Development and Validation of an LC-MS/MS Method for the Simultaneous Determination of Bedaquiline and Rifabutin in Human Plasma
This article describes the simultaneous determination of bedaquiline fumarate (TMC-207) and rifabutin in human plasma by stable isotope dilution tandem mass spectrometry. The methodology was developed for an investigation of potential drug-drug interactions of the two anti-tuberculosis drugs when given together to healthy human volunteers. Use of the two drugs in combination to treat disease caused by Mycobacterium tuberculosis is contemplated as the bacterium becomes resistant to many currently available drugs. (Source: Journal of Pharmaceutical and Biomedical Analysis)
Source: Journal of Pharmaceutical and Biomedical Analysis - August 18, 2019 Category: Drugs & Pharmacology Source Type: research

A Sensitive and Efficient Method for Simultaneous Profiling of Bile Acids and Fatty Acids by UPLC-MS/MS
Publication date: Available online 15 August 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Ting Hu, Zhuoling An, Chen Shi, Pengfei Li, Lihong LiuAbstractThe carboxyl group is the functional group in both bile acids (BAs) and fatty acids (FAs) (BAFAs). Considering the functional correlation and the structural similarity of these compounds, a sensitive and efficient method was developed here for the first time to simultaneously profile BAFAs based on ultrahigh performance liquid chromatography coupled with tandem mass spectrometry (UPLC-MS/MS). Through optimization of the chromatographic conditions,...
Source: Journal of Pharmaceutical and Biomedical Analysis - August 16, 2019 Category: Drugs & Pharmacology Source Type: research

A novel neutral loss/product ion scan-incorporated integral approach for the untargeted characterization and comparison of the carboxyl-free ginsenosides from Panax ginseng, Panax quinquefolius, and Panax notoginseng
Publication date: Available online 14 August 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Wen-zhi Yang, Xiao-jian Shi, Chang-liang Yao, Yong Huang, Jin-jun Hou, Su-mei Han, Zi-jin Feng, Wen-long Wei, Wan-ying Wu, De-an GuoAbstractDifferentiated composition in precursor ions for different subclasses of ginsenosides in the negative electrospray-ionization mode has been reported, which lays a foundation for the sorted and untargeted identification of ginsenosides. Carboxyl-free ginsenosides simultaneously from Panax ginseng, P. quinquefolius, and P. notoginseng, were comprehensively characterized an...
Source: Journal of Pharmaceutical and Biomedical Analysis - August 15, 2019 Category: Drugs & Pharmacology Source Type: research

Development of an LC-MS/MS method for quantitative analysis of Chlorogenic acid in human plasma and its application to a pharmacokinetic study in Chinese patients with advanced solid tumor
Publication date: Available online 14 August 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Fen Yang, Lin Shen, Chen Zhang, Fu rong Kou, Jing Gao, Yan Li, Guo bing Xu, Ji fang GongAbstractA simple and specific, rapid resolution liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated for determination of chlorogenic acid in human plasma using neochlorogenic acid as the internal standard. Plasma samples were precipitated with methanol and separated on a Zorbax C18 column (50 × 2.1 mm, i.d. 1.8 µm) at a flow rate of 0.4&thins...
Source: Journal of Pharmaceutical and Biomedical Analysis - August 15, 2019 Category: Drugs & Pharmacology Source Type: research

Screening of cathepsin B inhibitors in traditional Chinese medicine by capillary electrophoresis with immobilized enzyme microreactor
Publication date: Available online 13 August 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Baofang Zhang, Zilin ChenAbstractA simple and valid method for rapid screening of cathepsin B inhibitors from traditional Chinese medicines (TCMs) was established by the combination of immobilized enzyme microreactor (IMER) and capillary electrophoresis. Cathepsin B was immobilized on the inner surface of the capillary by glutaraldehyde method. The separation of substrate and product could be finished by baseline within 3 min. The activity of the immobilized cathepsin B remained approximately 90% afte...
Source: Journal of Pharmaceutical and Biomedical Analysis - August 14, 2019 Category: Drugs & Pharmacology Source Type: research

Investigating oral fluid and exhaled breath as alternative matrices for anti-doping testing: analysis of 521 matched samples
Publication date: Available online 12 August 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Geoffrey D. Miller, Ryan M. Van Wagoner, Benjamin B. Bruno, Jacob Husk, Matthew N. Fedoruk, Daniel EichnerAbstractCurrent anti-doping testing is primarily conducted in urine and blood. Recently, due to confounding factors with urine and blood collections such as invasiveness, cost, and stringent shipping conditions, there has been a push for the use of alternative sample matrices to ameliorate these issues. Gaining support within the anti-doping field is the use of oral fluid, and more recently exhaled breat...
Source: Journal of Pharmaceutical and Biomedical Analysis - August 14, 2019 Category: Drugs & Pharmacology Source Type: research

Application of the optimized and validated LC–MS method for simultaneous quantification of tryptophan metabolites in culture medium from cancer cells
Publication date: 30 November 2019Source: Journal of Pharmaceutical and Biomedical Analysis, Volume 176Author(s): Ilona Sadok, Kamila Rachwał, Magdalena StaniszewskaAbstractKynurenine pathway is the main route of tryptophan degradation generating a number of immunoregulatory compounds. Some conditions like oxidative stress, inflammatory factors might enhance tryptophan degradation. Process is active in several cells including fibroblasts, cancer cells, and immune cells, therefore it is intensively studied in context of cancer microenvironment. The validated and standardized methodology for kynurenine quantification is cru...
Source: Journal of Pharmaceutical and Biomedical Analysis - August 14, 2019 Category: Drugs & Pharmacology Source Type: research

Enantioselective separation of eight antihistamines with α1-acid glycoprotein-based chiral stationary phase by HPLC: Development and validation for the enantiomeric quality control
Publication date: Available online 10 August 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Bolin Zhu, Mengyao Xue, Beibei Liu, Qing Li, Xingjie GuoAbstractIn the present paper, a sensitive and selective chiral LC method has been developed for enantiomeric separation and determination of eight antihistamines in pharmaceutical formulations. Enantiomeric separation was achieved on the α1-acid glycoprotein-based chiral stationary phase known as Chiralpak AGP. The effects of the mobile phase composition, type and proportion of organic modifier and the concentration and pH of the buffer on retenti...
Source: Journal of Pharmaceutical and Biomedical Analysis - August 11, 2019 Category: Drugs & Pharmacology Source Type: research

Part 2: Physicochemical characterization of bevacizumab in 2 mg/mL antibody solutions as used in human i.v. administration: comparison of originator with a biosimilar candidate
Publication date: Available online 10 August 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Tudor Arvinte, Caroline Palais, Emilie Poirier, Amelia Cudd, Shanthi Rajendran, Stephen Brokx, Jason DowdAbstractThe physicochemical properties of Avastin® manufactured in the USA (Originator USA) and in Europe (Originator EU) and ABX-BEV, a bevacizumab biosimilar drug product candidate produced by Apobiologix Inc., were characterized at a clinically relevant concentration of 2 mg/mL following dilution of the 25 mg/mL drug products with 0.9% NaCl. Measurements using 14 orthogonal analytical...
Source: Journal of Pharmaceutical and Biomedical Analysis - August 11, 2019 Category: Drugs & Pharmacology Source Type: research

Separation and characterization of forced degradation products in homoharringtonine injection by UHPLC-Q-TOF-MS
Publication date: Available online 10 August 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Xiao Gu, Yue Chen, Yongjun Lou, Jinqi ZhengAbstractA rapid ultrahigh-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (UHPLC-Q-TOF-MS) method was developed for separation and characterization of the degradation products in HHT injection. Chromatographic separation was achieved on a ZORBAX Eclipse XDB-C18 HD column (2.1 × 100 mm, 1.8μm) using methanol- ammonium formate (pH 3.0; 30 mM) (30:70, v/v) as mobile phase in an isocratic mode of elution. Forced degrad...
Source: Journal of Pharmaceutical and Biomedical Analysis - August 11, 2019 Category: Drugs & Pharmacology Source Type: research

Subminute micro-isolation of pharmaceuticals with ultra-high pressure liquid chromatography
In this study we describe the isolation of small molecule and biomolecule crude mixtures at the microgram-scale (100 – 2500 µg) in single or library format with methods as fast as 1.0 min and system pressures averaging 10000 psi with an ultra-high pressure liquid chromatography (UHPLC) setup. UHPLC technology provides several advantages for rapid (
Source: Journal of Pharmaceutical and Biomedical Analysis - August 9, 2019 Category: Drugs & Pharmacology Source Type: research

LC-MS/MS combined with in vivo microdialysis sampling from conscious rat striatum for simultaneous determination of active constituents of Yuanhu- Baizhi herb pair and endogenous neurotransmitters: application to pharmacokinetic and pharmacodynamic study
In conclusion, the pharmacokinetic and pharmacodynamic study based on in vivo microdialysis sampling from awaken animals and LC-MS/MS quantitation is in favor of revealing the compatibility mechanism of herb pairs. (Source: Journal of Pharmaceutical and Biomedical Analysis)
Source: Journal of Pharmaceutical and Biomedical Analysis - August 8, 2019 Category: Drugs & Pharmacology Source Type: research

Chemical profliling of Dingkun Dan by Ultra High Performance Liquid Chromatography Q Exactive Orbitrap High Resolution Mass Spectrometry
Publication date: Available online 6 July 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Xiaoxia Gao, Nan Wang, Jinping Jia, Peiyi Wang, Airong Zhang, Xuemei QinAbstractDingkun Dan (DKD) has been widely used for a variety of gynecological disease. However, the systematic analysis of the chemical constituents of DKD has not been well established because of the complexity of the formula and confidentiality. In this paper, liquid chromatography Q Exactive high resolution accurate mass spectrometry (UHPLC-QE-HRMS) with automated MetaboLynx analysis was established to characterize the chemical constitue...
Source: Journal of Pharmaceutical and Biomedical Analysis - August 6, 2019 Category: Drugs & Pharmacology Source Type: research

Fabrication of carbon nanotube-polylactic acid composite electrode by melt compounding for capillary electrophoretic determination of tectoridin and irigenin in Belamcandae Rhizoma
Publication date: Available online 10 July 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Hua Mao, Xinming Ye, Weilong Chen, Wenye Geng, Gang ChenAbstractA sensitive detection electrode based on the composite of carbon nanotubes (CNTs) and polylactic acid (PLA) was fabricated for measuring the bioactive constituents in Belamcandae Rhizoma by capillary electrophoresis (CE). The composite was facilely fabricated by packing a blend of CNTs and melted PLA into a fused silica capillary under heat. The prepared CNT-PLA composite was characterized by scanning electron microscopy, Raman spectroscopy, Fouri...
Source: Journal of Pharmaceutical and Biomedical Analysis - August 6, 2019 Category: Drugs & Pharmacology Source Type: research

Optimization of an in vitro gut microbiome biotransformation platform with chlorogenic acid as model compound: from fecal sample to biotransformation product identification
This study optimized a ready-to-use platform to investigate colonic biotransformation of xenobiotics by using chlorogenic acid as a model compound. This platform can be used in the future to study differences in colonic biotransformation of xenobiotics using fecal samples of different patient groups.Graphical abstract (Source: Journal of Pharmaceutical and Biomedical Analysis)
Source: Journal of Pharmaceutical and Biomedical Analysis - August 6, 2019 Category: Drugs & Pharmacology Source Type: research

Novel “Matrix-Corrected Calibration” study for the detection of polyunsaturated fatty acids (PUFAs) in plasma and erythrocytes by means of a gas chromatography-mass spectrometry approach optimized to follow up long-term parental patients
Publication date: Available online 24 July 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Eugenio Alladio, Alessandra MancaGraphical abstract (Source: Journal of Pharmaceutical and Biomedical Analysis)
Source: Journal of Pharmaceutical and Biomedical Analysis - August 6, 2019 Category: Drugs & Pharmacology Source Type: research

Electrochemical behaviour of anticancer drug lomustine and in situ evaluation of its interaction with DNA
Publication date: Available online 25 July 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Paulina Andréa V. de Carvalho, Ilanna Campelo Lopes, Elizaura Hyeda C. Silva, Evellin Enny S. Bruzaca, Hugo José Chaves, Mayara Ingrid S. Lima, Auro Atsushi TanakaAbstractElectrochemical techniques were used to investigate the behavior of lomustine (CCNU) and its degradation in aqueous solution at a glassy carbon electrode (GCE). The in situ interaction of CCNU and chemically degraded CCNU (cdCCNU) with dsDNA was then investigated in dsDNA incubated solutions, using dsDNA electrochemical biosenso...
Source: Journal of Pharmaceutical and Biomedical Analysis - August 6, 2019 Category: Drugs & Pharmacology Source Type: research

Human Gastrointestinal Metabolism of the Anti-rheumatic Fraction of Dianbaizhu (Gaultheria leucocarpa var. yunnanensis) in Vitro: Elucidation of the Metabolic Analysis in Gastric Juice, Intestinal Juice and Human Intestinal Bacteria by UPLC-LTQ-Orbitrap-MSn and HPLC-DAD
Publication date: Available online 26 July 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Xiuhuan Wang, Xiao Li, Rufeng Wang, Le Wang, Shusheng Fan, Xiaoping Wang, Xiao Xu, Xin Yan, Ting He, Xueyang Ren, Gaimei SheAbstractThe anti-rheumatic fraction (ARF), is responsible for the anti-inflammatory and analgesic effects of Dianbaizhu derived from the aerial part of Gaultheria leucocarpa var. yunnanensis (Ericaceae). The gastrointestinal metabolism of ARF was investigated in vitro through simulating a series of models–gastric juice, intestinal juice, and human intestinal bacteria, analyzed by HP...
Source: Journal of Pharmaceutical and Biomedical Analysis - August 6, 2019 Category: Drugs & Pharmacology Source Type: research

Acetone immersion enhanced MALDI-MS imaging of small molecule metabolites in biological tissues
Publication date: Available online 1 August 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Chenglong Sun, Zhichao Li, Chunxia Ma, Qingce Zang, Jiangshuo Li, Wei Liu, Hengqiang Zhao, Xiao WangABSTRACTProfiling the endogenous tissue metabolites with spatial features is significant for our understanding of molecular histology, and provides an insightful way to uncover the complex associations between tissue metabolic response and external stimuli. Matrix-assisted laser desorption/ionization mass spectrometry imaging (MALDI-MSI) is an effective molecular imaging technology to illustrate the spatial loc...
Source: Journal of Pharmaceutical and Biomedical Analysis - August 6, 2019 Category: Drugs & Pharmacology Source Type: research

Multi-platform metabonomics unravel amino acids as markers of HIV/combination antiretroviral therapy-induced oxidative stress
Publication date: Available online 2 August 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Lungile J. Sitole, Fidele Tugizimana, Debra MeyerAbstractInfection by the human immunodeficiency virus (HIV) elicits an immune response wherein neutrophils produce reactive oxygen species (ROS) to defend against pathogen invasion. Consequently, disproportionate levels of ROS in relation to antioxidants lead to oxidative stress (OS), which plays a key role in HIV disease progression and pathogenesis. There is a close relationship between oxidative stress status and HIV infection/progression, both separately an...
Source: Journal of Pharmaceutical and Biomedical Analysis - August 6, 2019 Category: Drugs & Pharmacology Source Type: research

Effective Extraction with Deep Eutectic Solvents and Enrichment by Macroporous Adsorption Resin of Flavonoids from Carthamus tinctorius L.
In conclusion, the developed DES2-UAE combined with macroporous resin enrichment can be an alternative method for the green and efficient extraction of bioactive flavonoids from plant materials. (Source: Journal of Pharmaceutical and Biomedical Analysis)
Source: Journal of Pharmaceutical and Biomedical Analysis - August 6, 2019 Category: Drugs & Pharmacology Source Type: research

Application of the optimized and validated LC-MS method for simultaneous quantification of tryptophan metabolites in culture medium from cancer cells
Publication date: Available online 6 August 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Ilona Sadok, Kamila Rachwał, Magdalena StaniszewskaAbstractKynurenine pathway is the main route of tryptophan degradation generating a number of immunoregulatory compounds. Some conditions like oxidative stress, inflammatory factors might enhance tryptophan degradation. Process is active in several cells including fibroblasts, cancer cells, and immune cells, therefore it is intensively studied in context of cancer microenvironment. The validated and standardized methodology for kynurenine quantification is c...
Source: Journal of Pharmaceutical and Biomedical Analysis - August 6, 2019 Category: Drugs & Pharmacology Source Type: research

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