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Journal of Pharmaceutical and Biomedical Analysis

Tengfei Xu, Shizhe Li, Yufei Sun, Zifeng Pi, Shu Liu, Fengrui Song, Zhiqiang Liu
Wu-tou Decoction (WTD) is a famous traditional Chinese medicine (TCM) formula which is applied to treat arthritis and pain of joints. In this study, a sensitive and rapid method was developed for the separation and identification of the absorbed constituents and metabolites of WTD in the rats plasma by ultra high-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (UHPLC-Q-TOF-MS). A total of 22 absorbed prototype constituents and 49 metabolites were identified or tentatively characterized in dosed plasma...
April 13, 2017: Journal of Pharmaceutical and Biomedical Analysis
Emilie Bony, Yohan Mace, Adán Pinto, David Delvaux, Robert Kiss, Olivier Riant, Olivier Feron, Joëlle Quetin-Leclercq
The aim of this work is to develop the first validated HPLC-UV method quantification in blood serum for a new endoplasmic reticulum (ER)-specific benzophenazine photosensitizer (OR-141). A fast solid phase extraction (SPE) cleaning sample procedure was achieved on C18 encapped (ec) SPE cartridges and the separation was performed on a RP-18e column (5μM) using an isocratic elution with methanol. The method has been fully validated according to accuracy profiles based on total error and tolerance intervals. Calibration was performed in the matrix and trueness (<4...
April 13, 2017: Journal of Pharmaceutical and Biomedical Analysis
Szabolcs Fekete, Jean-Luc Veuthey, Davy Guillarme
The separation performance of a chromatographic system is often described in terms of column efficiency and peak capacity. Thanks to the new developments in column technology over the past few years, the achievable peak capacity drastically improved and the analysis time can be significantly shortened. Indeed, highly efficient wide-pore reversed-phase (RPLC) materials packed with small fully porous and superficially porous particles can be successfully used for the analytical characterization of therapeutic proteins...
April 12, 2017: Journal of Pharmaceutical and Biomedical Analysis
Wioleta Maruszak, Elżbieta U Stolarczyk, Krzysztof Stolarczyk
A fast capillary electrophoresis method was developed and validated for the in-process control (IPC) of the synthesis of active substances (APIs) with gold nanoparticles (AuNPs). The capillary electrophoresis method was key to ensure that the reaction step conducted in order to obtain AuNP and API conjugates will produce the expected product without the presence of free APIs, which is a critical parameter determining the quality of the synthetic material. Capillary electrophoresis was performed using uncoated fused-silica capillaries with the effective length of 40cm, 50μm i...
April 10, 2017: Journal of Pharmaceutical and Biomedical Analysis
Claudio Gardana, Cristian Del Bo', Paolo Simonetti
A simple and selective ultrahigh-performance liquid chromatographic-Orbitrap mass spectrometric (UHPLC-HR-MS) method was developed and validated for the simultaneous detection and quantification of short-chain fatty acids (SCFAs) such as acetic, propionic, butyric, isobutyric, valeric, isovaleric, 2-methyl-butyric (IS) and lactic, pyruvic and succinic acid in human faecal samples. A simple extraction procedure with 0.001% formic acid in water was performed on 40 samples. The extracts were centrifuged and analyzed by UHPLC-HR-MS on a sub-2μm column using gradient elution; meanwhile, the same samples were analyzed by GC-FID and HPLC-UV as reference methods The UHPLC-HR-MS method showed a recovery of 83-105%, a repeatability of 2...
April 10, 2017: Journal of Pharmaceutical and Biomedical Analysis
Deepti Ahluwalia, Harbhajan Dhillon, Thomas Slaney, Hangtian Song, Heather Boux, Sheetal Mehta, Lei Zhang, Anulfo Valdeza, Girija Krishnamurthy
Residual host cell proteins (HCPs) are process-related impurities present in biotherapeutics that can pose safety health risks to patients. An adequate control of HCP levels in the final product, and demonstration of HCP clearance throughout a product manufacturing process is critical for all biotherapeutic products. Developing effective downstream purification processes can be challenging as HCPs and product proteins may possess an affinity for each other or have similar physicochemical properties, resulting in co-purification...
April 9, 2017: Journal of Pharmaceutical and Biomedical Analysis
Lou Li, Liying Xu, Meng Chen, Guangbin Zhang, Hongfen Zhang, Anjia Chen
The purpose of this study was to develop a simple, quick and precise capillary zone electrophoresis method (CZE) for the separation and determination of uncaria alkaloids using dual cyclodextrins as additives for the separation. The four analytes were baseline separated within 15min at the applied voltage of 15kV with a running buffer (pH 5.7) consisting of 40.0mM phosphate buffer, 161.7mM 2-hydroxypropyl-β-cyclodextrin (HP-β-CD) and 2.21mM mono-(6-ethylenediamine-6-deoxy)-β-cyclodextrin (ED-β-CD). Under the optimum conditions, a good linearity was achieved with correlation coefficients from 0...
April 8, 2017: Journal of Pharmaceutical and Biomedical Analysis
Li Li, Dehui Yin, Kun Xu, Yushen Liu, Dandan Song, Juan Wang, Chao Zhao, Xiuling Song, Juan Li
Brucellosis is a serious zoonosis with a rapid increase in incidence across epidemic regions. Currently, there are numerous methods for diagnosing brucellosis. However, these studies often have a few defects, such as low sensitivity, poor specificity, time consuming, laborious, and even potential biological risk. To overcome these shortcomings, we have developed a rapid, sensitive and accurate diagnosis procedure for brucellosis based on the immune magnetic beads (IMB) probe and quantum dots (QDs) - staphylococcal protein A (SPA) probe...
April 6, 2017: Journal of Pharmaceutical and Biomedical Analysis
Joanna Raczak-Gutknecht, Antoni Nasal, Teresa Frąckowiak, Anita Kornicka, Franciszek Sączewski, Renata Wawrzyniak, Łukasz Kubik, Roman Kaliszan
Imidazol(in)e derivatives, having the chemical structure similar to clonidine, exert diverse pharmacological activities connected with their interactions with alpha2-adrenergic receptors, e.g. hypotension, bradycardia, sedation as well as antinociceptive, anxiolytic, antiarrhythmic, muscle relaxant and mydriatic effects. The mechanism of pupillary dilation observed after systemic administration of imidazol(in)es to rats, mice and cats depends on the stimulation of postsynaptic alpha2-adrenoceptors within the brain...
April 6, 2017: Journal of Pharmaceutical and Biomedical Analysis
Virgínia M F Gonçalves, Patrícia Rodrigues, Cláudia Ribeiro, Maria E Tiritan
A new two-dimensional liquid chromatography (2D-LC) method using a column switching valve, with a restricted-access media (RAM) column in the first dimension was developed and validated for the quantification of two β-blockers in human plasma. Several parameters, such as sample collection, mobile phase composition and flow rate for sample cleanup, transference and analytical separation of the β-blockers were investigated and optimized. The developed method allowed for the simultaneous pre-treatment and quantification of alprenolol (ALP) and propranolol (PRO) in human plasma in less than 25min...
April 2, 2017: Journal of Pharmaceutical and Biomedical Analysis
D M Mazur, G V Grishina, A T Lebedev
Synthesis of drugs, biologically active compounds or their derivatives always requires precise and reliable method of their identification, including differentiation of the possible isomers. Pseudodistamines and their precursors became a matter of elevated attention due to their different enzymatic inhibition. This paper deals with one of the groups of the pseudodistamine precursors - trans-3(4)-aminopiperidin-4(3)-ols. Their synthesis brings to a mixture of 2 regioisomers, resulting in the necessity of their reliable recognition...
April 2, 2017: Journal of Pharmaceutical and Biomedical Analysis
Xiangyuan Zheng, Lan Luo, Jie Zhou, Xiaoling Ruan, Wenyuan Liu, Feng Zheng
Acyl chlorides are important acylating agents in the synthesis of active pharmaceutical ingredients. Determining the residual acyl chlorides in drug substances is a challenge due to their high reactivity and the matrix interferences from drug substances and their related impurities. This paper describes a general derivatization HPLC method for the determination of aromatic and aliphatic acyl chlorides in lipophilic drug substances. Since most drug substances have weak absorptions in the visible range (above 380nm), the nitro-substituted anilines and nitro-substituted phenylhydrazines were selected as the derivatization reagents due to their weak basicity and red-shift of UV absorption spectra...
April 1, 2017: Journal of Pharmaceutical and Biomedical Analysis
Yang Huang, Tingting Zhang, Yumei Zhao, Haibo Zhou, Guangyun Tang, Marianne Fillet, Jacques Crommen, Zhengjin Jiang
Nucleobases, nucleosides and ginsenosides, which have a significant impact on the physiological activity of organisms, are reported to be the active components of ginseng, while they are less present in ginseng extracts. Few analytical methods have been developed so far to simultaneously analyze these three classes of compounds with different polarities present in ginseng extracts. In the present study, a simple and efficient analytical method was successfully developed for the simultaneous separation of 17 nucleobases, nucleosides and ginsenosides in ginseng extracts using supercritical fluid chromatography coupled with single quadrupole mass spectrometry (SFC-MS)...
March 31, 2017: Journal of Pharmaceutical and Biomedical Analysis
Shan Xiong, Mingxing Xue, Yanling Mu, Zhipeng Deng, Peilu Sun, Ruican Zhou
A simple and sensitive high performance liquid chromatography with tandem mass spectrometry (LC-MS/MS) method for determination of AZD3759, a novel epidermal growth factor receptor tyrosine kinase inhibitor, in rat plasma and brain homogenate was developed and validated over the range of 1.0-1000ng/mL. Chromatographic separation was carried out on a C18 column with acetonitrile and 0.1% formic acid in water as mobile phase with gradient elution at a flow rate of 0.4mL/min. The lower limits of quantification (LLOQs) were 1...
March 31, 2017: Journal of Pharmaceutical and Biomedical Analysis
Elena Sánchez-López, Alberto Marcos, Emilio Ambrosio, Oleg A Mayboroda, María Luisa Marina, Antonio L Crego
Alcohol is the most widely consumed legal drug, whereas cocaine is the illicit psychostimulant most commonly used in Europe. The combined use of alcohol and cocaine is frequent among drug-abuse consumers and leads to further exacerbation of health consequences compared to individual consumption. The pharmacokinetic and metabolic interactions leading to an increase in their combined toxicity still remains poorly understood. Here, the first metabolomics study of combined cocaine and ethanol chronic exposure effects is reported...
March 31, 2017: Journal of Pharmaceutical and Biomedical Analysis
Pavel Svoboda, Daniel Sander, Kateřina Plachká, Lucie Nováková
Matrix effect-free UHPLC-MS/MS method was developed and validated for the determination of cholesterol-lowering lovastatin in food samples represented by Pu-erh tea, oyster mushroom, and red yeast rice. The resulting method was fully validated in terms of intra-day and inter-day precision, accuracy, linearity, range, LOD, LOQ, and matrix effects. The matrix effect phenomenon evaluated by comparison of slopes of calibration curves was completely eliminated by solid-phase extraction based on the technique of molecularly imprinted polymers (MIPs)...
March 30, 2017: Journal of Pharmaceutical and Biomedical Analysis
Jakub Fibigr, Dalibor Šatínský, Petr Solich
The presented work describes the development and validation of a rapid UHPLC-UV/CAD method using a core-shell particle column for the separation and quantitative analysis of seven plant sterols and stanols. The phytosterols (ergosterol, brassicasterol, campesterol, fucosterol, stigmasterol, and β-sitosterol) and the phytostanol stigmastanol were separated and analyzed in 8.5min. The sample pre-treatment procedure was optimized to be less time-consuming than any other published method, especially due to no need of derivatization, evaporation and even reconstitution step...
March 30, 2017: Journal of Pharmaceutical and Biomedical Analysis
Chang-Jiang-Sheng Lai, Yuan Yuan, Da-Hui Liu, Chuan-Zhi Kang, Yu Zhang, Liangping Zha, Liping Kang, Tong Chen, Tie-Gui Nan, Qing-Xiu Hao, Lu-Qi Huang
In order to comprehensively elucidate the chemical biosynthesis process of the beige-scape Gastrodia elata Blume (Wutianma) as a traditional herbal medicines, the untargeted analysis-based UHPLC-PDA-ESI-Q-TOF-MS reveals the metabolites ranging from the skeletons to novel dimers of citric acids in fresh and dried immature/mature stem tubers. Interestingly, two novel types of dimers for citric acids with the anhydride groups at sn-1 and/or sn-5 were discovered in fresh samples. Moreover, the classical mono- versus novel di-mers, and the aglycons versus the glycosides could be easily discriminated by signature fragmentation patterns and some novel adduct ions...
March 29, 2017: Journal of Pharmaceutical and Biomedical Analysis
F Rinaldi, S Tengattini, E Calleri, T Bavaro, L Piubelli, L Pollegioni, G Massolini, C Temporini
Proteins and glycoproteins with therapeutic activity are susceptible to environmental factors, which can cause their degradation and the loss of their activity. Thus, the maintenance of their stability during the production process is a critical factor. In this work, a simple and rapid hydrophilic interaction liquid chromatography HILIC-UV method was validated in terms of accuracy, precision, linearity, LOD, LOQ and specificity and applied to the investigation of the stability of intact proteins and their neo-glycoconjugates with antigenic activity against tuberculosis...
March 28, 2017: Journal of Pharmaceutical and Biomedical Analysis
Lu Wang, Xin Zheng, Weicong Wang, Pei Hu, Ji Jiang
AC0010 is an irreversible, mutant-selective EGFR inhibitor that effectively inhibits EGFR active and T790M resistance mutations in non-small cell lung cancer (NSCLC). A sensitive ultra-performance liquid chromatography - tandem mass spectrometry (UPLC-MS/MS) method was developed and fully validated for determining AC0010 and its metabolites in human plasma. The samples were purified by solid-phase extraction (SPE) columns and separated on a BEH C18 column. Electrospray ionization (ESI) in positive ion mode and multiple reaction monitoring (MRM) were used to monitor the ion transitions of AC0010 (m/z 488→257) and its metabolites M1 (m/z 474→403), M2 (m/z 504→487), M4 (m/z 434→377), M7 (m/z 490→405), MII-1 (m/z 651→434) and MII-2 (m/z 609→434)...
March 28, 2017: Journal of Pharmaceutical and Biomedical Analysis
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