desired temperature in CD solutions with different concentration up to the attainme...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 25, 2018 Category: Drugs & Pharmacology Source Type: research

A new liquid chromatography-high resolution Orbitrap mass spectrometry-based strategy to characterize Glucuronide Oleanane-type Triterpenoid Carboxylic Acid 3, 28-O-Bidesmosides (GOTCAB) saponins.A case study of Gypsophila glomerata Pall ex M. B. (Caryophyllaceae)
In this study, the fragmentation behaviors of GOTCAB from methanol-aqueous root extract of Gypsophila glomerata Pall ex M. B. (Caryophyllaceae) were investigated using ultra-high performance liquid chromatography (UHPLC) coupled with hybrid quadrupole-Orbitrap high resolution mass spectrometry (HRMS). A new saponin was isolated and its structure was established by 1D and 2D-NMR spectroscopic experiments as 3-O-β-D-galactopyranosyl-(1→2)-[α-L-arabinopyranosyl-(1→3)]-β-D-glucuronopyranosyl gypsogenin 28-O-α-L-arabinopyranosyl-(1→3)-[β-D-xylopyranosyl-(1→4)]-α-L-rhamnopyran...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 25, 2018 Category: Drugs & Pharmacology Source Type: research

Quantification of diterpene acids in Copaiba oleoresin by UHPLC-ELSD and heteronuclear two-dimensional qNMR
In this study, we present the quantitation of eight diterpene acids in the oleoresin of Copaifera reticulata Ducke by UHPLC-ELSD and quantitative HSQC (heteronuclear single quantum correlation spectroscopy). UHPLC was performed using reversed phase material and external calibration and showed RSD values of ≤ 3% (repeatability) and ≤ 4% (precision), and mean recovery rates of 91.2 to 104.8%. LOQs were determined with 10 and 20 µg/mL, and LODs with 4 and 8 µg/mL, respectively. For the qHSQC method, calibration curves of eight different NMR cross-peaks (furylic, endo- and exocyclic methine sign...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 25, 2018 Category: Drugs & Pharmacology Source Type: research

Cross-platform metabolic profiling deciphering the potential targets of Shenfu injection against acute viral myocarditis in mice
Publication date: 25 October 2018Source: Journal of Pharmaceutical and Biomedical Analysis, Volume 160Author(s): Guangguo Tan, Qian Zhou, Kui Liu, Xin Dong, Ling Li, Wenting Liao, Hong WuAbstractAcute viral myocarditis (AVMC) is typically caused by cardiotropic viral infection. There is a paucity of specific treatment options available with proven efficacy. Chinese patented pharmaceutical product Shenfu injection (SFI) has potent efficacy on treating AVMC in clinical practice. However, the molecular mechanism is still unknown. We employed cross-platform metabolomics combined with computational systems analysis, based on re...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 25, 2018 Category: Drugs & Pharmacology Source Type: research

Quantification of residual BHK DNA by a novel droplet digital PCR technology
This study not only established a robust assay for the detection of residual BHK DNA, but also evaluated the capability of ddPCR technology for a new application. (Source: Journal of Pharmaceutical and Biomedical Analysis)
Source: Journal of Pharmaceutical and Biomedical Analysis - July 24, 2018 Category: Drugs & Pharmacology Source Type: research

Chemical analysis, pharmacological activity and process optimization of the proportion of bilobalide and ginkgolides in Ginkgo biloba extract
Publication date: Available online 23 July 2018Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Lu Xiaoyan, Chen Li, Ting Liu, Han Ke, Xingchu Gong, Qingqing Wang, Jianbing Zhang, Xiaohui FanAbstractVariations on the efficacy of commercial Ginkgo biloba preparations have been reported, although all the products follow the same standards. Terpene trilactones (TTLs), including bilobalide (BB) and ginkgolides, are one of the main active components in G. biloba extract and have been received the most attention due to their chemical uniqueness and their importance for quality control. A plenty of studies demo...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 24, 2018 Category: Drugs & Pharmacology Source Type: research

Process-related impurities of eplerenone: determination and characterisation by HPLC methods and Raman spectroscopy
Publication date: 10 September 2018Source: Journal of Pharmaceutical and Biomedical Analysis, Volume 159Author(s): Katarzyna Filip, Marta Łaszcz, Andrzej Leś, Justyna ChmielAbstractTwo novel high-performance liquid chromatography methods for the determination of process-related impurities of eplerenone drug substance and the designated starting material were developed and validated. Process impurities, including stereoisomers of eplerenone and the intermediate, were controlled using a Kromasil C18 column (250 mm x 4.6 mm; particle size 5 μm), under gradient conditions. Simple mobile ...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 24, 2018 Category: Drugs & Pharmacology Source Type: research

Simultaneous determination of fourteen compounds of Hedyotis diffusa Willd extract in rats by UHPLC–MS/MS method: Application to pharmacokinetics and tissue distribution study
Publication date: 10 September 2018Source: Journal of Pharmaceutical and Biomedical Analysis, Volume 159Author(s): Xiaoqing Chen, Pingchuan Zhu, Buming Liu, Liuting Wei, Yuanjin XuAbstractA rapid, sensitive and selective ultra high-performance liquid chromatography-tandem mass spectrometry UHPLC–MS/MS method has been developed and validated for the simultaneous determination of fourteen bioactive ingredients (gallic acid, geniposidic acid, protocatechuic acid, caffeic acid, ferulic acid, scopoletin, apigenin-7-o-glucuronide, daidzein, apigenin, ursolic acid, oleanolic acid, β-sitosterol, coniferin, and stigmaste...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 24, 2018 Category: Drugs & Pharmacology Source Type: research

Amplified colorimetric sensor for detecting radon by its daughter lead based on the free-fixed auto-assembly structure of Duplex-hemin/G-quadruplex
In this study, the primer dissociated by the DNAzyme was in a free state. Compared with the fixed-state primer chain, this system will be more convenient for the biological analysis of ultratrace metal ions. Therefore, this strategy has good application prospects for biosensors and is expected to become a novel platform for the amplification and detection of metal ion signals.Graphical abstract (Source: Journal of Pharmaceutical and Biomedical Analysis)
Source: Journal of Pharmaceutical and Biomedical Analysis - July 24, 2018 Category: Drugs & Pharmacology Source Type: research

LC-MS/MS reveals the Formation of Iminium and Quinone Methide Reactive Intermediates in Entrectinib Metabolism: In vivo and In vitro Metabolic Investigation
Publication date: Available online 22 July 2018Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Mohamed W. Attwa, Adnan A. Kadi, Haitham Alrabiah, Hany W. DarwishAbstractEntrectinib (RXDX-101) is orally available inhibitor of the tyrosine kinases including tropomyosin receptor kinases (Trk) A, B and C, C-ros oncogene 1 (ROS1) and anaplastic lymphoma kinase (ALK), with potential antineoplastic activity. Entrectinib (ENB) granted breakthrough designation by FDA for NTRK + Solid tumors. In vitro metabolism of ENB generates quinone methide and iminium reactive intermediates that were captured b...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 23, 2018 Category: Drugs & Pharmacology Source Type: research

Nanomaterial-based biosensors and immunosensors for quantitative determination of cardiac troponins
Publication date: 10 September 2018Source: Journal of Pharmaceutical and Biomedical Analysis, Volume 159Author(s): Alireza Nezami, Sadegh Dehghani, Rahim Nosrati, Negar Eskandari, Seyed Mohammad Taghdisi, Gholamreza KarimiAbstractCardiovascular diseases (CVDs) are the most frequent mortality cause in many countries. The acute myocardial infraction (AMI) is one of the most common types of CVDs. Cardiac troponin I (cTnI) and cardiac troponin T (cTnT) as predominant cardiac infarction biomarkers considered as “gold standard” for diagnosis of acute myocardial infraction (AMI). The restrictions of traditional method...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 22, 2018 Category: Drugs & Pharmacology Source Type: research

Investigation of inclusion behaviour of gefitinib with epichlorohydrin-β-cyclodextrin polymer: Preparation of binary complex, stoichiometric determination and characterization
Publication date: Available online 21 July 2018Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Bina Gidwani, Amber Vyas, Chanchal Deep KaurAbstractGefitinib is anticancer drug which is sparingly soluble in water. This limits its dissolution and bioavailability. Binary inclusion complex of gefitinib with Epi-β-CD was prepared by freeze-drying method. Stoichiometric ratio of 1:1 M was established by continuous variation (Job’s) plot. The stability constant of complex as determined by phase solubility study was found to be 15871.3 M−1. Complex was characterized by FTIR, DSC, DTA and...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 21, 2018 Category: Drugs & Pharmacology Source Type: research

Analytical Target Profile: Establishment of precision requirements for assay
Publication date: Available online 20 July 2018Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Joachim ErmerAbstractApproaches are presented to establish precision (or target measurement uncertainty) requirements to drug substance and drug product assays. They are based on the simple and well-known concept of the normal distribution probability around true content values represented either by manufacturing range limits, or by the manufacturing target (usually 100% label claim). A maximum acceptable precision is derived which allows a defined probability of analytical results within the established accep...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 21, 2018 Category: Drugs & Pharmacology Source Type: research

Investigation of antioxidant interaction between Green tea polyphenols and acetaminophen using isobolographic analysis
Publication date: 10 September 2018Source: Journal of Pharmaceutical and Biomedical Analysis, Volume 159Author(s): Aleksandra Sentkowska, Krystyna PyrzynskaAbstractThe antioxidant interactions between acetaminophen (APAP) and green tea polyphenols were investigated using 1,1-diphenyl- 2-picryl-hydrazyl (DPPH) radicals and cupric reducing antioxidant capacity (CUPRAC). The results obtained experimentally for the mixtures were compared with theoretical values calculated by adding up the effects of both individual components analyzed separately. The potential antagonistic, additive or synergistic effects were also evaluated u...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 21, 2018 Category: Drugs & Pharmacology Source Type: research

Determination of garlic phenolic compounds using supercritical fluid extraction coupled to supercritical fluid chromatography/tandem mass spectrometry
Publication date: Available online 20 July 2018Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Jian Liu, Feng Ji, Fengming Chen, Wei Guo, Minli Yang, Shengxiong Huang, Feng Zhang, Yongsheng LiuAbstractA rapid, simple and environmentally friendly supercritical fluid extraction and supercritical fluid chromatography coupled to mass spectrometry (SFE-SFC-MS/MS) method has been developed for the analysis of nine phenolic compounds in garlic. Through the optimization of the SFE parameters using response surface methodology (RSM), 15 phenolic compounds were successfully extracted at 50 °C in 9 min wit...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 21, 2018 Category: Drugs & Pharmacology Source Type: research

Targeted and non-targeted analysis of annonaceous alkaloids and acetogenins from Asimina and Annona species using UHPLC-QToF-MS
Publication date: Available online 19 July 2018Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Bharathi Avula, Ji-Yeong Bae, Taghreed Majrashi, Tung-Ying Wu, Yan-Hong Wang, Mei Wang, Zulfiqar Ali, Yang-Chang Wu, Ikhlas A. KhanAbstractIn current work, targeted and non-targeted analysis of alkaloids and acetogenins from methanolic extracts of Asimina, Annona species and dietary supplements have been performed using UHPLC-QToF in positive ion mode. Thirty-five standard compounds (twelve alkaloids and twenty-three acetogenins) were used for the analysis. The fragment ions produced by collision induced disso...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 20, 2018 Category: Drugs & Pharmacology Source Type: research

Pranoprofen quantification in ex vivo corneal and scleral permeation samples: Analytical validation
Publication date: Available online 18 July 2018Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): C. Cañadas-Enrich, G. Abrego, H.L. Alvarado, A.C. Calpena-Capmany, A. Boix-MontañesAbstractThe investigation of the ocular permeability and/or distribution of pranoprofen (PF), a non-steroidal antiinflamatory drug, demands for the selective analysis of its transit through specific ocular membranes. Therefore, customised ex vivo permeation experiments through external ocular tissues (cornea and sclera) have been validated for this drug in addition to its HPLC-UV quantification following standard b...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 19, 2018 Category: Drugs & Pharmacology Source Type: research

Quantification of Residual BHK DNA by a Novel Digital Droplet PCR Technology
This study not only established a robust assay for the detection of residual BHK DNA, but also evaluated the capability of ddPCR technology for a new application. (Source: Journal of Pharmaceutical and Biomedical Analysis)
Source: Journal of Pharmaceutical and Biomedical Analysis - July 19, 2018 Category: Drugs & Pharmacology Source Type: research