High-performance thin-layer chromatography linked with (bio)assays and FTIR-ATR spectroscopy as a method for discovery and quantification of bioactive components in native Australian plants
Publication date: Available online 24 February 2020Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Snezana Agatonovic-Kustrin, Ethan Doyle, Vladimir Gegechkori, David W. Morton (Source: Journal of Pharmaceutical and Biomedical Analysis)
Source: Journal of Pharmaceutical and Biomedical Analysis - February 25, 2020 Category: Drugs & Pharmacology Source Type: research

Frequentist approach for estimation of false decision risks in conformity assessment based on measurement uncertainty of liquid chromatography analytical procedures
Publication date: Available online 25 February 2020Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Luciana Separovic, Felipe Rebello Lourenço (Source: Journal of Pharmaceutical and Biomedical Analysis)
Source: Journal of Pharmaceutical and Biomedical Analysis - February 25, 2020 Category: Drugs & Pharmacology Source Type: research

1H HR-MAS NMR and chemometric methods for discrimination and classification of Baccharis (Asteraceae): A proposal for quality control of Baccharis trimera
Publication date: Available online 24 February 2020Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Livia Macedo Dutra, Alan Diego da Conceição Santos, Allan Vinicius Felix Lourenço, Noemi Nagata, Gustavo Heiden, Francinete Ramos Campos, Andersson BarisonAbstractBaccharis trimera is a species recognized by health agencies and recommended by the Brazilian Pharmacopoeia by having medicinal properties. In this work, HR-MAS NMR spectroscopy combined with chemometric tools, such as Principal Components Analysis (PCA), Partial Least Squares Discriminant Analysis (PLS-DA) and Soft Independe...
Source: Journal of Pharmaceutical and Biomedical Analysis - February 24, 2020 Category: Drugs & Pharmacology Source Type: research

Editorial for the special issue titled “Biopharmaceuticals 2020”
Publication date: Available online 22 February 2020Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Szabolcs Fekete, Davy Guillarme (Source: Journal of Pharmaceutical and Biomedical Analysis)
Source: Journal of Pharmaceutical and Biomedical Analysis - February 24, 2020 Category: Drugs & Pharmacology Source Type: research

Proteomic serum profile in menstrual-related and post menopause migraine
In conclusion, proteomic analysis was able to reveal differences in protein expression between migraine sufferers and non-headache women; as in other neurological diseases characterized by neuroinflammation, the serum proteome of migraine women presents an abundance of proteins indicative of cellular damage, oxidative stress and inflammation. This relevant inflammatory status, if confirmed in larger series, could represent a target for menstrual-related migraine treatment.Graphical abstract (Source: Journal of Pharmaceutical and Biomedical Analysis)
Source: Journal of Pharmaceutical and Biomedical Analysis - February 22, 2020 Category: Drugs & Pharmacology Source Type: research

Evaluation of a sensitive GC–MS method to detect polysorbate 80 in vaccine preparation
Publication date: Available online 23 January 2020Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Niraj Shende, Abhijeet Karale, Sudhakar Bhagade, Ashishkumar Gulhane, Prashant Bore, Preeti Marathe, Sourish Chakraborty, Asha D. Mallya, Rajeev M. DhereAbstractPolysorbates are the most versatile and common surfactants used as protein stabilizers. Analysis of residual polysorbate 80 (PS 80) in conjugate vaccine is challenging due to complexity of conjugate matrices and heterogeneity of the structure of the PS 80 analyte. The direct approach using high-performance liquid chromatography-evaporative light sca...
Source: Journal of Pharmaceutical and Biomedical Analysis - February 22, 2020 Category: Drugs & Pharmacology Source Type: research

Investigation of the chemical compounds in Pheretima aspergillum (E. Perrier) using a combination of mass spectral molecular networking and unsupervised substructure annotation topic modeling together with in silico fragmentation prediction
Publication date: Available online 20 February 2020Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Tao-Fang Cheng, Yu-Hao Zhang, Ji Ye, Hui-Zi Jin, Wei-Dong ZhangAbstractUntargeted mass spectrometry analysis is one of the most challenging and meaningful steps in the rapid structural elucidation of the highly complex and diverse constituents of traditional Chinese medicine. Specifically, it is a laborious and time-consuming way to identify unknown compounds. Herein, a workflow was proposed to expedite the annotations of the chemical structures in Pheretima aspergillum (E. Perrier) (Di-Long, DL). First, u...
Source: Journal of Pharmaceutical and Biomedical Analysis - February 22, 2020 Category: Drugs & Pharmacology Source Type: research

Characterization of two unknown impurities in roxithromycin by 2D LC–QTOF/MS/MS and NMR
Publication date: Available online 20 February 2020Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Jian Wang, Jinjin Zhou, Yu Xu, Bingqi Zhu, Yong JinAbstractTwo unknown impurities in roxithromycin were discovered and preliminarily characterized by two-dimensional liquid chromatography coupled with QTOF mass analyzer (2D LC–QTOF MS/MS). The column-switching technique of 2D LC made the chromatographic conditions in official standard of roxithromycin compatible with mass spectrometric detector. The complete MS/MS fragmentation patterns of the impurities were studied to obtain structural information ...
Source: Journal of Pharmaceutical and Biomedical Analysis - February 22, 2020 Category: Drugs & Pharmacology Source Type: research

Covalent immobilization of trypsin on polyvinyl alcohol-coated magnetic nanoparticles activated with glutaraldehyde
Publication date: Available online 20 February 2020Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Selmihan Sahin, Ismail OzmenAbstractMagnetic nanoparticles were coated with polyvinyl alcohol and activated with glutaraldehyde for trypsin immobilization. The prepared magnetic nanoparticles were characterized by transmission electron microscopy, fourier transform infrared spectroscopy, thermal gravimetric analysis, zeta potential meter and vibrating sample magnetometer. Free and immobilized trypsin showed optimum activity at pH 6.0, 30 °C and pH 7.0, 40 °C, respectively. Immobilized...
Source: Journal of Pharmaceutical and Biomedical Analysis - February 22, 2020 Category: Drugs & Pharmacology Source Type: research

Quantitation of serum pregnanediol-3-glucuronide level in different endocrine statuses by LC–MS/MS
In this study, a highly sensitive and accurate LC–MS/MS method was firstly established for subsequent measurement of PdG in serum of three different female groups: thyroid cancer patients (TCs), healthy controls (HCs) and pregnant women. The factors affecting the sample preparation, MS/MS method, gradient elution program, selection of chromatographic column and internal standard (IS) have been optimized in this study. Compared with enzyme immunoassay (EIA) method, we used LC–MS/MS to shorten analysis time, increase sensitivity, raise specificity, simplify sample preparation, and reduce costs. As a result, the l...
Source: Journal of Pharmaceutical and Biomedical Analysis - February 22, 2020 Category: Drugs & Pharmacology Source Type: research

Optimization of a High-Throughput Fluorescence Polarization Assay for STAT5B DNA Binding Domain-Targeting Inhibitors
Publication date: Available online 19 February 2020Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Pimyupa Manaswiyoungkul, Fettah Erdogan, Olasunkanmi O. Olaoye, Aaron D. Cabral, Elvin D. de Araujo, Patrick T. GunningAbstractSignal transducer and activator of transcription 5B (STAT5B) is constitutively activated in multiple cancers as a result of hyperactivating mutations or dysregulation of upstream effectors. Therapeutic strategies have predominantly targeted the Src homology 2 (SH2) domain to inhibit STAT phosphorylation, a prerequisite for STAT5B transcriptional activation. An alternative approach ...
Source: Journal of Pharmaceutical and Biomedical Analysis - February 20, 2020 Category: Drugs & Pharmacology Source Type: research

Study of chromatographic behavior of antibiotic drugs and their metabolites based on quantitative structure-retention relationships with the use of HPLC-DAD
Publication date: Available online 19 February 2020Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Justyna Walczak, Małgorzata Szultka-Młyńska, Katarzyna Pauter, Bogusław BuszewskiAbstractThe separation of eleven antibiotics and ten metabolites were studied using high performance liquid chromatography. The C18-PFP octadecyl with integral PFP, C18-AR octadecyl with integral phenyl, C18-HL octadecyl and phenyl phase were used as stationary phases. Mixtures of acetontrile–0.1% formic acid in water were investigated as mobile phases. The elution order of the target compounds was similar for all fo...
Source: Journal of Pharmaceutical and Biomedical Analysis - February 20, 2020 Category: Drugs & Pharmacology Source Type: research

The chemical transformations for Radix Astragali via different alkaline wash conditions by quantitative and qualitative analyses
In conclusion, this work would provide a scientific and practical method for quality control of Radix Astragali as well as its compound preparations.Graphical abstract (Source: Journal of Pharmaceutical and Biomedical Analysis)
Source: Journal of Pharmaceutical and Biomedical Analysis - February 20, 2020 Category: Drugs & Pharmacology Source Type: research

Comprehensive chemotaxonomic analysis of saffron crocus tepal and stamen samples, as raw materials with potential antidepressant activity
Publication date: Available online 18 February 2020Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Javad Mottaghipisheh, Mohammad Mahmoodi Sourestani, Tivadar Kiss, Attila Horváth, Barbara Tóth, Mehdi Ayanmanesh, Amin Khamushi, Dezso CsuporAbstractSaffron crocus (Crocus sativus L.) has been widely grown in Iran. Its stigma is considered as the most valuable spice for which several pharmacological activities have been reported in preclinical and clinical studies, the antidepressant effect being the most thoroughly studied and confirmed. This plant part contains several characteristic second...
Source: Journal of Pharmaceutical and Biomedical Analysis - February 19, 2020 Category: Drugs & Pharmacology Source Type: research

Investigating the molecular structure of placenta and plasma in pre-eclampsia by infrared microspectroscopy
In this study, IR microspectroscopy was applied to identify molecular changes associated with the pathogenesis of PE in placental tissues and plasma samples from pre-eclamptic women and normotensive matched controls. The obtained spectra were analyzed by multivariate analysis in the spectral ranges of 3050–2800 cm−1 and 1855–1485 cm−1 corresponding to lipid and protein-carbonyl components, respectively. In the lipid region, an increase in CH2/CH3 ratio was noticed and higher level of unsaturation index in placenta was evident. New lipid species emerged as a consequence of oxidative str...
Source: Journal of Pharmaceutical and Biomedical Analysis - February 19, 2020 Category: Drugs & Pharmacology Source Type: research

Quantitative analysis of 3’- and 6’- sialyllactose in human milk samples by HPLC-MS/MS: a validated method for the comparison of two consecutive lactation periods in the same woman
Publication date: Available online 19 February 2020Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Orsolya Csernák, Barbara Rácz, Ágnes Alberti, Szabolcs BéniAbstractHuman milk oligosaccharides (HMOs) are complex carbohydrates that exist naturally in mother’s milk. Due to their myriad beneficial biological effects, HMOs are in the focus of current researches. Some of these complex carbohydrates are already commercially available utilizing their health-promoting benefits not just in infant formula but in dietary supplements. Among the acidic oligosaccharides 3’- an...
Source: Journal of Pharmaceutical and Biomedical Analysis - February 19, 2020 Category: Drugs & Pharmacology Source Type: research

Validation of an Assay for Quantifying Ganciclovir in Dried Blood Spots
We describe a simple method for determining systemic GCV concentrations using dried blood spot (DBS) samples. GCV was extracted from a single 6 mm punch via sonication in methanol, then quantified using liquid chromatography-tandem mass spectrometry. The assay was accurate and precise in the dynamic range of 10 to 10,000 ng/mL. GCV concentrations determined in DBS agreed well with GCV concentrations observed in serum. The assay was successfully applied to patient samples, and will be used to support pharmacokinetic studies in an ongoing clinical trial of VGC in infants with CMV-mediated hearing loss. (Source:...
Source: Journal of Pharmaceutical and Biomedical Analysis - February 18, 2020 Category: Drugs & Pharmacology Source Type: research

Development of an ICP-MS/MS approach for absolute quantification and determination of phosphodiester to phosphorothioate ratio in therapeutic oligonucleotides
Publication date: Available online 15 February 2020Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Juliusz Bianga, Magali Perez, Damien Mouvet, Caroline Cajot, Philippe De Raeve, Arnaud DelobelAbstractA new analytical method based on ICP-MS/MS is proposed for the characterization of synthetic phosphorothioate oligonucleotides. Absolute quantification of oligonucleotides is challenging, as well as the determination of phosphodiester to phosphorothioate ratio for phosphorothioate oligonucleotides. Both are considered as critical quality attributes and should be determined using robust validated methods. T...
Source: Journal of Pharmaceutical and Biomedical Analysis - February 16, 2020 Category: Drugs & Pharmacology Source Type: research

Magnetic solid phase extraction followed with LC-MS/MS for determination of glimepiride in beagle dog plasma and its application to bioequivalence study
In this study, the core-shell polydopamine-coated magnetic nanomaterials were synthesized with one-step approach and applied as magnetic solid phase extraction adsorbents combined with LC-MS/MS for quantification of the diabetes drug glimepiride in beagle dog plasma. The Fe3O4@PDA nanomaterials have strong magnetic response, good dispersibility in aqueous solution, and numerous binding sites for π–π interaction and hydrogen bonding with glimepiride. Based on these merits, glimepiride could be quickly extracted and separated from plasma within 10min. The established method has good linearity (1-2000ng•mL-1)...
Source: Journal of Pharmaceutical and Biomedical Analysis - February 16, 2020 Category: Drugs & Pharmacology Source Type: research

UPLC-MS identification and anticomplement activity of the metabolites of Sophora tonkinensis flavonoids treated with human intestinal bacteria
Publication date: Available online 14 February 2020Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Xin Jin, Yan Lu, Shaoxin Chen, Daofeng ChenAbstractAnticomplement activity played an important role in anti-inflammatory effects of traditional Chinese herbs. The total flavonoids of Sophora tonkinensis (TFST) were inactive on the complement system but showed obvious anticomplement activity after incubated with human intestinal bacteria in vitro. In order to discover the metabolic activation of TFST by intestinal flora, the constituents of TFST and its metabolites were identified by UPLC-ESI-LTQ/MS. Their ...
Source: Journal of Pharmaceutical and Biomedical Analysis - February 15, 2020 Category: Drugs & Pharmacology Source Type: research

Metabolomic approach for rapid differentiation of Fritillaria bulbs by matrix-assisted laser desorption/ionization mass spectrometry and multivariate statistical analysis
Publication date: Available online 14 February 2020Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Ze Wang, Hanyi Xie, Juan Ren, Yang Chen, Xiaofei Li, Xiangfeng Chen, Tak-Wah Dominic ChanAbstractThe bulbs of Fritillaria have been used for centuries as food and medicinal products in many Asian countries. Different Fritillaria species have distinct pharmacological effects despite of their similar appearances. Effective differentiation of Fritillaria species can avoid adulteration and is crucial to its clinical uses. In this paper, a hybrid method of matrix assisted laser desorption/ionization mass spectr...
Source: Journal of Pharmaceutical and Biomedical Analysis - February 15, 2020 Category: Drugs & Pharmacology Source Type: research

Bridging Size and Charge Variants of a Therapeutic Monoclonal Antibody by Two-Dimensional Liquid Chromatography
Publication date: Available online 14 February 2020Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Zhi Chen, Ming Zeng, Sung-Joo Park, Gurusamy Balakrishnan, Kaimeng Zhou, Duohai Pan, Tapan K.AbstractMonoclonal antibodies are heterogeneous in nature and may contain numerous variants with differences in size, charge, and hydrophobicity, which may impact clinical efficacy, immunogenicity, and safety. Characterization of antibody variants is necessary to build structure-function correlation and establish a proper control strategy. Isolation and enrichment of variants by conventional chromatographic peak fr...
Source: Journal of Pharmaceutical and Biomedical Analysis - February 15, 2020 Category: Drugs & Pharmacology Source Type: research

Inside gel electromembrane extraction: A novel green methodology for the extraction of morphine and codeine from human biological fluids
Publication date: Available online 14 February 2020Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Atyeh Rahimi, Saeed Nojavan, Hadi TabaniAbstractIn this work, a new mode of gel-electromembrane extraction (G-EME), called “inside” gel-EME (IG-EME) is proposed for the extraction of morphine and codeine as model basic drugs from complex biological samples. Here, an aqueous media that was captured inside the agarose gel membrane, acted as both gel membrane and the acceptor phase (AP) at the same time. In this regard, the membrane served as the separation filter (membrane) and supported liquid a...
Source: Journal of Pharmaceutical and Biomedical Analysis - February 15, 2020 Category: Drugs & Pharmacology Source Type: research

Fast simultaneous quantification of gabapentin and cetirizine in cell lysates by means of HPLC-MS/MS
Publication date: Available online 13 February 2020Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Lukas Schlatt, Ana Carolina Conchon Costa, Vivien Barz, Giuliano Ciarimboli, Uwe KarstAbstractA high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was successfully developed for the simultaneous detection of gabapentin (GBP) and cetirizine (CTZ) in cell lysates. Multiple reaction monitoring (MRM) transitions were found for GBP, CTZ and deuterated internal standards of both, allowing a selective and sensitive detection. Limits of detection (LODs) of 0.04 ng/mL and 0.0...
Source: Journal of Pharmaceutical and Biomedical Analysis - February 15, 2020 Category: Drugs & Pharmacology Source Type: research

Conventional and nonconventional extraction techniques for optimal extraction processes of rosmarinic acid from six Lamiaceae plants as determined by HPLC-DAD measurement
Publication date: Available online 13 February 2020Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Beatrix Sik, Erika Lakatos Hanczné, Viktória Kapcsándi, Zsolt AjtonyAbstractThe goal of this study was to improve the extraction efficiency of rosmarinic acid (RA) from Lamiaceae herbs (lemon balm, peppermint, oregano, rosemary, sage, and thyme) using various extraction techniques (maceration with stirring, MACS; heat reflux, HRE; and microwave-assisted extraction, MAE) and extraction conditions (solvent acidity, solvent type, extraction time and temperature). The RA content was measur...
Source: Journal of Pharmaceutical and Biomedical Analysis - February 15, 2020 Category: Drugs & Pharmacology Source Type: research

Corrigendum to “LC–MS/MS method for the simultaneous analysis of seven antimalarials and two active metabolites in dried blood spots for applications in field trials: Analytical and clinical validation” [J. Pharm. Biomed. Anal. 154 (2018) 263–277]
Publication date: Available online 13 February 2020Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Joanna Gallay, Sylvain Prod’hom, Thomas Mercier, Carine Bardinet, Dany Spaggiari, Emilie Pothin, Thierry Buclin, Blaise Genton, Laurent Arthur Decosterd (Source: Journal of Pharmaceutical and Biomedical Analysis)
Source: Journal of Pharmaceutical and Biomedical Analysis - February 15, 2020 Category: Drugs & Pharmacology Source Type: research

Mass spectrometry-based methods in characterization of the higher order structure of protein therapeutics
Publication date: Available online 12 February 2020Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Igor A. Kaltashov, Cedric E. Bobst, Jake Pawlowski, Guanbo WangAbstractHigher order structure of protein therapeutics is an important quality attribute, which dictates both potency and safety. While modern experimental biophysics offers an impressive arsenal of state-of-the-art tools that can be used for the characterization of higher order structure, many of them are poorly suited for the characterization of biopharmaceutical products. As a result, these analyses were traditionally carried out using class...
Source: Journal of Pharmaceutical and Biomedical Analysis - February 13, 2020 Category: Drugs & Pharmacology Source Type: research

Universal quantification method of degradation impurities in 16-membered macrolides using HPLC-CAD and study on source of the impurities
In this study, a reliable method was established for the analysis of impurities in 16-membered macrolides for the first time by high performance liquid chromatography tandem with charged aerosol detector (HPLC-CAD). The chromatographic conditions and CAD parameters were optimized for a good separation and sensitivity. The impurities were identified by ion trap time-of-flight mass spectrometry (IT-TOF/MS), the developed method was validated, and the sources of degradation impurities in production were investigated. Based on the experimental results, the superiority of the developed method over UV detection was demonstrated ...
Source: Journal of Pharmaceutical and Biomedical Analysis - February 13, 2020 Category: Drugs & Pharmacology Source Type: research

Quantitation of serum pregnanediol-3-glucuronide level in different endocrine statuses by LC-MS/MS
In this study, a highly sensitive and accurate LC-MS/MS method was firstly established for subsequent measurement of PdG in serum of three different female groups: thyroid cancer patients (TCs), healthy controls (HCs) and pregnant women. The factors affecting the sample preparation, MS/MS method, gradient elution program, selection of chromatographic column and internal standard (IS) have been optimized in this study. Compared with enzyme immunoassay (EIA) method, we used LC-MS/MS to shorten analysis time, increase sensitivity, raise specificity, simplify sample preparation, and reduce costs. As a result, the linear range ...
Source: Journal of Pharmaceutical and Biomedical Analysis - February 13, 2020 Category: Drugs & Pharmacology Source Type: research

Sensitive and selective quantification of mid-regional proadrenomedullin in human plasma using ultra-performance liquid chromatography coupled with tandem mass spectrometry
Publication date: Available online 11 February 2020Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Motoshi Iwao, Yosuke Suzuki, Ryota Tanaka, Teruhide Koyama, Etsuko Ozaki, Takeshi Nakata, Kohei Aoki, Akihiro Fukuda, Yuhki Sato, Nagato Kuriyama, Naoya Fukunaga, Fuminori Sato, Fumihiko Katagiri, Keiko Ohno, Hirotaka Shibata, Hiromitsu Mimata, Hiroki ItohAbstractMid-regional pro-adrenomedullin (MR-proADM) is suggested to be a prognostic indicator for various diseases. Plasma MR-proADM concentration is commonly measured using immunoassays based on its immunochemical characteristics. However, some immunolog...
Source: Journal of Pharmaceutical and Biomedical Analysis - February 12, 2020 Category: Drugs & Pharmacology Source Type: research

Determination of size variants by CE-SDS for approved therapeutic antibodies: key implications of subclasses and light chain specificities
Publication date: Available online 10 February 2020Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Elsa Wagner, Olivier Colas, Stéphane Chenu, Alexandre Goyon, Amarande Murisier, Sarah Cianferani, Yannis François, Szabolcs Fekete, Davy Guillarme, Valentina D’Atri, Alain BeckAbstractIn the present work, a generic non-reducing capillary electrophoresis sodium dodecyl sulphate (nrCE-SDS) method was tested for a wide range of 26 FDA and EMA approved monoclonal antibodies (mAbs) and 2 antibody drug conjugates (ADCs) as well as for the NISTmab, in a QC environment (e.g. testing quality req...
Source: Journal of Pharmaceutical and Biomedical Analysis - February 12, 2020 Category: Drugs & Pharmacology Source Type: research

Finding a reliable limit of detection in the NIR determination of residual moisture in a freeze-dried drug product
Publication date: Available online 11 February 2020Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Gloria Clua-Palau, Enric Jo, Sasha Nikolic, Jordi Coello, Santiago MaspochAbstractThe validation of an analytical method in the pharmaceutical industry follows strictly regulated guidelines. The introduction of multivariable calibration methods requires a revision of these recommendations, since some of them are contradictory regarding the limit of detection (LOD). This work compares the LOD values obtained using pseudounivariate and multivariate procedures in the PLS-NIR determination of residual moisture...
Source: Journal of Pharmaceutical and Biomedical Analysis - February 12, 2020 Category: Drugs & Pharmacology Source Type: research

An effective method for the determination of the enantio-purity of L-α-glycerophosphocholine (L-α-GPC)
Publication date: Available online 8 February 2020Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Lorenzo de Ferra, Antonio Massa, Antonia Di Mola, Bernd DiehlAbstractHerein we describe for the first time a practical analytical method for determining the enantio-purity of L-α-glycerophosphocholine (L-α-GPC) by chiral derivatization. The use of a suitable chiral boronic acid allowed the formation of a mixture of two diastereomeric boronate esters whose ratio, carefully analyzed by 1HNMR spectroscopy, reflects L-α-GPC enantiomeric excesses. The determination of the enantiopurity of L-&al...
Source: Journal of Pharmaceutical and Biomedical Analysis - February 9, 2020 Category: Drugs & Pharmacology Source Type: research

Kinetics and Thermodynamics Evaluation of Oxidative Stability in Oleum hyperici: A comparative Study
In this study, Oleum hyperici (St. John's Wort oil) was investigated according to its oxidative stability and antioxidant activity parameters. A homemade and two different brands of oils were used for comparative reasons. Oxidation process regarding kinetics and thermodynamics studies achieved by accelerated Rancimat conditions (100-140 °C). The quality parameters of the oil samples were compared depending on phenolic and flavonoid contents, antioxidant activity, free fatty acid quantity and shelf-life. Principal component analysis (PCA) has been also applied to comprehend the relationship between these three gr...
Source: Journal of Pharmaceutical and Biomedical Analysis - February 9, 2020 Category: Drugs & Pharmacology Source Type: research

Preface
Publication date: Available online 8 February 2020Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Coral Barbas, Bezhan Chankvetadze, Sandra Furlanetto, Markus Ganzera, Jun Haginaka, Shaoping Li, Ruin Moaddel, Sibel Ozkan, Jean-Luc Veuthey (Source: Journal of Pharmaceutical and Biomedical Analysis)
Source: Journal of Pharmaceutical and Biomedical Analysis - February 9, 2020 Category: Drugs & Pharmacology Source Type: research

Tissue distribution of 35S-metabolically labeled neublastin (BG00010) in rats
Publication date: Available online 6 February 2020Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Natalia Penner, Shobha Purushothama, Blake PepinskyAbstractNeublastin (NBN) is a neurotrophic growth factor that promotes the survival and regenerative properties of nociceptive neurons and has been tested in clinical trials as a treatment for neuropathic pain in individuals with sciatica and painful lumbosacral radiculopathy. Like many low molecular weight heparin binding proteins, NBN is rapidly cleared from the blood following systemic administration. To explore ADME properties of NBN in rats, we used me...
Source: Journal of Pharmaceutical and Biomedical Analysis - February 7, 2020 Category: Drugs & Pharmacology Source Type: research

Large scale consumption monitoring of benzodiazepines and z-drugs by hair analysis
The objective of the present study was to retrospectively evaluate BDZ/z-drug levels in hair for better interpretation of hair testing results. For this purpose, 4,630 authentic samples (head/body hair) from a heterogeneous cohort in Switzerland tested for the presence of 20 BDZ/BDZ metabolites and three z-drugs by liquid chromatography-tandem mass spectrometry were included. Drug concentrations in hair were statistically evaluated by box-plots in 1,726 positive samples. Further, metabolite-to-parent drug ratios were determined. Zolpidem, diazepam, nordazepam, oxazepam, lorazepam, midazolam, alprazolam, and bromazepam were...
Source: Journal of Pharmaceutical and Biomedical Analysis - February 7, 2020 Category: Drugs & Pharmacology Source Type: research

Analysis of chlorhexidine gluconate in skin using tape stripping and ultrahigh-performance liquid chromatography-tandem mass spectrometry
Publication date: Available online 6 February 2020Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Xueheng Zhao, Joshua K. Schaffzin, Jennifer Carson, Andrea Ankrum, Edward Dobrzykowski, David Haslam, Christopher Dandoy, Kenneth D.R. SetchellAbstractBackgroundTopical chlorhexidine gluconate (CHG) is used widely to reduce healthcare-associated infection. The optimal therapeutic dose for maximum efficacy and reduced toxicity is unclear, in part because of the lack of analytical methods to monitor CHG levels in skin. A novel method was developed to accurately measure CHG levels in skin after topical applica...
Source: Journal of Pharmaceutical and Biomedical Analysis - February 7, 2020 Category: Drugs & Pharmacology Source Type: research

Determination of Heavy Metals in Cancerous and Healthy Colon Tissues using Laser Induced Breakdown Spectroscopy and its Cross-Validation with ICP-AES Method
Publication date: Available online 7 February 2020Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): M.A. Gondal, R.K. Aldakheel, M.A. Almessiere, M.M. Nasr, J.A. Almusairii, B. GondalAbstractCertain types of cancer deaths are widespread due to the diagnostic complexities at the early stages. Recent studies revealed that the bio-accumulated heavy metals (act as pro-carcinogens) in the human colon cause strong interactions with the nuclear proteins, leading to the DNA damages and repair processes inhibition, resulting in the cancers. Most of the conventional detection techniques suffer from the insensitiven...
Source: Journal of Pharmaceutical and Biomedical Analysis - February 7, 2020 Category: Drugs & Pharmacology Source Type: research

Impurity profiling of l-aspartic acid and glycine using high-performance liquid chromatography coupled with charged aerosol and ultraviolet detection
Publication date: Available online 5 February 2020Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Ruben Pawellek, Klaus Schilling, Ulrike HolzgrabeAbstractFor the compendial related substances test of L-aspartic acid (Asp) and glycine (Gly), two separate reversed-phase ion-pair high-performance liquid chromatography methods coupled with charged aerosol and ultraviolet detection were developed. Separation of all putative impurities, in particular of the related carboxylic and amino acids, was achieved using volatile perfluorocarboxylic acids as ion-pairing reagents on a polar embedded C18 stationary phas...
Source: Journal of Pharmaceutical and Biomedical Analysis - February 7, 2020 Category: Drugs & Pharmacology Source Type: research

Synthesis and characterization of oxitropium bromide related substances and novel stability indicating HPLC methods
Publication date: Available online 5 February 2020Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Esen Bellur Atici, Çağan Ağtaş, Yücel Yazar, Nurten RıdvanoğluAbstractThe European Pharmacopoeia (Ph. Eur.) described two separate HPLC methods for determination of organic impurities in oxitropium bromide, a synthetic anticholinergic agent used by inhalation in the treatment of asthma and other bronchial disorders, and a potentiometric titration assay method which is not a stability indicating method. During synthetic process development and analytical studies of oxitropium; besides known ...
Source: Journal of Pharmaceutical and Biomedical Analysis - February 7, 2020 Category: Drugs & Pharmacology Source Type: research

A stability-indicating LC–MS/MS method optimization for Pemetrexed through design of experiments: Identification and characterization of major oxidative degradation product
Publication date: Available online 5 February 2020Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): S.T Narenderan, J Ramesh, B Babu, S.N MeyyanathanAbstractA stability-indicating high-performance liquid chromatography method for Pemetrexed bulk was developed and validated as per the ICH guidelines by employing design of experiments methodology equipped with Box–Behnken design. The separation of Pemetrexed and its oxidative degradation product was achieved in isocratic elution mode with Zorbax C18 column (150 mm x 4.6 mm x5 µm) using 10 mM ammonium ace...
Source: Journal of Pharmaceutical and Biomedical Analysis - February 7, 2020 Category: Drugs & Pharmacology Source Type: research

Reversed phase UPLC/APCI-MS determination of Vitamin K1 and menaquinone-4 in human plasma: application to a clinical study
Publication date: Available online 4 February 2020Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Yuning Zhang, Yashpal S. Chhonker, Veenu Bala, Alex Hagg, Linda G. Snetselaar, Terry L. Wahls, Daryl J. MurryAbstractA rapid and sensitive liquid chromatographic-tandem mass spectrometric method was developed and validated to simultaneously quantitate vitamin K1 (PK) and vitamin K2 (MK-4) concentrations in human plasma to evaluate nutritional interventions. Charcoal-stripped human plasma was used for standard and calibration preparation with vitamin E-d6 as the internal standard. Patient plasma samples were...
Source: Journal of Pharmaceutical and Biomedical Analysis - February 5, 2020 Category: Drugs & Pharmacology Source Type: research

Qualitative and quantitative determination of anaprazole and its major metabolites in human plasma
Publication date: Available online 4 February 2020Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Chongzhuang Tang, Liang Li, Xifeng Ma, Jin Wang, Bo Chen, Xiaojian Dai, Yifan Zhang, Xiaoyan ChenAbstractAnaprazole is a novel proton pump inhibitor under development for the treatment of gastric and duodenal ulcers. In the present study, an ultra-performance liquid chromatography-ultraviolet detector/quadrupole time-of-flight mass spectrometry method was developed for the metabolic profiling of human plasma after an oral administration of 40 mg anaprazole. The principal metabolic pathways were ident...
Source: Journal of Pharmaceutical and Biomedical Analysis - February 5, 2020 Category: Drugs & Pharmacology Source Type: research

Correlation study between the pharmacokinetics of seven main active ingredients of Mahuang decoction and its pharmacodynamics in asthmatic rats
Publication date: Available online 3 February 2020Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Pengcheng Huang, Yinghong Tang, Chang Li, Huifen Zhou, Li Yu, Haitong Wan, Yu HeAbstractThe aim of this study was to investigate the pharmacokinetics and pharmacodynamics of seven main active components of Mahuang decoction (MHD) and its time-concentration-effect relationship. The asthmatic rat model was established by the method of ovalbumin (OVA) sensttization. The plasma concentrations of ephedrine, pseudoephedrine, methylephedrine, amygdalin, liquiritin, cinnamic acid, glycyrrhizic acid in asthmatic mod...
Source: Journal of Pharmaceutical and Biomedical Analysis - February 4, 2020 Category: Drugs & Pharmacology Source Type: research

Elimination pharmacokinetics of sphaeralcic acid, tomentin and scopoletin mixture from a standardized fraction of Sphaeralcea angustifolia (Cav.) G. Don orally administered
The objective of this work was to determine the pharmacokinetic constants of urinary and fecal elimination in mice of the anti-arthritic compounds, after oral administration (400 mg / kg) of a standardized active fraction (SaTES) of S. angustifolia. It was established that the coumarin mixture (scopoletin and tomentin) were eliminated by the urine; while, sphaeralcic acid was mainly eliminated by fecal path, following both a non-compartmental behavior. No products derived from their biotransformation were detected.Graphical abstract (Source: Journal of Pharmaceutical and Biomedical Analysis)
Source: Journal of Pharmaceutical and Biomedical Analysis - February 4, 2020 Category: Drugs & Pharmacology Source Type: research

NMR-derived targeted serum metabolic biomarkers appraisal of bladder cancer: A pre- and post-operative evaluation
This study was conducted on 160 sera samples involving HC (n = 52), pre-operative (n = 55) and post-operative (n = 53) BC cases. 1H nuclear magnetic resonance (NMR) spectroscopy was used to generate serum metabolic profiles and to gauge aberrantly expressed metabolites. The targeted metabolomic approach revealed that the expression levels of these signature metabolites were progressively and significantly decreased in post-operative follow-up at the interval of 30, 60, and 90 days compared to pre-operative BC sera samples and were maintained at HC levels. Serum metabolic biomarkers...
Source: Journal of Pharmaceutical and Biomedical Analysis - February 3, 2020 Category: Drugs & Pharmacology Source Type: research

Development and validation of a UPLC-MS/MS method for simultaneous quantification of levofloxacin, ciprofloxacin, moxifloxacin and rifampicin in human plasma: application to the therapeutic drug monitoring in osteoarticular infections
ConclusionA simple, rapid, and selective liquid chromatography-tandem mass spectrometry method was developed and validated for the simultaneous quantification of levofloxacin, ciprofloxacin, moxifloxacin and rifampicin in human plasma.Graphical abstract (Source: Journal of Pharmaceutical and Biomedical Analysis)
Source: Journal of Pharmaceutical and Biomedical Analysis - February 3, 2020 Category: Drugs & Pharmacology Source Type: research

Pharmacokinetics, tissue distribution, and safety evaluation of a ligustilide derivative (LIGc)
Publication date: Available online 31 January 2020Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Yanxia Zhang, Yaming Zhang, Yanming Han, Ye Tian, Pengcheng Wu, Aiyi Xin, Xiaoning Wei, Yanbin Shi, Zhenchang Zhang, Gang Su, Yanping Shi, Junxi LiuAbstractLigustilide (LIG) is the main active ingredient of Angelica sinensis (Oliv.) Diels and has a neuroprotective effect against ischemic stroke. However, owing to its multi-conjugated unstable structure, the compound has poor drug-forming properties. Therefore, we synthesized highly stable colorless needle crystals (known as ligusticum cycloprolactam, LIGc) ...
Source: Journal of Pharmaceutical and Biomedical Analysis - February 1, 2020 Category: Drugs & Pharmacology Source Type: research

Active vitamin D and vitamin D analogs stimulate fibroblast growth factor 23 production in osteocyte-like cells via the vitamin D receptor
Publication date: Available online 31 January 2020Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Mitsuru Yashiro, Masaki Ohya, Toru Mima, Yuri Nakashima, Kazuki Kawakami, Shuto Yamamoto, Sou Kobayashi, Takurou Yano, Yusuke Tanaka, Tomohiro Sonou, Kouichi Tatsuta, Shigeo Negi, Takashi ShigematsuAbstractOsteocytes play an important role in the regulation of serum phosphorus by producing fibroblast growth factor 23 (FGF23). FGF23 production is stimulated by 1α,25-dihydroxyvitamin D in osteocytes. However, it is unclear whether vitamin D induces FGF23 production in osteocytes directly. Therefore, we ...
Source: Journal of Pharmaceutical and Biomedical Analysis - February 1, 2020 Category: Drugs & Pharmacology Source Type: research