Novel method for metalloproteins determination in human breast milk by size exclusion chromatography coupled to inductively coupled plasma mass spectrometry
Publication date: 5 September 2018 Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 158 Author(s): Mariano Acosta, Sabier Torres, Leonardo Mariño-Repizo, Luis D. Martinez, Raúl A. Gil Levels of essential metals in human breast milk (HBM) have been determined by different analytical techniques, but there is few woks about human whey milk fractions. However, the current trend lies in metalloproteomic and identification of different metalloproteins. In this sense, native separative techniques (N-PAGE and SEC) coupled to ICP-MS provide us with valuable information. Besides it is necessary the dev...
Source: Journal of Pharmaceutical and Biomedical Analysis - June 22, 2018 Category: Drugs & Pharmacology Source Type: research

Analysis of monofluoroacetic acid in human plasma by UFLC –MS/MS and its application in patients with sodium monofluoroacetate or monofluoroacetamide poisoning
Publication date: 5 September 2018 Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 158 Author(s): Liang Liu, Shuang Hu, Suodi Zhai, Xin Hai Monofluoroacetic acid (FAcOH), was once widely used in baits as a rodenticide in agriculture. For intentional and unintentional misuses, the incidence of FAcOH poisoning has increased in recent years. Organic fluorine rodenticides such as sodium monofluoroacetate and monofluoroacetamide, the analogs of FAcOH, can easily be converted to FAcOH in vivo and cause injury. It is urgent to establish a simple and sensitive analytical method of FAcOH in human plasma and applie...
Source: Journal of Pharmaceutical and Biomedical Analysis - June 22, 2018 Category: Drugs & Pharmacology Source Type: research

Optimization of LC method for the quantification of doxorubicin in plasma and urine samples in view of pharmacokinetic, biomedical and drug monitoring therapy studies
Publication date: 5 September 2018 Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 158 Author(s): Olga Maliszewska, Alina Plenis, Ilona Olędzka, Piotr Kowalski, Natalia Miękus, Ewa Bień, Małgorzata Anna Krawczyk, Elżbieta Adamkiewicz-Drożynska, Tomasz Bączek A simple, rapid, reliable and sensitive method based on liquid chromatography with fluorescence detection (LC-FL) for the quantification of doxorubicin (DOX) in human plasma and urine samples was developed. The assay was carried out after the solid-phase extraction procedure (SPE) with hydrophilic-lipophilic balance (HLB) cartridges, and with d...
Source: Journal of Pharmaceutical and Biomedical Analysis - June 22, 2018 Category: Drugs & Pharmacology Source Type: research

Sandwich pair nanobodies, a potential tool for electrochemical immunosensing serum prostate-specific antigen with preferable specificity
In this study, a sandwich pair of nanobodies (Nbs) (i.e., Nb2 and Nb40) against PSA surface antigen was obtained from an alpaca-derived immune phage display library. A sandwich-type immunosensor for the sensitive and selective detection of PSA in serum samples was ingeniously designed based on the pair of Nbs. The small size of Nb40 allowed high capture densities on the surface of reduced graphene oxide (rGO) nanocomposed with massive Au nanoparticles (rGO@AuNPs), which significantly improved the conductivity and provided a large area to anchor many primary antibodies. The secondary antibody Nb2 fused with streptavidin -bi...
Source: Journal of Pharmaceutical and Biomedical Analysis - June 21, 2018 Category: Drugs & Pharmacology Source Type: research

In vitrometabolic mapping of neobavaisoflavone in human cytochromes P450 and UDP-glucuronosyltransferase enzymes by ultra high-performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry
Publication date: 5 September 2018 Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 158 Author(s): Jinjin Xu, Mengsen Li, Zhihong Yao, Yezi Zhang, Shishi Li, Liufang Hu, Zifei Qin, Frank J. Gonzalez, Xinsheng Yao Neobavaisoflavone (NBIF), a phenolic compound isolated from Psoralea corylifolia L., possesses several significant biological properties. However, the pharmacokinetic behaviors of NBIF have been characterized as rapid oral absorption, high clearance, and poor oral bioavailability. We found that NBIF underwent massive glucuronidation and oxidation by human liver microsomes (HLM) in this study with ...
Source: Journal of Pharmaceutical and Biomedical Analysis - June 20, 2018 Category: Drugs & Pharmacology Source Type: research

Dopamine: Acid-base properties and membrane penetration capacity
Publication date: 5 September 2018 Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 158 Author(s): Arash Mirzahosseini, Tamás Pálla, Gábor Orgován, Gergő Tóth, Béla Noszál Dopamine and 4 related compounds were studied by 1H NMR-pH titrations and a case-tailored evaluation method. The resulting acid-base properties of dopamine are quantified in terms of 3 macroscopic and 12 microscopic protonation constants and the concomitant 3 interactivity parameters. The species- and site-specific basicities are interpreted by means of inductive and shielding effects thr...
Source: Journal of Pharmaceutical and Biomedical Analysis - June 20, 2018 Category: Drugs & Pharmacology Source Type: research

RNA-seq based transcriptome analysis of the protective effect of compound longmaining decoction on acute myocardial infarction
This study demonstrated that CLMN decoction might regulate the expressions of Ccl6, Ccr5, Itgam, Ncf1 and Mmp9, inhibit the chemokine signaling pathway and leukocyte transendothelial migration to play a protective effect on AMI. Graphical abstract (Source: Journal of Pharmaceutical and Biomedical Analysis)
Source: Journal of Pharmaceutical and Biomedical Analysis - June 20, 2018 Category: Drugs & Pharmacology Source Type: research

Gender-related differences in pharmacokinetics, tissue distribution, and excretion of 20(R)-25-methoxyl-dammarane-3 β,12β,20-triol and its metabolite in rats and anti-ovarian cancer evaluation
Publication date: 5 September 2018 Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 158 Author(s): Meng Ding, Yumeng Zhang, Xude Wang, Yuqing Zhao Our previous study suggests a well-defined pharmacological activity of 20(R)-25-methoxyl-dammarane-3β,12β,20-triol (AD-1) and its metabolite 20(R)-dammarane-3β,12β,20,25-tetrol (AD-2). The current study aims to investigate the gender-related differences in pharmacokinetics, tissue distribution, and excretion of AD-1 and its metabolite in both male and female rats. A sensitive and rapid ultra-performance liquid chromatography tandem mass spect...
Source: Journal of Pharmaceutical and Biomedical Analysis - June 20, 2018 Category: Drugs & Pharmacology Source Type: research

Natural deep eutectic solvents as eco-friendly and sustainable dilution medium for the determination of residual organic solvents in pharmaceuticals with static headspace-gas chromatography
Publication date: 5 September 2018 Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 158 Author(s): Meilian Wang, Sheng Fang, Xianrui Liang Reported here is a simple and rapid static headspace gas chromatography (SHS-GC) method for the determination of trace solvents including ethanol, isopropanol, n-butanol, 1,4-dioxane, tetrahydrofuran, acetonitrile, methanol and acetone which commonly used in drug production process. Natural deep eutectic solvents (NADESs) are firstly used as the matrix medium for this method, which provided high sensitivity for residual solvents detection. With the optimized method, val...
Source: Journal of Pharmaceutical and Biomedical Analysis - June 19, 2018 Category: Drugs & Pharmacology Source Type: research

Efficient extraction of proanthocyanidin from Ginkgo biloba leaves employing rationally designed deep eutectic solvent-water mixture and evaluation of the antioxidant activity
Publication date: 5 September 2018 Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 158 Author(s): Jun Cao, Luyao Chen, Mohan Li, Fuliang Cao, Linguo Zhao, Erzheng Su Proanthocyanidin (PAC) holds strong free radicals scavenging ability and is widely used as oxygen free radical scavenger. Huge demand, safety and economic aspect are forcing the PAC extraction to explore new resource and greener solvent. An efficient extraction method of PAC from Ginkgo biloba leaves was established by employing deep eutectic solvent (DES)-water mixture. After a rational design, a DES-water mixture (named as Ch-M55) was chose...
Source: Journal of Pharmaceutical and Biomedical Analysis - June 16, 2018 Category: Drugs & Pharmacology Source Type: research

Tuberculosis vaccine candidate: Characterization of H4-IC31 formulation and H4 antigen conformation
Publication date: 5 August 2018 Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 157 Author(s): Sasmit S. Deshmukh, Federico Webster Magcalas, Kristen N. Kalbfleisch, Bruce W. Carpick, Marina D. Kirkitadze Tuberculosis (TB) is one of the leading causes of death worldwide, making the development of effective TB vaccines a global priority. A TB vaccine consisting of a recombinant fusion protein, H4, combined with a novel synthetic cationic adjuvant, IC31®, is currently being developed. The H4 fusion protein consists of two immunogenic mycobacterial antigens, Ag85 B and TB10.4, and the IC31® adjuvan...
Source: Journal of Pharmaceutical and Biomedical Analysis - June 15, 2018 Category: Drugs & Pharmacology Source Type: research

Method optimization of hydrophilic interaction chromatography separation of nucleotides using design of experiment approaches I: Comparison of several zwitterionic columns
Publication date: 5 September 2018 Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 158 Author(s): Shuntaro Arase, Susumu Kimura, Tohru Ikegami A systematic method in hydrophilic interaction chromatography (HILIC) was developed for the separation of four monophosphate nucleotides using design of experiment (DOE) approaches. Three HPLC parameters, the buffer concentration (ammonium acetate concentration), gradient time, and temperature, were evaluated within the quality design framework, and the effects on chromatographic parameters were investigated. Four zwitterionic columns (ZIC-HILIC, ZIC-cHILIC, NUCLEO...
Source: Journal of Pharmaceutical and Biomedical Analysis - June 15, 2018 Category: Drugs & Pharmacology Source Type: research

Artificial neural networks (ANNs) and partial least squares (PLS) regression in the quantitative analysis of cocrystal formulations by Raman and ATR-FTIR spectroscopy
Publication date: 5 September 2018 Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 158 Author(s): P. Barmpalexis, A. Karagianni, I. Nikolakakis, K. Kachrimanis The present work describes the development of an efficient, fast and accurate method for the quantification of polymer-based cocrystal formulations. Specifically, the content of carbamazepine–nicotinamide (CBZ/NIC) and ibuprofen-nicotinamide (IBU/NIC) cocrystals in Soluplus®-based formulations was independently determined with the aid of either Raman or Attenuated Total Reflectance Fourier-Transform Infrared Spectroscopy (ATR-FTIR) spectr...
Source: Journal of Pharmaceutical and Biomedical Analysis - June 15, 2018 Category: Drugs & Pharmacology Source Type: research

Simultaneous determination of plasma methotrexate and 7-hydroxy methotrexate by UHPLC –MS/MS in patients receiving high-dose methotrexate therapy
Publication date: 5 September 2018 Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 158 Author(s): Shenghui Mei, Xiaoxu Shi, Yaming Du, Yong Cui, Chun Zeng, Xiaohui Ren, Kefu Yu, Zhigang Zhao, Song Lin The plasma concentrations of methotrexate (MTX) and its major metabolite 7-hydroxy methotrexate (7-OH-MTX) are highly correlated with the toxicities in patients with high-dose MTX therapy. Routine monitoring of MTX and 7-OH-MTX plasma levels is useful for dose adjustment of rescue drugs and toxicity prevention. A UHPLC-MS/MS method for simultaneous determination of plasma MTX and 7-OH-MTX was developed, vali...
Source: Journal of Pharmaceutical and Biomedical Analysis - June 15, 2018 Category: Drugs & Pharmacology Source Type: research

Metabolome based classification of artichoke leaf: A prospect for phyto-equivalency of its different leaf origins and commercial preparations
Publication date: 5 September 2018 Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 158 Author(s): Mohamed A. Farag, Mahmoud F. Elsebai, Amira R. Khattab The growing interest in assuring phytomedicines efficacy and moreover the increase in requirements for its safety drive the development of analytical methods for its quality control assurance. Herein, we present a nuclear magnetic resonance (NMR) fingerprinting approach of artichoke leaf material from different origins and in its commercial preparations. Under optimized conditions, we were able to simultaneously identify 23 metabolites including sugars, a...
Source: Journal of Pharmaceutical and Biomedical Analysis - June 15, 2018 Category: Drugs & Pharmacology Source Type: research

Study on the stability control strategy of Triphala solution based on the balance of physical stability and chemical stabilities
Publication date: 5 September 2018 Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 158 Author(s): Hao-zhou Huang, Sheng-yu Zhao, Xiu-mei Ke, Jun-zhi Lin, Shu-sen Huang, Run-chun Xu, Hong-yan Ma, Yi Zhang, Li Han, Ding-kun Zhang Triphala is a well-known prescription in Indian Ayurveda and TCM medicine for its great effect on gingivitis and hyperlipidemia. However, its solution is unstable for the containing of excessive polyphenol, leading to the production of sediment in the short term and the decrease of efficacy. Based on the analysis of sediment formation, a novel control strategy is proposed. To condu...
Source: Journal of Pharmaceutical and Biomedical Analysis - June 15, 2018 Category: Drugs & Pharmacology Source Type: research

Simultaneous determination of dextromepromazine and related substances 2-methoxyphenothiazine and levomepromazine sulfoxide in levomepromazine on a cellulose tris(4-methylbenzoate) chiral column
Publication date: 5 September 2018 Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 158 Author(s): Stephan Niedermeier, Iza Matarashvili, Bezhan Chankvetadze, Gerhard K.E. Scriba A high-performance liquid chromatography method for the determination of dextromepromazine, levomepromazine sulfoxide and 2-methoxyphenothiazine in levomepromazine samples was developed. The separation of the analytes was achieved within 10 min on a stationary phase containing cellulose tris(4-methylbenzoate) as chiral selector. The mobile phase consisted of 0.1% diethylamine in methanol with a flow rate of 1.0 mL/min. The met...
Source: Journal of Pharmaceutical and Biomedical Analysis - June 13, 2018 Category: Drugs & Pharmacology Source Type: research

Bioanalysis of free and liposomal Amphotericin B in rat plasma using solid phase extraction and protein precipitation followed by LC-MS/MS
In this study, an original strategy was developed to separately determine F-AMB and L-AMB in rat plasma using LC–MS/MS. F-AMB was analyzed after separation by solid phase extraction, total AMB (T-AMB) was determined after protein precipitation and L-AMB was determined by difference. The method was fully validated. Calibration curves were linear in the ranges 0.7–120 μg/mL for T-AMB and 0.2–20 μg/mL for F-AMB. Accuracy and precision results were within acceptable variability limits, recoveries were consistent and reproducible, matrix effects were insignificant and analytes were stable under all t...
Source: Journal of Pharmaceutical and Biomedical Analysis - June 12, 2018 Category: Drugs & Pharmacology Source Type: research

Quantification of nucleotides and their sugar conjugates in biological samples: Purposes, instruments and applications
Publication date: 5 September 2018 Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 158 Author(s): Xuan Qin, Xin Wang Nucleotides and their sugar conjugates are fundamental molecules in life, participating in processes of DNA/RNA composition, cell wall build-up, glycosylation reactions, and signal conduction. Therefore, the quantification of these compounds in biological samples significantly benefits the understanding of their functions. However, nucleotides and nucleotide sugars are extremely hydrophilic, causing bad retention and peak symmetry on regular C18 chromatographic columns. To solve this proble...
Source: Journal of Pharmaceutical and Biomedical Analysis - June 12, 2018 Category: Drugs & Pharmacology Source Type: research

Comparison of multivariate data analysis techniques to improve glucose concentration prediction in mammalian cell cultivations by Raman spectroscopy
In this study, four mammalian cell cultivation runs were followed with Raman spectroscopy and the spectra were analysed quantitatively and qualitatively as well. The PCA analysis showed that one of the most dominant factors in the Raman spectra were the concentration of glucose, which strongly correlated with the score values of the eighth principal component. This observation further substantiated that Raman spectroscopy is an excellent tool for bioprocess monitoring and induced the test of the Multivariate Linear Regression (MLR), Principal Component Regression (PCR) and Partial Least Squares Regression (PLSR) algorithms...
Source: Journal of Pharmaceutical and Biomedical Analysis - June 10, 2018 Category: Drugs & Pharmacology Source Type: research

Identification of a new tadalafil analogue, N-3-hydroxypropylnortadalafil, in a supplement product
Publication date: 5 September 2018 Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 158 Author(s): Hui-Chun Lee, Yun-Lian Lin, Yen-Chun Huang, Chia-Fen Tsai, Der-Yuan Wang A novel tadalafil analogue, which exhibits similarity to 2-hydroxypropylnortadalafil, was found in dietary supplements using adulterants screening and isolated using column chromatography. By using extensive 1D- and 2D-NMR and MS spectral analyses, the structure was determined as 6-(1,3-Benzodioxol-5-yl)-2,3,6,7,12,12a-hexahydro-2-(3-hydroxypropyl)pyrazino(1′,2′:1,6)pyrido(3,4-b)indole-1,4-dione, and the analogue was named N-...
Source: Journal of Pharmaceutical and Biomedical Analysis - June 9, 2018 Category: Drugs & Pharmacology Source Type: research

Multiwavelength UV-metric and pH-metric determination of the multiple dissociation constants of the lesinurad
Publication date: 5 September 2018 Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 158 Author(s): Milan Meloun, Aneta Čápová, Lucie Pilařová, Tomáš Pekárek Potentiometric and spectrophotometric pH-titrations of the lesinurad for three consecutive dissociation constants determination were compared. Lesinurad is a selective inhibitor of uric acid reabsorption as part of a combination of medicines to treat high levels of uric acid in blood, also called hyperuricemia. Nonlinear regression of the pH-spectra with REACTLAB and SQUAD84 and of the pH-titration curve with...
Source: Journal of Pharmaceutical and Biomedical Analysis - June 8, 2018 Category: Drugs & Pharmacology Source Type: research

New developments and possibilities of wide-pore superficially porous particle technology applied for the liquid chromatographic analysis of therapeutic proteins
Publication date: 5 September 2018 Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 158 Author(s): Balázs Bobály, Jean-Luc Veuthey, Davy Guillarme, Szabolcs Fekete This review paper discusses the success of columns packed with superficially porous particles (SPP) in liquid chromatography for the analysis of peptides and proteins. First, it summarizes the history of SPP, including the development of different SPP generations from particles of 50 μm to sub-2 μm. It also critically discusses the improved kinetic performance of SPP particles in comparison to fully porous particles. The ...
Source: Journal of Pharmaceutical and Biomedical Analysis - June 8, 2018 Category: Drugs & Pharmacology Source Type: research

Discrimination of magnoliae officinalis cortex based on the quantitative profiles of magnolosides by two-channel liquid chromatography with electrochemical detection
Publication date: 5 September 2018 Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 158 Author(s): Zhenzhen Xue, Akira Kotani, Bin Yang, Hideki Hakamata A two-channel liquid chromatography with electrochemical detection system (2LC-ECD) was newly designed for the simultaneous determination of magnolosides A, B, F, H, and L in the first channel and other magnolosides D and M in the second channel, respectively. Peak heights had linear relationships to the magnoloside concentrations in a range of 0.02–16 μmol/L for H, 0.01–12 μmol/L for A, 0.02–12 μmol/L for F and L, 0.01&nda...
Source: Journal of Pharmaceutical and Biomedical Analysis - June 7, 2018 Category: Drugs & Pharmacology Source Type: research

Structure-based manual screening and automatic networking for systematically exploring sansanmycin analogues using high performance liquid chromatography tandem mass spectroscopy
This study employed high performance liquid chromatography-mass spectrometry detector (HPLC–MSD) ion trap and LTQ orbitrap tandem mass spectrometry (MS/MS) to explore sansanmycin analogues manually and automatically by re-analysis of the Streptomyces sp. SS fermentation broth. The structure-based manual screening method, based on analysis of the fragmentation pathway of known UPAs and on comparisons of the MS/MS spectra with that of sansanmycin A (SS-A), resulted in identifying twenty sansanmycin analogues, including twelve new structures (1-12). Furthermore, to deeply explore sansanmycin analogues, we utilized a GNP...
Source: Journal of Pharmaceutical and Biomedical Analysis - June 7, 2018 Category: Drugs & Pharmacology Source Type: research

Real-time quantitative PCR detection of circulating tumor cells using tag DNA mediated signal amplification strategy
Publication date: 5 September 2018 Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 158 Author(s): Ting mei, Xuewen Lu, Ning Sun, Xiaomei Li, Jitao Chen, Min Liang, Xinke Zhou, Zhiyuan Fang The level of circulating tumor cell (CTCs) is a reliable marker for tumor burden and malignant progression. Quantification of CTCs remains technically challenging due to the rarity of these cells in peripheral blood. In the present study, we established a real-time quantitative PCR (Q-PCR) based method for sensitive detection of CTCs without DNA extraction. Blood sample was first turned to erythrocyte lyses and then inc...
Source: Journal of Pharmaceutical and Biomedical Analysis - June 7, 2018 Category: Drugs & Pharmacology Source Type: research

Doping control analysis of 121 prohibited substances in equine hair by liquid chromatography –tandem mass spectrometry
Publication date: 5 September 2018 Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 158 Author(s): J.K.Y. Wong, T.L.S. Choi, K.Y. Kwok, E.N.Y. Lei, T.S.M. Wan Equine hair is becoming an increasingly popular biological matrix for doping control of horse sports; one of the reasons for this is the significantly longer detection window hair can offer. Hair analysis opens up the opportunity for longitudinal monitoring of drug exposure which would otherwise not be possible with the more traditional and common biological matrices, such as urine and blood. As such, there is a need for more multi-target screening m...
Source: Journal of Pharmaceutical and Biomedical Analysis - June 7, 2018 Category: Drugs & Pharmacology Source Type: research

Liquid chromatography-tandem mass spectrometric assay for therapeutic drug monitoring of the EGFR inhibitors afatinib, erlotinib and osimertinib, the ALK inhibitor crizotinib and the VEGFR inhibitor nintedanib in human plasma from non-small cell lung cancer patients
Publication date: 5 September 2018 Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 158 Author(s): Rafael Reis, Laurence Labat, Marie Allard, Pascaline Boudou-Rouquette, Jeanne Chapron, Audrey Bellesoeur, Audrey Thomas-Schoemann, Jennifer Arrondeau, Frédérique Giraud, Jérôme Alexandre, Michel Vidal, François Goldwasser, Benoît Blanchet A new method for the quantitative analysis by liquid chromatography-tandem mass spectrometry (LC–MS/MS) of five tyrosine kinase inhibitors (afatinib, crizotinib, osimertinib, erlotinib and nintedanib) used in the treatment of non...
Source: Journal of Pharmaceutical and Biomedical Analysis - June 6, 2018 Category: Drugs & Pharmacology Source Type: research

Development and validation of a liquid chromatography-tandem mass spectrometry assay for the quantification of lurbinectedin in human plasma and urine
This article describes the development and validation of a liquid chromatography-tandem mass spectrometry (LC–MS/MS) assay to quantify lurbinectedin in human plasma and urine. Plasma samples were pre-treated with 1 M aqueous ammonia after which they were brought onto supported liquid extraction (SLE) columns. Lurbinectedin was eluted from the columns using tert-butyl methyl ether (TBME). Urine was first diluted in plasma and lurbinectedin was extracted from this matrix by liquid-liquid extraction using TBME. Samples were measured by LC–MS/MS in the positive electron ion spray mode. The method was linear over ...
Source: Journal of Pharmaceutical and Biomedical Analysis - June 6, 2018 Category: Drugs & Pharmacology Source Type: research

Monitoring of tobramycin in human plasma via mixed matrix membrane extraction prior to capillary electrophoresis with contactless conductivity detection
Publication date: 5 September 2018 Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 158 Author(s): Nurul Hazirah Mukhtar, Nor Akma Mamat, Hong Heng See A sample pre-treatment method based on a dynamic mixed matrix membrane tip extraction followed by capillary electrophoresis with contactless conductivity detection (CE-C4D) was evaluated for the determination of tobramycin in human plasma. The extraction tip device consisted of a cellulose triacetate membrane tip wall immobilised with 15% (w/w) of hydrophilic lipophilic balance (HLB) nanoparticles as adsorbent. The extraction was performed dynamically by wi...
Source: Journal of Pharmaceutical and Biomedical Analysis - June 6, 2018 Category: Drugs & Pharmacology Source Type: research

Optimizing the extraction of polyphenols from Sideritis montana L. using response surface methodology
Publication date: 5 September 2018 Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 158 Author(s): Mehmet Bilgin, Elaf Abdelillah Ali Elhussein, Mustafa Özyürek, Kubilay Güçlü, Selin Şahin Sideritis montana L. endemic of Turkey was screened for its polyphenols content and antioxidant activity. Factor analysis and experimental design have been applied to understand the structure of the separation process, to determine the effective parameters, and to accomplish the performance improvement. Face-centred composite design (FCD) of response surface methodology (RSM) was applied to ev...
Source: Journal of Pharmaceutical and Biomedical Analysis - June 5, 2018 Category: Drugs & Pharmacology Source Type: research

Development and validation of an ICP-MS method for quantification of total carbon and platinum in cell samples and comparison of open-vessel and microwave-assisted acid digestion methods
Publication date: 5 September 2018 Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 158 Author(s): Mie Riisom, Bente Gammelgaard, Ian H. Lambert, Stefan Stürup Cisplatin is a widely used chemotherapeutic drug. Due to severe side effects and intrinsic or acquired resistance, there is a great interest in developing new platinum-based anticancer agents and a need for robust and validated analytical methods for determination of platinum accumulation in biological samples. A validated ICP-MS method for quantification of total carbon and platinum in cell samples is presented, applicable for cellular drug ac...
Source: Journal of Pharmaceutical and Biomedical Analysis - June 3, 2018 Category: Drugs & Pharmacology Source Type: research

Metabolomics coupled with system pharmacology reveal the protective effect of total flavonoids of Astragali Radix against adriamycin-induced rat nephropathy model
In this study, a NMR based metabolomic approach coupled with biochemical assay and histopathological inspection had been employed to study the protective effect of total flavonoids (TFA) in AR against adriamycin-induced nephropathy using rats model. Multivariate analysis revealed that 11 of perturbed metabolites could be reversed by TFA, and the MetaboAnalyst analysis revealed that the anti-nephrotic syndrome effect of TFA was probably related with regulation of alanine, aspartate and glutamate metabolism, citrate cycle, pyruvate metabolism, cysteine and methionine metabolism and glyoxylate and dicarboxylate metabolism. Th...
Source: Journal of Pharmaceutical and Biomedical Analysis - June 3, 2018 Category: Drugs & Pharmacology Source Type: research

Simultaneous quantitation of two direct acting hepatitis C antivirals (sofosbuvir and daclatasvir) by an HPLC-UV method designated for their pharmacokinetic study in rabbits
Publication date: 5 September 2018 Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 158 Author(s): Noha N. Atia, Salwa R. El-Shaboury, Samia M. El-Gizawy, Mohammad Nabil Abo-Zeid Sofosbuvir (SOF) and daclatasvir (DCS) are novel, recently developed direct acting antiviral agents characterized by potent anti-hepatitis C virus action. A fast and efficient HPLC-UV method was developed, validated and applied for simultaneous determination of SOF and DCS in pharmaceutical formulations and biological fluids based on coupling liquid-liquid extraction with ultrasound and dual wavelength detection at λmax; 26...
Source: Journal of Pharmaceutical and Biomedical Analysis - June 2, 2018 Category: Drugs & Pharmacology Source Type: research

Identification and quantification of ethylene oxide in sterilized medical devices using multiple headspace GC/MS measurement
Publication date: 5 September 2018 Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 158 Author(s): Pascal Gimeno, Marie-Laure Auguste, Vagn Handlos, Anne Mette Nielsen, Stephan Schmidt, Nelly Lassu, Martin Vogel, Antonius Fischer, Charlotte Brenier, Françoise Duperray This manuscript, based on the ISO 10993-7 approach, describes a multiple HS-GC measurement of residual EO present in sterilized plastic samples. The quantification of EO is done, according to the ISO standard, by addition of EO amounts extracted for each repeated extraction. During the method development, the specificity of the detecti...
Source: Journal of Pharmaceutical and Biomedical Analysis - June 2, 2018 Category: Drugs & Pharmacology Source Type: research

Study of degradation behaviour of montelukast sodium and its marketed formulation in oxidative and accelerated test conditions and prediction of physicochemical and ADMET properties of its degradation products using ADMET Predictor ™
This study was aimed to understand the degradation behaviour of the drug in different oxidative media containing hydrogen peroxide, AIBN, Fe3+, Fenton’s reagent and O2 environment under normal laboratory light conditions. The degradation behaviour of the drug was also evaluated in solid sate under ICH recommended accelerated stability condition of 40 °C/75% RH to correlate with the degradation products (DPs) formed in a solid oral formulation. A total of nine DPs (MTK 1 to MTK 9) were formed from both the drug substance and the marketed tablet formulation on storage under controlled oxygen environment in normal...
Source: Journal of Pharmaceutical and Biomedical Analysis - June 2, 2018 Category: Drugs & Pharmacology Source Type: research

Determination of phenolic acids in extra virgin olive oil using supercritical fluid chromatography coupled with single quadrupole mass spectrometry
Publication date: 5 August 2018 Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 157 Author(s): Guangyun Tang, Yang Huang, Tingting Zhang, Qiqin Wang, Jacques Crommen, Marianne Fillet, Zhengjin Jiang Phenolic acids represent one third of the total phenolic compounds in extra virgin olive oil (EVOO) and contribute greatly to the biological and sensory properties of EVOO. In the present research, an analytical method based on supercritical fluid chromatography coupled with single quadrupole mass spectrometry (SFC-MS) was developed for the analysis of phenolic acids in EVOOs. The chromatographic and MS condit...
Source: Journal of Pharmaceutical and Biomedical Analysis - June 1, 2018 Category: Drugs & Pharmacology Source Type: research

Probing DNA damage induced by common antiviral agents using multiple analytical techniques
In this study, we explore the potential DNA damaging effect of some FDA-approved antiviral drugs which may be able to serve as anticancer agents for hepatocellular carcinoma, in order to better elucidate their mode of action. Five antiviral drugs were selected; ribavirin, sofosbuvir, tenofovir disoproxil fumerate, daclatasvir and ledipasvir. Several methods, including absorption spectroscopy, MALDI-TOF mass spectrometry and fluorimetric analysis using the EvaGreen (EG) intercalating dye, were used to probe the drug-induced DNA damage. Results show that only daclatasvir and ledipasvir induced DNA damage. Absorption spectros...
Source: Journal of Pharmaceutical and Biomedical Analysis - June 1, 2018 Category: Drugs & Pharmacology Source Type: research

pH-Dependent stability of azithromycin in aqueous solution and structure identification of two new degradation products
Publication date: 5 September 2018 Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 158 Author(s): Maria Grazia Saita, Danilo Aleo, Barbara Melilli, Sergio Mangiafico, Melina Cro, Claudia Sanfilippo, Angela Patti The degradation profile of azithromycin in buffered solutions was investigated using HPLC and found to be pH dependent in the range of 6.0–7.2. Desosaminylazitromycin, derived from hydrolytic loss of cladinose of the parent molecule, was the major degradation product at pH 6.0 but its amount progressively decreased moving toward pH 7.2. Two additional unreported degradation products were als...
Source: Journal of Pharmaceutical and Biomedical Analysis - June 1, 2018 Category: Drugs & Pharmacology Source Type: research

Validated LC –MS/MS method for the determination of amlodipine enantiomers in rat plasma and its application to a stereoselective pharmacokinetic study
Publication date: 5 September 2018 Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 158 Author(s): Lijuan Wang, Wenxia Liu, Zunjian Zhang, Yuan Tian A rapid and sensitive method was established to determine amlodipine enantiomers using liquid chromatography-tandem mass spectrometry (LC–MS/MS). Stereoselective separation was performed on CHIRALCEL OZ-RH column (150 mm × 4.6 mm i.d., 5 μm) with acetonitrile-water (10 mM ammonium acetate, 0.5% ammonia solution) (95:5, v/v) at a flow rate of 0.5 mL/min. The substances were detected by mass spectrometer equipped with an electrospray...
Source: Journal of Pharmaceutical and Biomedical Analysis - June 1, 2018 Category: Drugs & Pharmacology Source Type: research

Simultaneous quantitation of folates, flavins and B6 metabolites in human plasma by LC –MS/MS assay: Applications in colorectal cancer
Publication date: 5 September 2018 Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 158 Author(s): Isaac Asante, Hua Pei, Eugene Zhou, Siyu Liu, Darryl Chui, EunJeong Yoo, Stan G. Louie An analytical method using electrospray ionization and high- performance liquid chromatography/tandem mass spectrometry (LC/ESI–MS/MS) was developed to quantify the vitamin B metabolites found in the folate one-carbon metabolism, using 50 μL of human plasma. Analytes in plasma were extracted using protein precipitation after being stabilized in 1% ascorbic acid. The analytes were separated using a Kinetex 2.6 &...
Source: Journal of Pharmaceutical and Biomedical Analysis - June 1, 2018 Category: Drugs & Pharmacology Source Type: research

Aromatic aldehydes as selective fluorogenic derivatizing agents for α‐dicarbonyl compounds. Application to HPLC analysis of some advanced glycation end products and oxidative stress biomarkers in human serum
Publication date: 5 September 2018 Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 158 Author(s): Mahmoud H. El-Maghrabey, Taro Nakatani, Naoya Kishikawa, Naotaka Kuroda α-Dicarbonyl compounds (α-DCs) are very clinically important as they are considered as advanced glycation end products (AGEs) precursors and biomarkers for many chronic diseases such as diabetes and vascular diseases, in addition to their major role in progression of complications of such diseases. Aromatic aldehydes and ammonium acetate were productively used as a one-pot co-reagents for fluorogenic derivatization of α-...
Source: Journal of Pharmaceutical and Biomedical Analysis - June 1, 2018 Category: Drugs & Pharmacology Source Type: research

Degradation caused by incompatibility between sodium stearyl fumarate (PRUV) and AZD7986 in the drug product
Publication date: 5 September 2018 Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 158 Author(s): Jufang Wu Ludvigsson, Håkan Wikström, Thomas Andersson, Per-Ola Norrby During compatibility study of the AZD7986 project, a peak of 3 area% at the tail (RRT 1.03) of the active pharmaceutical ingredient (API) was discovered for all tablets containing sodium stearyl fumarate (PRUV) under humid condition (e.g. 50 °C/75% RH), regardless of choice of disintegrant or filler combination. The degradant was needed to be identified to understand the corresponding reaction mechanism and help the final ...
Source: Journal of Pharmaceutical and Biomedical Analysis - June 1, 2018 Category: Drugs & Pharmacology Source Type: research

Metabolomics and antioxidant activity of the leaves of Prunus dulcis Mill. (Italian cvs. Toritto and Avola)
Publication date: 5 September 2018 Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 158 Author(s): Alfredo Bottone, Paola Montoro, Milena Masullo, Cosimo Pizza, Sonia Piacente Prunus dulcis leaves have been reported to exert some biological activity, in particular potent free radical-scavenging capacity, but so far there is limited information on their chemical composition. With the aim to achieve deep insight on the chemical constituents of the leaves of P. dulcis cultivars “Toritto” and “Avola”, the most appreciated in Italy, an approach based on liquid chromatography-mass spectro...
Source: Journal of Pharmaceutical and Biomedical Analysis - June 1, 2018 Category: Drugs & Pharmacology Source Type: research

The determination of pharmaceutically active thiols using hydrophilic interaction chromatography followed postcolumn derivatization with o-phthaldialdehyde and fluorescence detection
Publication date: 15 July 2018 Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 156 Author(s): Michal Douša A rapid, precise and specific hydrophilic interaction chromatography (HILIC) combined with postcolumn derivatization using o-phthaldialdehyde and fluorescence detection was developed and validated for the determination of selected pharmaceutically active thiols. The analysis was carried out on a Diol HILIC column using a mobile phase consisting of acetonitrile and solution of 10 mmol/L citric acid adjusted with 1-propylamine to pH 5.5 in ratio 75:25 (v/v) for separation of cysteine and homoc...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 30, 2018 Category: Drugs & Pharmacology Source Type: research

Quantitation of polymorphic impurity in entecavir polymorphic mixtures using powder X-ray diffractometry and Raman spectroscopy
Publication date: 5 September 2018 Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 158 Author(s): Yanlei Kang, Zhanying Shao, Qiang Wang, Xiurong Hu, Dongdong Yu Entecavir was used for the treatment of chronic hepatitis B through inhibiting hepatitis B virus. The anhydrous form of entecavir (ENT-A) often appeared as impurity polymorph in the manufacturing process of entecavir monohydrate (ENT-H) such as granulation, drying and compression. Since different crystal forms might affect drug bioavailability and therapeutic effect, it was vital to control the ENT-A content of the drug product. The work aimed to...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 30, 2018 Category: Drugs & Pharmacology Source Type: research

Development of supercritical CO2 extraction of bioactive phytochemicals from black poplar (Populus nigra L.) buds followed by GC –MS and UHPLC-DAD-QqTOF-MS
Publication date: 5 September 2018 Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 158 Author(s): Piotr M. Kuś, Piotr Okińczyc, Martina Jakovljević, Stela Jokić, Igor Jerković The supercritical CO2 (SC-CO2) extraction process of black poplar (Populus nigra L.) buds was optimized (pressure, temperature) based on the yields of major phytochemicals (volatiles and non-volatiles). The optimal settings were 30 MPa/60 °C. Major volatiles determined by GC–MS in the optimized SC-CO2 extract (mg of benzyl salicylate equivalent (BSE) per 100 g of buds) were: pinostrobin chalcone (1574.2), β...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 29, 2018 Category: Drugs & Pharmacology Source Type: research

Simultaneous determination of parecoxib and its main metabolites valdecoxib and hydroxylated valdecoxib in mouse plasma with a sensitive LC –MS/MS method to elucidate the decreased drug metabolism of tumor bearing mice
In this study, a sensitive, rapid and specific LC–MS/MS method for quantification of PX, VX and OH-VX in the plasma of tumor bearing mouse was developed and validated. After protein precipitation, all the analytes were separated on an Agilent ZORBAX Extend-C18 HPLC column (2.1 × 100 mm, 3.5 μm) with gradient elution. The analytes were detected by an electrospray negative ionization mass spectrometry in the multiple reaction monitoring mode. The transition m/z 369.0 → 119.0, m/z 312.9 → 117.9, m/z 329.0 → 196.0, and m/z 307.1 → 161.3 were used for monitoring PX, V...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 27, 2018 Category: Drugs & Pharmacology Source Type: research

Simultaneous determination of tryptophan, kynurenine, kynurenic acid and two monoamines in rat plasma by HPLC-ECD/DAD
Publication date: 5 September 2018 Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 158 Author(s): Ting-ting Du, Ting Cui, Hong-mei Qiu, Nian-ru Wang, Dan Huang, Xin-hui Jiang A high-performance liquid chromatography method with a diode array and an electrochemical detection (HPLC-ECD/DAD) was developed to determine the levels of tryptophan (TRP), kynurenine (KYN), kynurenic acid (KYA), 5-hydroxytryptamine (5-HT) and 5-hydroxyindoleacetic acid (5-HIAA) in rat plasma. The prepared samples were separated on a BDS column (4.6 mm × 250 mm, 5 mm) with column oven temperature of 25 °C. The ...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 27, 2018 Category: Drugs & Pharmacology Source Type: research

Lipidomics study of the protective effects of isosteviol sodium on stroke rats using ultra high-performance supercritical fluid chromatography coupling with ion-trap and time-of-flight tandem mass spectrometry
Publication date: 5 August 2018 Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 157 Author(s): Yang Yang, Qisheng Zhong, Hao Zhang, Canlong Mo, Jinting Yao, Taohong Huang, Ting Zhou, Wen Tan Isosteviol sodium (STV-Na) was reported to possess significant protective effects on ischemic stroke in recent years. However, the protective mechanism of STV-Na against stroke was still unclear. In this work, an untargeted lipidomics approach based on the ultra high-performance supercritical fluid chromatography coupling with ion-trap and time-of-flight tandem mass spectrometry (UHSFC-IT-TOF/MS) was employed to inves...
Source: Journal of Pharmaceutical and Biomedical Analysis - May 26, 2018 Category: Drugs & Pharmacology Source Type: research