Identification of Prototype Compounds and Derived Metabolites of Naoxintong Capsule in Beagle Dog Urine and Feces by UFLC-Q-TOF-MS/MS
In this study, by applying the ultra-fast liquid chromatography/quadrupole-time-of-flight tandem mass spectrometry (UFLC-Q-TOF-MS/MS), we have investigated the in vivo metabolism of NXTC in beagle dog urine and feces. After a single dose of oral administration, a total of 36 prototype compounds and 52 metabolites of NXTC were identified or tentatively characterized in beagle dog urine and feces. We have also proposed the in vivo transformation pathways of such metabolites including phase I (reduction, oxidation, hydroxylation, demethylation) and phase II reactions (glucuronidation, sulfation, methylation). For the first ti...
Source: Journal of Pharmaceutical and Biomedical Analysis - August 6, 2019 Category: Drugs & Pharmacology Source Type: research

Quantification of urinary derivatives of Phenylbutyric and Benzoic acids by LC-MS/MS as treatment compliance biomarkers in Urea Cycle disorders
Publication date: 30 November 2019Source: Journal of Pharmaceutical and Biomedical Analysis, Volume 176Author(s): Fernando Andrade, Isidro Vitoria, Elena Martín Hernández, Guillem Pintos-Morell, Patricia Correcher, Rocío Puig-Piña, Pilar Quijada-Fraile, Luis Peña-Quintana, Ana Mª Marquez, Olatz Villate, Mª Teresa García Silva, Javier de las Heras, Leticia Ceberio, Esmeralda Rodrigues, Teresa Almeida Campos, Raquel Yahyaoui, Javier Blasco, Inmaculada Vives-Piñera, David Gil, Mireia del ToroAbstractPurposeSalts of phenylacetic acid (PAA) and phenylbutyric acid (PBA) ...
Source: Journal of Pharmaceutical and Biomedical Analysis - August 6, 2019 Category: Drugs & Pharmacology Source Type: research

Potential hepatoxicity risk of the shell of Herpetospermum caudigerum Wall in rats based on 1H-NMR metabonomics
Publication date: 30 November 2019Source: Journal of Pharmaceutical and Biomedical Analysis, Volume 176Author(s): Xin Feng, Han Xu, Jian-Feng Chen, Ling-Yu Ruan, Wen-Long Zhao, Hui-Hui Meng, Wen-Ya Liu, Wen-Li Zhao, Qi Zheng, Zhi-Chao Liu, Zhao-Ben Kan, Ge-Jia Zhong, Jun-Song WangAbstractThe Herpetospermum caudigerum Wall (HCW) is a traditional Tibetan medicine and is widely used in clinical practice. However, the shell of the HCW (SHCW) has rarely been studied, and some researchers have suggested that the SHCW may be toxic. Therefore, in this study, SHCW was administered to rats at two doses (0.1 and 0.33 g/kg) once a d...
Source: Journal of Pharmaceutical and Biomedical Analysis - August 6, 2019 Category: Drugs & Pharmacology Source Type: research

Electrochemical oxidation of selected immunosuppressants and identification of their oxidation products by means of liquid chromatography and tandem mass spectrometry (EC-HPLC-MS/MS)
Publication date: 30 November 2019Source: Journal of Pharmaceutical and Biomedical Analysis, Volume 176Author(s): Malgorzata Szultka-Mlynska, Boguslaw BuszewskiAbstractElectrochemistry (EC) coupled with liquid chromatography and tandem mass spectrometry (HPLC/ESI-MS/MS) was used to study the oxidation products of cyclosporine A (CYC), everolimus (EWE), mycophenolic acid (MFA), sirolimus (SIR) and tacrolimus (TAK). Mimicry of the oxidative phase I and II metabolism was achieved in a thin-layer cell equipped with a boron doped diamond (BDD) working electrode. Structures of the electrochemically generated products were elucid...
Source: Journal of Pharmaceutical and Biomedical Analysis - August 6, 2019 Category: Drugs & Pharmacology Source Type: research

Application of reversed-phase thin layer chromatography and QSRR modelling for prediction of protein binding of selected β-blockers
Publication date: 30 November 2019Source: Journal of Pharmaceutical and Biomedical Analysis, Volume 176Author(s): Krzesimir Ciura, Piotr Kawczak, Katarzyna Ewa Greber, Hanna Kapica, Joanna Nowakowska, Tomasz BączekAbstractChromatographic properties of sixteen β-blockers were studied using planar chromatography. The aim of presented study was to investigate influence of different organic solvents (acetonitrile, methanol, dioxin and tetrahydrofurane) on β-blockers’ retention on C18 bonded silica gel stationary phase. Group of sixteen, diverse in terms of structure, beta blockers was used as a model set. The ...
Source: Journal of Pharmaceutical and Biomedical Analysis - August 6, 2019 Category: Drugs & Pharmacology Source Type: research

Chromatographic methods and sample pretreatment techniques for aldehydes determination in biological, food, and environmental samples
Publication date: 25 October 2019Source: Journal of Pharmaceutical and Biomedical Analysis, Volume 175Author(s): Naoya Kishikawa, Mahmoud H. El-Maghrabey, Naotaka KurodaAbstractAldehydes are very reactive carbonyl compounds that are widespread naturally. Aldehydes can be produced in vivo by oxidative reactions and are able to disturb biological functions through binding and modifying biomolecules. Thus, it is necessary to determine their levels in biological samples to estimate their possible adverse effect on human health in addition to their consideration as a biomarker for oxidative stress-related diseases. Furthermore,...
Source: Journal of Pharmaceutical and Biomedical Analysis - August 5, 2019 Category: Drugs & Pharmacology Source Type: research

A high resolution LC–MS targeted method for the concomitant analysis of 11 contraceptive progestins and 4 steroids
Publication date: 25 October 2019Source: Journal of Pharmaceutical and Biomedical Analysis, Volume 175Author(s): Csaba Ferenc Laszlo, Jonathan Paz Montoya, Marie Shamseddin, Fabio De Martino, Alexandre Beguin, Rene Nellen, Stephen James Bruce, Marc Moniatte, Hugues Henry, Cathrin BriskenAbstractIn the context of hormonal contraception and hormone replacement therapy (HRT), many women are exposed to exogenous hormones. Current use of hormonal contraception with combined ethinyl estradiol and different progestins bestows a breast cancer relative risk (RR) of 1.2- while combined HRT has a RR of 2. Although these exposures pre...
Source: Journal of Pharmaceutical and Biomedical Analysis - August 5, 2019 Category: Drugs & Pharmacology Source Type: research

An artifactual solution degradant of pregabalin due to adduct formation with acetonitrile catalyzed by alkaline impurities during HPLC sample preparation
Publication date: 25 October 2019Source: Journal of Pharmaceutical and Biomedical Analysis, Volume 175Author(s): Jinsheng Lin, Xiaofei Liu, Jing Wang, Dan Li, Wenquan Zhu, Wenbin Chen, Xianhua Zhang, Qiangming Li, Min LiAbstractDuring the HPLC related substances testing of pregabalin API, an unknown peak was observed at a level exceeding the identification threshold. Preliminary investigation revealed that this impurity is not a process impurity but rather an artifactual solution degradant or “ghost peak” during the HPLC analysis. By using a strategy that combines LC-PDA/UV-MSn with mechanism-based stress studi...
Source: Journal of Pharmaceutical and Biomedical Analysis - August 4, 2019 Category: Drugs & Pharmacology Source Type: research

Screening and analysis of cyclooxygenase-2 inhibitors from the complex matrix: A case study to illustrate the important effect of immobilized enzyme activity in magnetic ligand fishing
Publication date: 25 October 2019Source: Journal of Pharmaceutical and Biomedical Analysis, Volume 175Author(s): Dapeng Li, Lin Xu, Jin Qi, Boyang YuAbstractMagnetic ligand fishing is one of the most widely used methods to screen and separate potentially bioactive compounds from complex mixtures. However, it is poorly understood the ambiguous relations between immobilized enzyme activity and fishing results (accuracy and sensitivity). Therefore, to investigate the underlying relationship of them, we fabricated the immobilized enzyme with different activities by introducing a novel support material, nickel ions (Ni2+) funct...
Source: Journal of Pharmaceutical and Biomedical Analysis - August 4, 2019 Category: Drugs & Pharmacology Source Type: research

Study on hepatotoxicity of different dosages of Polygoni multiflori radix praeparata in rats by metabolomics based on UPLC-Q-TOF-MS
Publication date: 25 October 2019Source: Journal of Pharmaceutical and Biomedical Analysis, Volume 175Author(s): Xiaohong Gong, Meichen Liu, Lihong Gong, Yunxia Li, Cheng PengAbstractAs a kind of replenishing Chinese medicine, polygoni multiflori radix praeparata (PMP) had high application value in clinic. However, with the increase of clinical applications, more and more hepatotoxicity reports have been reported which had shown has a dose-time-toxicity dependent correlation of PMP hepatotoxicity. Therefore, it was particularly important to investigate the safe and effective dose of PMP in clinical drug administration. At ...
Source: Journal of Pharmaceutical and Biomedical Analysis - August 4, 2019 Category: Drugs & Pharmacology Source Type: research

Separation and characterization of unknown impurities in latamoxef sodium by LC-Q-TOF MS and a summary of their positive-ion fragmentation regularities
Publication date: 25 October 2019Source: Journal of Pharmaceutical and Biomedical Analysis, Volume 175Author(s): Lulu He, Jianqin Qian, Peixi Zhu, Weifeng Yang, Yuanbin SheAbstractA simple and sensitive method was developed for separation and characterization of seventeen impurities from commercial latamoxef sodium for injection by liquid chromatography combined with electrospray ionization and QTOF mass spectrometer (LC-ESI-QTOF MS). The chromatographic separation was performed on a Boston Green ODS-AQ C18 column (250 mm × 4.6 mm, 5 μm) under gradient mode using binary mobile phase: (A) ammonium acetate...
Source: Journal of Pharmaceutical and Biomedical Analysis - August 2, 2019 Category: Drugs & Pharmacology Source Type: research

Two validated liquid chromatography–mass spectrometry methods with different pretreatments for the quantification of an anti-CD47 monoclonal antibody in rat and cynomolgus monkey serum compared with an electrochemiluminescence method
In conclusion, the established LC–MS methods exhibited superior accuracy, efficiency and cost-effectiveness for the PK assessment of SHR-1603 in the preclinical study. Thus, it provides a promising alternative to LBA in pre-clinical and clinical evaluation studies of mAb drugs in various matrices to facilitate the development of anti-tumor drugs.Graphical abstract (Source: Journal of Pharmaceutical and Biomedical Analysis)
Source: Journal of Pharmaceutical and Biomedical Analysis - August 1, 2019 Category: Drugs & Pharmacology Source Type: research

Development of a novel assay of molecularly imprinted membrane by design-based gaussian pattern for vancomycin determination
Publication date: 25 October 2019Source: Journal of Pharmaceutical and Biomedical Analysis, Volume 175Author(s): Haining Yu, Ru Yao, Shengrong ShenAbstractA molecularly imprinted membrane (MIM) with vancomycin (VCM) as a template and other related different material membranes (organic nylon microporous membranes, polyvinylidene fluoride (PVDF) membranes, polypropylene membranes) as a support respectively were synthesized by surface imprinting for the selective absorption of VCM, which can be used for pretreatment biological samples and rapid determination of VCM. The optimal ratio of template and functional monomer was 1:4...
Source: Journal of Pharmaceutical and Biomedical Analysis - August 1, 2019 Category: Drugs & Pharmacology Source Type: research

Challenges in simultaneous extraction and chromatographic separation of metformin and three SGLT-2 inhibitors in human plasma using LC–MS/MS
Publication date: 25 October 2019Source: Journal of Pharmaceutical and Biomedical Analysis, Volume 175Author(s): Priyanka A. Shah, Pranav S. Shrivastav, Vinay Sharma, Manish S. YadavAbstractOptimization of extraction and chromatographic conditions is essential for the simultaneous analysis of drugs having different physico-chemical properties, especially for in vivo applications. The present work describes concurrent estimation of metformin (MET) and three sodium-glucose co-transporter 2 (SGLT-2) inhibitors namely canagliflozin (CANA), dapagliflozin (DAPA) and empagliflozin (EMPA) in human plasma by liquid chromatography-t...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 29, 2019 Category: Drugs & Pharmacology Source Type: research

Challenges and opportunities in blood flow through porous substrate: A design and interface perspective of dried blood spot
Publication date: 25 October 2019Source: Journal of Pharmaceutical and Biomedical Analysis, Volume 175Author(s): Prasoon Kumar, Prashant Agrawal, Kaushik ChatterjeeAbstractBlood microsampling is desired in clinical, pharmaceutical and biomedical fields to overcome the challenges of conventional whole blood sampling. One of the popular methods for blood microsampling is the dried blood spot (DBS) kit and the collected sample is subsequently used for bioanalysis. The current practice of DBS is simple to use, cheap and very well standardized from sample collection to analysis. However, DBS suffers from several well documented...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 29, 2019 Category: Drugs & Pharmacology Source Type: research

Simultaneous enantiomeric analysis of six chiral pesticides in functional foods using magnetic solid-phase extraction based on carbon nanospheres as adsorbent and chiral liquid chromatography coupled with tandem mass spectrometry
Publication date: 25 October 2019Source: Journal of Pharmaceutical and Biomedical Analysis, Volume 175Author(s): Pengfei Zhao, Shuang Li, Xiaoming Chen, Xingjie Guo, Longshan ZhaoAbstractThis work presented a novel method for the simultaneous enantioselective analysis of six chiral pesticides in seven functional foods at enantiomeric levels. Samples were extracted from matrices using a magnetic solid-phase extraction method based on Fe3O4 modified carbon nanospheres as adsorbent. Experimental variables were optimized using one-variable-at-a-time and response surface methodology. Six chiral pesticides were simultaneously en...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 27, 2019 Category: Drugs & Pharmacology Source Type: research

High-throughput screening of the nucleosides and nucleotides using characteristic structural fragments fusion
Publication date: 25 October 2019Source: Journal of Pharmaceutical and Biomedical Analysis, Volume 175Author(s): Wei Jia, Lin Shi, Feng Zhang, James Chang, Xiaogang ChuAbstractCordyceps sinensis is a traditional Chinese food. A high-throughput screening and quantitative method based on hydrophilic interaction chromatography coupled to quadrupole/Orbitrap high resolution mass spectrometry has been proposed for the joint measurement of nucleosides and their corresponding nucleotides in thirty-two Cordyceps sinensis samples. A total of thirty-two natural samples from six regions were enrolled. A multiple-step analysis strateg...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 27, 2019 Category: Drugs & Pharmacology Source Type: research

Daptomycin-modified magnetic beads integrated with lysostaphin for selective analysis of Staphylococcus
Publication date: 25 October 2019Source: Journal of Pharmaceutical and Biomedical Analysis, Volume 175Author(s): Mengyao Wang, Enci Fan, Yue Wu, Zhifeng FuAbstractAn antibiotic-affinity method was developed for analyzing Staphylococcus on the basis of the strong binding capability of daptomycin towards Gram-positive bacteria cellular membrane, as well as the selective lytic action of lysostaphin towards Staphylococcus. Daptomycin-modified magnetic beads were adopted to enrich Staphylococcus from sample matrix. Afterwards lysostaphin was adopted to lyse Staphylococcus, which can hydrolyze pentaglycine cross-linkers of pepti...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 26, 2019 Category: Drugs & Pharmacology Source Type: research

Development and validation of reverse-phase high-performance liquid chromatographic (RP-HPLC) method for quantification of Efavirenz in Efavirenz-Enfuvirtide co-loaded polymer-lipid hybrid nanoparticles
The objective of present work was to develop rapid, sensitive, selective, accurate and precise RP-HPLC method for analysis of Efavirenz from combination anti-HIV drug (Efavirenz-Enfuvirtide) incorporated into polymer-lipid hybrid nanoparticles (PLN). Chromatographic separation of Efavirenz was performed on Waters Spherisorb® 5 μm ODS (C18) column (4.6 x 250 mm) with acetonitrile and 10 mM phosphate buffer pH 6.8 (70:30, v/v) as mobile phase. The UV detection wavelength was 246 nm. The method was found to be linear between the concentration range of 500–20000 ng/ml with 160 ng/ml and 480 ng/ml...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 24, 2019 Category: Drugs & Pharmacology Source Type: research

Part 1: Physicochemical characterization of bevacizumab in undiluted 25 mg/mL drug product solutions: Comparison of originator with a biosimilar candidate
In this study 13 orthogonal, spectroscopy and particle size determination methods were used to characterize the structure and aggregation of undiluted, 25 mg/mL bevacizumab drug products Avastin® manufactured in the USA and in Europe, and ABX-BEV, a bevacizumab biosimilar candidate produced by Apobiologix Inc. Secondary structure, conformation and the potential occurrence of chemical degradation of the monoclonal antibodies were characterized and compared using infrared spectroscopy, intrinsic fluorescence and ANS fluorescence spectroscopy. Protein aggregation and particulate matter in the monoclonal antibody solutio...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 23, 2019 Category: Drugs & Pharmacology Source Type: research

LC-Q-TOF/MS-oriented systemic metabolism study of pedunculoside with in vitro and in vivo biotransformation
This study would contribute to a better understanding of pedunculoside metabolism, which can provide scientific evidence for its pharmacodynamic mechanism research and prove its clinical application.Graphical abstract (Source: Journal of Pharmaceutical and Biomedical Analysis)
Source: Journal of Pharmaceutical and Biomedical Analysis - July 21, 2019 Category: Drugs & Pharmacology Source Type: research

Online comprehensive hydrophilic interaction chromatography × reversed phase liquid chromatography coupled to mass spectrometry for in depth peptidomic profile of microalgae gastro-intestinal digests
In this study, a comprehensive hydrophilic interaction chromatography × reversed phase coupled to high resolution mass spectrometry was developed for the peptide profile of microalgae formulations subjected to gastro-intestinal digestion. A BEH Amide column was employed in the first dimension, while a BIOshell ES-C18 Peptide in the second. As modulation interface, two trapping columns, in house packed with 1.9 µm fully porous monodisperse C18 particles characterized by high retention and efficiency, were tested and compared with SecurityGuard C18 cartridges, together with a dilution flow, t...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 20, 2019 Category: Drugs & Pharmacology Source Type: research

Incorporating solid-phase extraction into compendial procedures for the determination of dexamethasone and impurities in low-dose drug products
Publication date: Available online 19 July 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Qun XuAbstractA low-dose drug product is characterized by extremely low concentrations of analytes and a high ratio of excipients to the drug substance; the analysis of these drug products presents a number of analytical challenges for detection and quantitation, which in turn could impact potency, purity, and uniformity of the dosage units. In this work solid-phase extraction (SPE) was used to enrich analytes and minimize the interference of excipients, despite the fact that the application of SPE to pharmace...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 20, 2019 Category: Drugs & Pharmacology Source Type: research

Quantification of coagulation factor VIII in human plasma with liquid chromatography tandem mass spectrometry using a selective sample purification with camelid nanobodies
Publication date: Available online 19 July 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Mohsin El Amrani, Anouk A.M. Donners, Gerard Graat, Eef G. Lentjes, Albert Huisman, Ruben E.A. Musson, Erik M. van MaarseveenAbstractPatients with hemophilia A are currently diagnosed and monitored by measuring the activity of coagulation factor VIII (FVIII) in plasma mostly with the one-stage clotting assay (OSA). Although the OSA is routinely available in many clinical laboratories, it has in some circumstances relatively low sensitivity and specificity. Therefore, the FVIII activity as a biomarker does not ...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 20, 2019 Category: Drugs & Pharmacology Source Type: research

Sensitive and reliable gas chromatography tandem mass spectrometry assay for ethyl glucuronide in neonatal meconium
Publication date: 25 October 2019Source: Journal of Pharmaceutical and Biomedical Analysis, Volume 175Author(s): Nunzia La Maida, Annagiulia Di Trana, Giulio Mannocchi, Simona Zaami, Francesco Paolo BusardòAbstractPrenatal exposure to maternal ethanol leads to serious physical and mental irreversible disabilities. Ethyl glucuronide (EtG) is a direct metabolite of alcohol and its measurement in neonatal meconium has been established as the best biomarker to assess prenatal exposure to social and excessive gestational ethanol.We developed and validated the first gas chromatography tandem mass spectrometry method to qu...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 20, 2019 Category: Drugs & Pharmacology Source Type: research

One-pot preparation of zwitterionic sulfoalkylbetaine monolith for rapid and efficient separation of lysozyme from egg white
Publication date: 25 October 2019Source: Journal of Pharmaceutical and Biomedical Analysis, Volume 175Author(s): Wei Gao, Xiao-lan Liu, Jia-yuan Li, Hong-zhen Lian, Li MaoAbstractA porous zwitterionic monolithic column was prepared to rapidly and efficiently separate lysozyme from egg white. The monolith was synthesized in a stainless steel HPLC column (5 cm × 4.6 mm i.d.) by in-situ thermal initiated co-polymerization of N,N-dimethyl-N-methacryloxyethyl-N-(3-sulfopropyl) ammonium betaine (MSA) and ethylene dimethacrylate (EDMA). Due to the combination of quaternary ammonium and sulfonic groups on the monolithic matr...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 20, 2019 Category: Drugs & Pharmacology Source Type: research

An improved 2D-HPLC-UF-ESI-TOF/MS approach for enrichment and comprehensive characterization of minor neuraminidase inhibitors from Flos Lonicerae Japonicae
This study provides support for the rapid screening of minor neuraminidase inhibitors from complex natural medicines.Graphical abstract (Source: Journal of Pharmaceutical and Biomedical Analysis)
Source: Journal of Pharmaceutical and Biomedical Analysis - July 20, 2019 Category: Drugs & Pharmacology Source Type: research

Characterization of unknown impurities in Coenzyme Q10 using LC–MS and NMR
In this study, an ultra-performance liquid chromatography complied with quadrupole time-of-flight tandem mass spectrometry (UPLC-QTOF/MS) via atmospheric pressure chemical ionization (APCI) was used to identify the proposed structure of the three impurities (Impurity 1, Impurity 2-1 and Impurity 2-2). We got the three impurities through preparative high performance liquid chromatography and their structures were further confirmed by 1D and 2D nuclear magnetic resonance (NMR). Based on the significance of these results, Impurity 1 was the impurity E referred in British Pharmacopoeia (BP), Impurity 2-1 and Impurity 2-2 were ...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 20, 2019 Category: Drugs & Pharmacology Source Type: research

Development and validation of Reversed-phase high-performance liquid chromatography (RP-HPLC) method for quantification of Efavirenz in Efavirenz-Enfuvirtide co-loaded polymer-lipid hybrid nanoparticles
The objective of present work was to develop rapid, sensitive, selective, accurate and precise RP-HPLC method for analysis of Efavirenz from combination anti-HIV drug (Enfuvirtide-Efavirenz) incorporated into polymer-lipid hybrid nanoparticles (PLN). Chromatographic separation of Efavirenz was performed on Waters Spherisorb® 5 µm ODS (C18) column (4.6 x 250 mm) with acetonitrile and 10 mM phosphate buffer pH 6.8 (70:30, v/v) as mobile phase. The UV detection wavelength was 246 nm. The method was found to be linear between the concentration range of 500-20000 ng/ml ...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 20, 2019 Category: Drugs & Pharmacology Source Type: research

Highly sensitive HPLC-MS/MS assay for the quantitation of ondansetron in rat plasma and rat brain tissue homogenate following administration of a very low subcutaneous dose
The objective of this study was to develop and validate a highly sensitive HPLC-MS/MS assay capable of quantifying ondansetron in rat plasma and rat brain homogenate following a low subcutaneous administration of 1.0 µg/kg. Ondansetron was extracted by protein precipitation with methanol containing labeled ondansetron. The chromatography was performed on a Thermo Scientific Aquasil C18 analytical column (100 x 2.1 mm I.D., 5 μm) operating at 40 °C. The mobile phase consisted of acetonitrile and 10 mM ammonium formate pH 3 at a ratio of 30:70, respectively. The f...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 20, 2019 Category: Drugs & Pharmacology Source Type: research

Analysis of impurities of cannabidiol from hemp. Isolation, characterization and synthesis of cannabidibutol, the novel cannabidiol butyl analog
Publication date: Available online 12 July 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Cinzia Citti, Pasquale Linciano, Flavio Forni, Maria Angela Vandelli, Giuseppe Gigli, Aldo Laganà, Giuseppe CannazzaAbstractCannabidiol (CBD), one of the two major active principles present in Cannabis sativa, is gaining great interest among the scientific community for its pharmaceutical, nutraceutical and cosmetic applications. CBD can be prepared either by chemical synthesis or extraction from Cannabis sativa (hemp). The latter is more convenient from several points of view, including environmental a...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 20, 2019 Category: Drugs & Pharmacology Source Type: research

Novel amperometric flow-injection analysis of creatinine using a molecularly-imprinted polymer coated copper oxide nanoparticle-modified carbon-paste-electrode
We report a novel amperometric flow-injection (FI) analysis of creatinine based on a sensor comprising copper oxide nanoparticles (CuO) coated with a molecularly-imprinted polymer (CuO@MIP) and decorating a carbon-paste electrode (CPE) to form the CuO@MIP/CPE electrode. The CuO@MIP was synthesized by using CuO as the supporting core, creatinine as the template, methacrylic acid (MAA) as monomer, N, N′-(1,2-dihydroxyethylene)bis(acrylamide) (DHEBA) as cross-linker, and 2,2′-azobis (2-methylpropionitrile) (AIBN) as initiator. Morphology and structural characterization reveal that CuO nanoparticle imprinted sites ...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 20, 2019 Category: Drugs & Pharmacology Source Type: research

Characterization of unknown impurities in Coenzyme Q10 using LC-MS and NMR
In this study, an ultra-performance liquid chromatography complied with quadrupole time-of-flight tandem mass spectrometry (UPLC-QTOF/MS) via atmospheric pressure chemical ionization (APCI) was used to identify the proposed structure of the three impurities (Impurity 1, Impurity 2-1 and Impurity 2-2). We got the three impurities through preparative high performance liquid chromatography and their structures were further confirmed by 1D and 2D nuclear magnetic resonance (NMR). Based on the significance of these results, Impurity 1 was the impurity E referred in British Pharmacopoeia (BP), Impurity 2-1 and Impurity 2-2 were ...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 20, 2019 Category: Drugs & Pharmacology Source Type: research

Nutraceutical Polyphenols: new analytical challenges and opportunities
Publication date: Available online 15 July 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Simona Piccolella, Giuseppina Crescente, Lorenzo Candela, Severina PacificoAbstractNowadays, the research for secondary metabolites with health promoting effects in countering or slowing-down chronic and degenerative diseases (e.g. cancer, cardiovascular, and neurodegenerative diseases) identify phenols and polyphenols, widespread and mostly copious in dietary plant sources, as beneficial for human health. These compounds, as intrinsically antioxidant, are claimed as nutraceuticals with preventive efficacy in ...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 20, 2019 Category: Drugs & Pharmacology Source Type: research

Simultaneous determination of alflutinib and its active metabolite in human plasma using liquid chromatography–tandem mass spectrometry
Publication date: Available online 16 July 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Xiaoyun Liu, Wei Li, Yifan Zhang, Yong Jiang, Qianyu Zhao, Dafang ZhongAbstractAlflutinib, or known as AST2818, is an irreversible tyrosine kinase inhibitor that selectively inhibits EGFR mutations, especially T790M. At present, alflutinib has undergone phase II/III clinical trials for non-small cell lung cancer (NSCLC) treatment in China. The present study aimed to analye the pharmacokinetics of alflutinib and its active metabolite AST5902 in a plasma sample of NSCLC patient. A sensitive and highly selective ...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 20, 2019 Category: Drugs & Pharmacology Source Type: research

Large inter-individual variability in pharmacokinetics of dexmedetomidine and its two major N-glucuronides in adult intensive care unit patients
Publication date: Available online 16 July 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Mengbi Yang, Andrew H.W. Tse, Anna Lee, Gavin M. Joynt, Zhong ZuoAbstractDexmedetomidine (DMTD), an α2-adrenoceptor agonist, is commonly used for sedation and analgesia in intensive care unit (ICU) patients. The primary plasma metabolites of DMTD are its direct N-glucuronides, namely N3-glucuronide of dexmedetomidine (DG1) and N1-glucuronide of dexmedetomidine (DG2), accounting for 41% of DMTD metabolism in healthy volunteers. Since variations on the extent of N-glucuronidation could be one of the key fa...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 20, 2019 Category: Drugs & Pharmacology Source Type: research

A novel peptide-based sensor platform for detection of anti-Toxoplasma gondii immunoglobulins
Publication date: Available online 17 July 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Lívia M. Alves, Heber L.S. Barros, José M.R. Flauzino, Pedro H.G. Guedes, Janser M. Pereira, Ricardo Toshio Fujiwara, Tiago W.P. Mineo, José R. Mineo, Ronaldo J. de Oliveira, João M. Madurro, Ana G.Brito-MadurroAbstractToxoplasma gondii is an intracellular protozoan parasite responsible for toxoplasmosis, which affects humans and animals. Serologic detection of anti-T. gondii immunoglobulins plays a crucial role in the clinical diagnosis of toxoplasmosis. In this work, a novel elect...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 20, 2019 Category: Drugs & Pharmacology Source Type: research

Polysaccharide deriving from Ophiopogonis Radix promotes metabolism of ginsenosides in the present of human gut microbiota based on UPLC-MS/MS assay
Publication date: Available online 17 July 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Huai-You Wang, Cheng Wang, Shu-Chen Guo, Zhi-Cong Chen, Zhi-Tian Peng, Ran Duan, Tina T.X. Dong, Karl W.K. TsimAbstractThe combined usage of Ginseng Radix et Rhizoma (ginseng) and Ophiopogonis Radix is common in oriental countries for thousands of years. The major active constituents of ginseng are ginsenosides, and the conversion of ginsenosides to different metabolites by gut microbiota has been reported. However, the effect of Ophiopogonis Radix, especially its polysaccharides, on the metabolism of ginsenos...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 20, 2019 Category: Drugs & Pharmacology Source Type: research

Cost-effective monitoring of microRNA-205 applied as a biomarker using G-quadruplex DNAzyme and 1,1’-oxalyldiimidazole chemiluminescence
Publication date: Available online 18 July 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Kyungeun Kim, Prestan Park, Ji Hoon LeeAbstractTrace levels of microRNA-205, known as a biomarker of lung cancer, in human serum was quantified for the first-time using G-quadruplex DNAzyme linked to detection complementary probe and 1,1’-oxalyldiimidazole chemiluminescence (ODI-CL). First, capture complementary probes immobilized on the surface of paramagnetic bead selectively bound with microRNA-205 existing in human serum. Then, with the addition of detection complementary probe linked to hemin aptame...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 20, 2019 Category: Drugs & Pharmacology Source Type: research

Simulation of Phase I Metabolism Reactions of Selected Calcium Channel Blockers by Human Liver Microsomes and Photochemical Methods with the use of Q-TOF LC/MS
Publication date: Available online 19 July 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Maciej Gawlik, Jakub Trawiński, Robert SkibińskiAbstractThe in vitro phase I metabolism of perhexiline and flunarizine, two calcium channel blockers was investigated during this study with the use of human liver microsomes (HLM) method compared with TiO2, WO3 and ZnO catalyzed photochemical reaction. In order to determine the structures of metabolites an quadrupole time-of-flight mass spectrometry combined with liquid chromatography (Q-TOF LC/MS) system was used. The obtained high resolution mass spectra ena...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 20, 2019 Category: Drugs & Pharmacology Source Type: research

Simultaneous determination of phenolic acids and flavonoids in Artemisiae Argyi Folium by HPLC-MS/MS and discovery of antioxidant ingredients based on relevance analysis
Publication date: 25 October 2019Source: Journal of Pharmaceutical and Biomedical Analysis, Volume 175Author(s): Jia-Xuan Xia, Bin-Bin Zhao, Jun-Feng Zan, Ping Wang, Lin-Lin ChenAbstractA rapid and reliable LC–MS/MS method was developed for the quantitation of major components in Folium Artemisiae Argyi (mugwort), a widely used traditional Chinese herbal medicine. A total of 5 phenolic acids and 17 flavonoids were separated and simultaneously determined by using a Shiseido C18 column (150 × 3.0 mm, 3 μm) and gradient elution of acetonitrile-aqueous formic acid (100:0.1, v/v) at a 0.5 mL min&minus...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 20, 2019 Category: Drugs & Pharmacology Source Type: research

Rosmarinic and carnosic acid contents and correlated antioxidant and antidiabetic activities of 14 Salvia species from Anatolia
This study firstly aims the determination of rosmarinic and carnosic acid contents of 14 Anatolian Salvia species by a simple and rapid capillary electrophoresis method. Moreover, the antioxidant activities and total phenolic contents of the Salvia samples were investigated. α-Glucosidase enzyme inhibitory effects of the samples were tested concerning their antidiabetic activities. The rosmarinic acid contents in the samples were well-correlated with the bioactivitiesGraphical abstract (Source: Journal of Pharmaceutical and Biomedical Analysis)
Source: Journal of Pharmaceutical and Biomedical Analysis - July 20, 2019 Category: Drugs & Pharmacology Source Type: research

Liquid chromatography–tandem mass spectrometry for the simultaneous quantitation of enmetazobactam and cefepime in human plasma
Publication date: 10 September 2019Source: Journal of Pharmaceutical and Biomedical Analysis, Volume 174Author(s): M. Mameli, A. Vezzelli, S. Verze’, S. Biondi, P. Motta, A. Greco, M. Michi, M. BredaAbstractA simple ultra-performance liquid chromatography-tandem mass spectrometry (UPLC–MS/MS) method was developed and validated for the simultaneous analysis enmetazobactam (also known as AAI101) and cefepime in human plasma. Sample preparation was based on protein precipitation with acetonitrile. Separation was performed on Acquity BEH HILIC column (50 mm × 2.1 mm, 1.7 μm) with a mobile phase c...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 7, 2019 Category: Drugs & Pharmacology Source Type: research

Effect of Xiao-Ai-Ping injection on paclitaxel pharmacokinetics in rats by LC–MS/MS method
In conclusion, pretreatment with XAP enhanced the exposure of PTX and C3’-OHP. There would be herb-drug interaction happening between XAP and PTX in rats.Graphical abstract (Source: Journal of Pharmaceutical and Biomedical Analysis)
Source: Journal of Pharmaceutical and Biomedical Analysis - July 5, 2019 Category: Drugs & Pharmacology Source Type: research

A HILIC-MS/MS assay for the quantification of metformin and sitagliptin in human plasma and urine: A tool for studying drug transporter perturbation
This article describes the development and validation of a HILIC-MS/MS method for the simultaneous quantification of metformin and sitagliptin from human plasma and urine. The presented method uses quick sample preparation and fast chromatography allowing for high sample throughput. The quantification is performed using multi-reaction monitoring and ESI positive mode with stable isotope labelled internal standards for both metformin and sitagliptin. Excellent linearity in the selected calibrations ranges, low inter-day variability (CV%
Source: Journal of Pharmaceutical and Biomedical Analysis - July 5, 2019 Category: Drugs & Pharmacology Source Type: research

Improvement of hair testing for Ethylglucuronide by supported liquid extraction and ultra-high performance liquid chromatography tandem mass spectrometry
Publication date: Available online 3 July 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Sara Malaca, Luisa Mastrobattista, Claudia Mortali, Raffaele Giorgetti, Simona ZaamiAbstractTo improve the reproducibility, suitability and speed of hair testing for Ethylglucuronide (EtG), an ultra-high performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS) method was developed and validated together with a supported liquid extraction (SLE) EtG from the keratin matrix. EtG was analyzed using reversed phase chromatography with gradient elution and detection with tandem mass spectrom...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 5, 2019 Category: Drugs & Pharmacology Source Type: research

Simultaneous quantification and identification of Amaryllidaceae alkaloids in Narcissus tazetta by ultra performance liquid chromatography-diode array detector-electrospray ionisation tandem mass spectrometry
Publication date: Available online 2 July 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Deepali Katoch, Upendra SharmaAbstractNarcissus tazetta is used traditionally for treatment of sores, wounds, skin diseases, cancer in different parts of world. Present study focus on the analysis of amaryllidaceae alkaloids in this plant using an ultra-performance liquid chromatography-diode array detection method. The method was developed for simultaneous quantification of eight Amaryllidaceae alkaloids i.e. pseudolycorine (1), lycorine (2), galanthamine (3), 8-O-demethylhomolycorine (4), N-methylhaemanthidin...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 4, 2019 Category: Drugs & Pharmacology Source Type: research

Simultaneous Separation and Quantitation of Three Phytosterols from the Sweet Potato, and Determination of their Anti-Breast Cancer Activity
Publication date: Available online 2 July 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Pu Jiang, Bing Han, Lingmin Jiang, Yuanfeng Li, Yang Yu, Heshan Xu, Zhaoxing Li, Deqi Zhou, Xiaoxin Jia, Xuegang Li, Xiaoli YeAbstractThe present study provides the method for simultaneous separation and determination of concentration and evaluates anti-breast cancer activity of three phytosterols from the sweet potato (Ipomoea batatas L.): daucosterol linolenate (DLA), daucosterol linoleate (DL), and daucosterol palmitate (DP). A cell viability assay revealed that the three phytosterols had a stronger inhibito...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 4, 2019 Category: Drugs & Pharmacology Source Type: research

Liquid chromatography-tandem mass spectrometry for the simultaneous quantitation of enmetazobactam and cefepime in human plasma
Publication date: Available online 1 July 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): M. Mameli, A. Vezzelli, S. Verze’, S. Biondi, P. Motta, A. Greco, M. Michi, M. BredaAbstractA simple ultra-performance liquid chromatography-tandem mass spectrometry (UPLC–MS/MS) method was developed and validated for the simultaneous analysis enmetazobactam (also known as AAI101) and cefepime in human plasma. Sample preparation was based on protein precipitation with acetonitrile. Separation was performed on Acquity BEH HILIC column (50 mm × 2.1 mm, 1.7 &mic...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 2, 2019 Category: Drugs & Pharmacology Source Type: research

Development and Validation of In-line Near-Infrared Spectroscopy Based Analytical Method for Commercial Production of a Botanical Drug Product
Publication date: Available online 2 July 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Shunnan Zhang, Haoshu Xiong, Lihong Zhou, Wei Ju, Zhexuan Yang, Kaijing Yan, Binjun Yan, Haibin QuAbstractNear-infrared (NIR) spectroscopy is one of the most successful pharmaceutical process analytical tools. For botanical drug products (BDPs), many studies have applied NIR spectroscopy for rapid analysis of botanical raw materials, extracts and formulations. However, the real-time process analysis reported for BDPs was still mainly conducted on lab- or pilot- scale equipment, where some essential conditions o...
Source: Journal of Pharmaceutical and Biomedical Analysis - July 2, 2019 Category: Drugs & Pharmacology Source Type: research