Rapid, hydrolysis-free, dilute-and-shoot method for the determination of buprenorphine, norbuprenorphine and their glucuronides in urine samples using UHPLC-MS/MS
Publication date: Available online 11 January 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Marco Agostini, Caterina Renzoni, Elisabetta Pierini, Maurizio Piergiovanni, Veronica Termopoli, Giorgio Famiglini, Pierangela Palma, Achille CappielloAbstractBuprenorphine and its metabolites are routinely monitored to assess patient compliance with drug detoxification programs or as pain killers. A rapid method for the simultaneous analysis of buprenorphine, norbuprenorphine, and glucuronides in urine using ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) was developed. ...
Source: Journal of Pharmaceutical and Biomedical Analysis - January 12, 2019 Category: Drugs & Pharmacology Source Type: research

The Effect of Fatty Acids in Red Blood Cell Membranes on the Dynamics of Inflammatory Markers Following the Coronary Stent Implantation
Publication date: Available online 11 January 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Vladimíra Mužáková, Milan Meloun, Andrea Jindrová, Alexander ČeganAbstractThe effect of 20 fatty acids in erythrocyte cell membranes on the extent of inflammatory response and cell oxidative stress was evaluated using multidimensional statistical data analysis in 54 patients suffering from ischemic heart disease undergoing percutaneous coronary intervention with coronary stent implantation using multidimensional statistical data analysis. A systemic inflammatory response was in...
Source: Journal of Pharmaceutical and Biomedical Analysis - January 12, 2019 Category: Drugs & Pharmacology Source Type: research

Determination of total and unbound ribociclib in human plasma and brain tumor tissues using liquid chromatography coupled with tandem mass spectrometry
This study was to develop and validate a liquid chromatography with tandem mass spectrometry (LC-MS/MS) method for determining total and unbound concentrations of ribociclib in human plasma and brain tumor tissue samples. Plasma and tumor homogenate samples were extracted using protein precipitation with acetonitrile. Unbound fraction in plasma or tumor homogenate was determined by equilibrium dialysis method. Chromatographic separation was achieved based on aqueous normal-phase chromatography mechanism on a Waters XBridgeTM Amide column under isocratic elution with acetonitrile-ammonium formate (10 mM, pH 3) (75:25...
Source: Journal of Pharmaceutical and Biomedical Analysis - January 12, 2019 Category: Drugs & Pharmacology Source Type: research

A strategy based on fingerprinting and chemometrics for the detection of regulated plants in plant food supplements from the Belgian market: two case studies
Publication date: Available online 11 January 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Deconinck E., Vanhamme M., Bothy J.L., P. CourselleAbstractThe sale and consumption of plant food supplements is increasing, especially in the western world. A lot of these supplements can be bought through internet, where a lot of illegal trade is going on. Every year seized dietary supplements are send to laboratories in order to screen for the presence of chemical adulterants or illegally added active pharmaceutical ingredients, though also herbal adulteration occurs and is given less attention.In this p...
Source: Journal of Pharmaceutical and Biomedical Analysis - January 11, 2019 Category: Drugs & Pharmacology Source Type: research

A systematic review of the stability of finished pharmaceutical products and drug substances beyond their labeled expiry dates
Publication date: Available online 11 January 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Markus Zilker, Fritz Sörgel, Ulrike HolzgrabeAbstractIn recent years, there has been a very active debate about the stability of drug products especially after exceeding the expiry dates. The regulatory authorities require comprehensive stability data for market approval. The shelf-life obtained determines the expiry date, which is typically between 1 and 5 years and commonly set in a conservative manner. Conducting stability studies is a resource- and time-consuming matter for the pharmaceutical manuf...
Source: Journal of Pharmaceutical and Biomedical Analysis - January 11, 2019 Category: Drugs & Pharmacology Source Type: research

Editorial Board
Publication date: 20 February 2019Source: Journal of Pharmaceutical and Biomedical Analysis, Volume 165Author(s): (Source: Journal of Pharmaceutical and Biomedical Analysis)
Source: Journal of Pharmaceutical and Biomedical Analysis - January 11, 2019 Category: Drugs & Pharmacology Source Type: research

A validated UPLC-MS/MS method for pharmacokinetic study of Inflachromene, a novel microglia inhibitor
Publication date: Available online 9 January 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Hwan Hee Lee, So Hee Im, Sunjoo Ahn, Myung Ae Bae, Seung Bum Park, Sang Kyum Kim, Jin Sook SongAbstractInflachromene (ICM), a novel microglia inhibitor, is under development to treat neuroinflammatory disorders. For the pharmacokinetic evaluation of ICM, we developed quantitative ultra-performance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS) method in rat plasma. Protein precipitation method with acetonitrile (ACN) was used for plasma sample preparation. The analyte and carbamazepin...
Source: Journal of Pharmaceutical and Biomedical Analysis - January 10, 2019 Category: Drugs & Pharmacology Source Type: research

Qualitative analysis of the roots of salvia miltiorrhiza and Salvia yunnanensis based on NIR, UHPLC and LC-MS-MS
Publication date: Available online 9 January 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Lijun Ni, Fangfang Zhang, Mingyue Han, Liguo Zhang, Shaorong Luan, Wei Li, Haixing Deng, Zhuhui Lan, Zhongxiang Wu, Xiaofang Luo, Leslaw MleczkoAbstractNear infrared spectroscopy (NIR) was applied to discriminate the roots of salvia miltiorhiza Bunge (Danshen for short) and salvia yunnanensis C. H. Wright (Zidanshen for short) by means of principal component analysis (PCA), improved and simplified K nearest neighbors (IS-KNN). Furthermore, an ultra-high performance liquid chromatographic (UHPLC) coupled with...
Source: Journal of Pharmaceutical and Biomedical Analysis - January 10, 2019 Category: Drugs & Pharmacology Source Type: research

Monolith weak affinity chromatography for µg-protein-ligand interaction study
Publication date: Available online 9 January 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Lucile Lecas, Jérôme Randon, Alain Berthod, Vincent Dugas, Claire DemesmayAbstractAffinity monolith columns of 375 nL (effective length 8.5 cm, internal diameter 75 µm) were developed for protein-ligand affinity investigations needing only 3 µg of human serum albumin (HSA). To promote specific interactions and avoid non-specific ones, different combinations of monolithic supports and bio-functionalization pathways were evaluated. Silica and glycidylmethacr...
Source: Journal of Pharmaceutical and Biomedical Analysis - January 10, 2019 Category: Drugs & Pharmacology Source Type: research

Sub-picomolar quantification of PTH1-34 in plasma by UHPLC-MS/MS after subcutaneous injection of teriparatide and identification of PTH1-33, its degradation product
Publication date: Available online 9 January 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Philippe J. Eugster, Haithem Chtioui, Adeline Herren, Marielle Dunand, Delphine Cappelle, Julien Bourquin, Thierry Buclin, Eric GrouzmannAbstractTeriparatide (PTH1-34, Forsteo®) is a bioactive N-terminal fragment of the native endogenous parathyroid hormone (PTH1-84) recommended for the treatment of osteoporosis in patients with high risk of fracture. Since PTH1-34 may undergo proteolysis we have validated an ultra-high pressure liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) method for unam...
Source: Journal of Pharmaceutical and Biomedical Analysis - January 10, 2019 Category: Drugs & Pharmacology Source Type: research

Bioassay based screening for the antiplatelet aggregation quality markers of Polygonum multiflorum with UPLC and chemometrics
Publication date: Available online 9 January 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Chunyu Li, Can Tu, Yi Che, Mingyu Zhang, Bin Dong, Xiaowei Zhou, Yafei Shi, Guohui Li, Jiabo WangAbstractCurrently, an increasing number of human’s health is seriously affected by acute thrombotic events. In China, Polygonum multiflorum (PM) is commonly used to treat diseases associated with thrombosis. Our previous work showed that PM could inhibit platelet aggregation that play a key role in the pathogenesis of thrombosis. However, the constituents of PM are complicated and its quality control method...
Source: Journal of Pharmaceutical and Biomedical Analysis - January 10, 2019 Category: Drugs & Pharmacology Source Type: research

Stability behaviour of antiretroviral drugs and their combinations. 9: Identification of incompatible excipients
Publication date: Available online 8 January 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Moolchand Kurmi, Archana Sahu, Mayurbhai Kathadbhai Ladumor, Arvind Kumar Bansal, Saranjit SinghAbstractIncompatibility studies of antiretroviral drugs, viz., lamivudine (3TC), emtricitabine (FTC), abacavir sulfate (ABC), tenofovir disoproxil fumarate (TDF), zidovudine (ZDV), efavirenz (EFV) and nevirapine (NVP) were carried out in the presence of ten selected excipients, i.e., microcrystalline cellulose, lactose monohydrate, starch, magnesium stearate, sodium lauryl sulfate, sodium starch glycolate, croscar...
Source: Journal of Pharmaceutical and Biomedical Analysis - January 9, 2019 Category: Drugs & Pharmacology Source Type: research

Development of a UPLC-ESI-MS method for simultaneous determination of flavonoids and diterpenes in Egletes viscosa (L.) Less herbal products
Publication date: Available online 8 January 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Kaline Rodrigues Carvalho, Guilherme Julião Zocolo, Rita de Cássia Alves Pereira, Fátima Itana Chaves Custódio Martins, Paulo Riceli Vasconcelos Ribeiro, Edy Sousa de Brito, Edilberto Rocha Silveira, Kirley Marques CanutoAbstractEgletes viscosa (L.) Less (Asteraceae) is a tropical aromatic herb whose flower buds are used for gastrointestinal disorders. Its gastroprotective properties have been attributed to the flavonoid ternatin and the furan diterpenes tanabalin and centipedic a...
Source: Journal of Pharmaceutical and Biomedical Analysis - January 9, 2019 Category: Drugs & Pharmacology Source Type: research

Corrigendum to “Quantification of diterpene acids in Copaiba oleoresin by UHPLC-ELSD and heteronuclear two-dimensional qNMR” [J. Pharm. Biomed. Anal. 160 (2018) 126–134]
Publication date: Available online 8 January 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Serhat Sezai Çiçek, Anna Laís Pfeifer Barbosa, Ulrich Girreser (Source: Journal of Pharmaceutical and Biomedical Analysis)
Source: Journal of Pharmaceutical and Biomedical Analysis - January 9, 2019 Category: Drugs & Pharmacology Source Type: research

Investigations into the therapeutic effects of aerial and stem parts of Buxus papillosa C.K. Schneid.: In vitro chemical, biological and toxicological perspectives
In this study, different solvent extracts (methanol, dichloromethane and n-hexane) from aerial and stem parts of Buxus papillosa C.K. Schneid (Buxaceae) were investigated for a panoply of bioassays. Biological profiles were established by determining antioxidant and enzyme inhibition profiles. Toxicity was tested using MTT cell viability assay on five different human cancer cell lines i.e, MCF-7, MDA-MB-231 CaSki, DU-145 and SW-480. For chemical fingerprinting, total bioactive contents and UHPLC-MS secondary metabolites profile were determined. Generally, both aerial and stem methanol extracts had highest total bioactive c...
Source: Journal of Pharmaceutical and Biomedical Analysis - January 8, 2019 Category: Drugs & Pharmacology Source Type: research

Isolation and structural characterization of degradation products of afatinib dimaleate by LC-Q-TOF/MS/MS and NMR: cytotoxicity evaluation of afatinib and isolated degradation products
Publication date: Available online 7 January 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Balasaheb B. Chavan, Sawant Vitthal, Roshan M. Borkar, R. Srinivas, M.V.N. Kumar TalluriAbstractAfatinib is an irreversible tyrosine kinase receptor inhibitor which was approved lately by USFDA for the treatment of metastatic non-small cell lung cancer (NSCLC). AFT was subjected to stress degradation studies under hydrolytic (acid, base and neutral), oxidative, thermal and photolytic conditions to investigate the inherent stability of the drug. The present study describes the simple and rapid HPLC method dev...
Source: Journal of Pharmaceutical and Biomedical Analysis - January 8, 2019 Category: Drugs & Pharmacology Source Type: research

Enantioseparation of N-acetyl-dl-cysteine as o-phtaldialdehyde derivatives obtained with various primary aliphatic amine additives on polysaccharide-based chiral stationary phases
Publication date: Available online 8 January 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Michal DoušaAbstractA sensitive and rapid high-performance liquid chromatography (HPLC) method was developed to enantioseparation of N-acetyl-DL-cysteine after precolumn derivatization using o-phthaldialdehyde and primary aliphatic amines. Seven polysaccharide-based chiral columns were tested in a reversed phase mode. Under the optimal chromatographic conditions, N-acetyl-DL-cysteine derivatives were completely enantioseparated on Chiralcel OZ-3R column with the resolution more than 2.5. The impact of...
Source: Journal of Pharmaceutical and Biomedical Analysis - January 8, 2019 Category: Drugs & Pharmacology Source Type: research

Solid-phase extraction combined with dispersive liquid-liquid microextraction/HPLC-UV as a sensitive and efficient method for extraction, pre-concentration and simultaneous determination of antiretroviral drugs nevirapine, efavirenz and nelfinavir in pharmaceutical formulations and biological samples
Publication date: Available online 4 January 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Mehregan Safari, Mojtaba Shamsipur, Parvin Zohrabi, Homeira EbrahimzadehAbstractTherapeutic drug monitoring (TDM) of antiretroviral drugs requires accurate and precise analysis of their trace amounts in plasma samples. Solid-phase extraction (SPE) coupled with dispersive liquid-liquid microextraction based on solidification of floating organic drop (DLLME-SFO) was introduced as a simple and sensitive method for extraction, pre-concentration and simultaneous determination of efavirenz (EFV), nelfinavir (NFV) ...
Source: Journal of Pharmaceutical and Biomedical Analysis - January 5, 2019 Category: Drugs & Pharmacology Source Type: research

Hydrophilic-interaction planar chromatography in ultra-sensitive determination of α-aminocephalosporin antibiotics. Application to analysis of cefalexin in goat milk samples using modified QuEChERS extraction technique
Publication date: Available online 3 January 2019Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Azza H. Rageh, Sherien A. Abdel-Rahim, Hassan F. Askal, Gamal A. SalehAbstractA highly sensitive, selective and precise HPTLC method coupled with fluorescence detection was developed and validated for the determination of α-aminocephalosporin antibiotics; namely cefalexin, cefadroxil and cefradine in their standard solutions. The applicability of the developed methodology was demonstrated via analysis of cefalexin in goat milk samples. Full optimization of the fluorescence derivatization reaction was c...
Source: Journal of Pharmaceutical and Biomedical Analysis - January 4, 2019 Category: Drugs & Pharmacology Source Type: research

Hypercrosslinked strong anion-exchange polymers for selective extraction of fluoroquinolones in milk samples
Publication date: Available online 31 December 2018Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Xiaoping Liang, Ping Hu, Hongyang Zhang, Wen TanAbstractIn this work, hypercrosslinked strong anion-exchange polymer resins (HXLPP-SAX) were synthesized and evaluated as solid-phase extraction (SPE) sorbents for extracting fluoroquinolones (FQs) in milk samples. These particles were prepared using a protocol that was facile and cost-effective by combining hypercrosslinking reactions and quaternisation reactions in one step. After the synthesis, the morphological properties and anion-exchange, adsorption, a...
Source: Journal of Pharmaceutical and Biomedical Analysis - January 1, 2019 Category: Drugs & Pharmacology Source Type: research

Isolation of punicalagin from Punica granatum rind extract using mass-directed semi-preparative ESI-AP single quadrupole LC-MS
Publication date: Available online 31 December 2018Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Mirko Barbieri, Charles M. HeardAbstractWe are living in a era of alarming increases in microbial resistance to currently available antibiotics, and there is a growing need for new pharmaceutical products to treat infectious diseases. The pomegranate is an edible fruit that has virucidal and antimicrobial activities which is primarily attributable to the high concentration of hydrolysable tannins. Punicalagin, a high molecular weight tannin (1084.7), accounts for approximately 70% of the total and is conce...
Source: Journal of Pharmaceutical and Biomedical Analysis - January 1, 2019 Category: Drugs & Pharmacology Source Type: research

Micro-solid phase extraction and LC–MS3 for the determination of triptorelin in rat plasma and application to a pharmacokinetic study
Publication date: 20 March 2019Source: Journal of Pharmaceutical and Biomedical Analysis, Volume 166Author(s): Tianming Ren, Zhi Zhang, John Paul Fawcett, Dong Sun, Jingkai GuAbstractTriptorelin is a synthetic decapeptide used for the treatment of prostate cancer. Attempts to determine triptorelin in clinical use by liquid chromatography-tandem mass spectrometry with multiple reaction monitoring have encountered problems due to its low concentration in plasma (pg/mL) and interference from endogenous peptides. We have overcome these issues using micro-solid phase extraction (μ-SPE) on Oasis® HLB 96-well μElution p...
Source: Journal of Pharmaceutical and Biomedical Analysis - January 1, 2019 Category: Drugs & Pharmacology Source Type: research

A high-performance liquid chromatography-tandem mass spectrometry method for the determination of lifrafenib, a novel RAF kinase and EGFR inhibitor, in human plasma and urine and its application in clinical pharmacokinetic study
Publication date: 20 March 2019Source: Journal of Pharmaceutical and Biomedical Analysis, Volume 166Author(s): Xueting Yao, Ling Song, Yang Liu, Huanhuan Wang, Jie Liu, Ji Jiang, Dongyang Liu, Pei HuAbstractLifirafenib (BGB-283), a dual inhibitor trageting BRAF kinase and EGFR, showed favorable efficacy and safety in treating patients with different cancer types harboring mutations in BRAF, KRAS and NRAS. In order to support the clinical pharmacokinetic study, a sensitive high performance liquid chromatography-tandem mass spectrometry (HPLC–MS/MS) method was developed and validated to quantify lifirafenib concentrati...
Source: Journal of Pharmaceutical and Biomedical Analysis - January 1, 2019 Category: Drugs & Pharmacology Source Type: research

Study on the herb-herb interaction of Danqi Tongmai Tablet based on the pharmacokinetics of twelve notoginsenoides in acute myocardial ischemia and sham rats
Publication date: Available online 29 December 2018Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Haijuan Zhi, Yanping Deng, Bingpeng Yan, Zhenwei Li, Sumei Han, Yibei Zhang, Jinjun Hou, Wu Wanying, Dean GuoAbstractDanqi Tongmai tablet (DQTT), an innovative TCM formula under clinical trials, is composed of salvianolic acids (SA) and panax notoginsenosides (PNE) for the treatment of coronary heart disease and angina pectoris. However, the in vivo herb-herb interaction of DQTT remains unclear. In the present research, a rapid, reliable and sensitive method for quantitative analysis of multi-notoginsenosi...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 30, 2018 Category: Drugs & Pharmacology Source Type: research

LC-MS application for Therapeutic Drug Monitoring in alternative matrices
Publication date: Available online 29 December 2018Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Valeria Avataneo, Antonio D’Avolio, Jessica Cusato, Marco Cantù, Amedeo De NicolòAbstractNowadays the practice of therapeutic drug monitoring, consisting in the measurement of drugs concentrations in biological matrices in order to guide possible posological adjustments, is becoming more and more important for the management and optimization of several treatments, especially when drugs with narrow therapeutic indexes are administered.Although TDM on plasma samples is currently considere...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 30, 2018 Category: Drugs & Pharmacology Source Type: research

Development and validation of a sensitive method for alkyl sulfonate genotoxic impurities determination in drug substances using gas chromatography coupled to triple quadrupole mass spectrometry
Publication date: Available online 30 December 2018Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Zhen Liu, Huajun Fan, Yihui Zhou, Xiaowei Qian, Jihui Tu, Bin Chen, Gengli DuanAbstractAlkyl sulfonate esters have been widely concerned as genotoxic impurities (GTIs). A gas chromatography triple-quadrupole mass spectrometry (GC-MS/MS) method has been developed for trace determination of 9 commonly encountered sulfonate esters in drug substances. Three different solvents of acetonitrile (ACN), dichloromethane (DCM) and ethyl acetate (EtOAc) were evaluated as diluents to accommodate different solubilities ...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 30, 2018 Category: Drugs & Pharmacology Source Type: research

Quantitative bioanalytical assay for the human epidermal growth factor receptor (HER) inhibitor dacomitinib in rat plasma by UPLC-MS/MS
Publication date: Available online 28 December 2018Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Xiangjun Qiu, Qianmeng Lin, Zongdi Ning, Xin Qian, Pengbo Li, Lei Ye, Saili XieAbstractDacomitinib is a highly selective irreversible small-molecule inhibitor of the human epidermal growth factor receptor (HER) family of tyrosine kinases. A simple and quick bioanalytical method was completely developed and validated for the assay and pharmacokinetic investigation of dacomitinib in rat plasma using ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). Proteins in 0.1 mL plasm...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 29, 2018 Category: Drugs & Pharmacology Source Type: research

Predictive metabolic signatures for the occurrence and development of diabetic nephropathy and the intervention of Ginkgo biloba leaves extract based on gas or liquid chromatography with mass spectrometry
Publication date: Available online 26 December 2018Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Yan Du, Bing-ju Xu, Xu Deng, Xiao-wen Wu, Yin-jie Li, Shi-rui Wang, Yi-nan Wang, Shuai Ji, Meng-zhe Guo, Dong-zhi Yang, Dao-quan TangAbstractDiabetic nephropathy (DN) is one of the leading causes of death in diabetes mellitus (DM). Early warning and therapy has significant clinical value for DN. This research sought to find biomarkers to predict the occurrence and development of DN and the intervention of Ginkgo biloba leaves extract (GBE) by quantifying fatty acids, amino acids, and nucleosides and nucleo...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 27, 2018 Category: Drugs & Pharmacology Source Type: research

Micro-solid phase extraction and LC-MS3 for the determination of triptorelin in rat plasma and application to a pharmacokinetic study
Publication date: Available online 26 December 2018Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Tianming Ren, Zhi Zhang, John Paul Fawcett, Dong Sun, Jingkai GuAbstractTriptorelin is a synthetic decapeptide used for the treatment of prostate cancer. Attempts to determine triptorelin in clinical use by liquid chromatography-tandem mass spectrometry with multiple reaction monitoring have encountered problems due to its low concentration in plasma (pg/mL) and interference from endogenous peptides. We have overcome these issues using micro-solid phase extraction (µ-SPE) on Oasis® HLB 96-well &m...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 27, 2018 Category: Drugs & Pharmacology Source Type: research

Two distinct conformers of SAG investigated by solution NMR and variable-temperature experiments
Publication date: Available online 12 December 2018Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Haipeng Jiang, Xian Wang, Xiaoliang CuiAbstractSAG (Smo agonist) is high specific agonist of Smo receptor, it is widely used as chemical probe to explore the therapeutic value of activating the Hh-signaling pathway. In the present work, the coexistence of two distinct conformers (A and B) of SAG are revealed by solution NMR, the 3D structural difference of the two conformers are elucidated by ROESY spectroscopy and MMFF94 program. It is discovered that both conformers are agonists of Smo receptor, and the ...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 25, 2018 Category: Drugs & Pharmacology Source Type: research

Effect of Wuziyanzong pill on metabolism of dapoxetine in vivo and in vitro
Publication date: Available online 15 December 2018Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Hong-chang Yuan, Zhi-jian Deng, Xin-min Liu, Ting-fang Dong, Xiang-jun Qiu, Zeng NanAbstractIn vitro incubation of rat liver microsomes with 30 µL of 100 μmol L-1 dapoxetine and 30 µL of 10, 100, 250, 500, 1,000, 2,500, or 5,000 μg mL-1 Wuziyanzong pill was performed at 37℃ for 60 min. Dapoxetine concentration was analyzed by high performance liquid chromatography (HPLC). The half maximal inhibitory concentration (IC50) of Wuziyanzong pil...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 25, 2018 Category: Drugs & Pharmacology Source Type: research

Efficient extraction of flavonoids from Flos Sophorae Immaturus by tailored and sustainable deep eutectic solvent as green extraction media
In this study, the extraction of six compounds from Flos Sophorae Immaturus (FSI) with DES-5 (choline chloride/1,4-butanediol) as its topgallant solvent was determined by screening nine DESs. After single factor test and BBD experiment, the optimum conditions of deep eutectic solvent-based microwave-assisted extraction (DES-MAE) were: choline chloride/1,4-butanediol (molar ratio of 1:2) and water content (25%, v/v), time 20 min, microwave power 600 W, temperature 62 ℃, liquid/solid ratio 26 mL/g. The extraction yields of rutin, nicotiflorin, narcissin, quercetin, kaempferol and isorhamnetin were 116....
Source: Journal of Pharmaceutical and Biomedical Analysis - December 25, 2018 Category: Drugs & Pharmacology Source Type: research

Validation of a UPLC-PDA method to study the content and stability of 5-chloro 8-hydroxyquinoline and 5,7-dichloro 8-hydroxyquinoline in medicated feed used in swine farming
Publication date: Available online 21 December 2018Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Castillo Rodríguez Miriam Aide, Rodríguez Patiño Gabriela, Revilla Vázquez Alma Luisa, Rodríguez de San Miguel Eduardo, López-Arellano RaquelABSTRACTA new, rapid, simple and specific method to determine 5-chloro 8-hydroxyquinoline (5-HQ) and 5,7-dichloro 8-hydroxyquinoline (5,7-HQ) stability in swine feed was optimized and validated. A system consisting of an ACQUITY UPLC BEH C18 column (1.7 µm, 2.1 mm x 100 mm), a mobile ph...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 25, 2018 Category: Drugs & Pharmacology Source Type: research

UPLC-MS/MS method for the simultaneous determination of imatinib, voriconazole and their metabolites concentrations in rat plasma
Publication date: Available online 21 December 2018Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Ren-ai Xu, Qianmeng Lin, Xiangjun Qiu, Jingjing Chen, Yuanyuan Shao, Guoxin Hu, Guanyang LinABSTRACTIn the present study, a simple ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) method used to measure the plasma concentrations of imatinib, voriconazole and their metabolites (N-desmethyl imatinib and N-oxide voriconazole) in rats simultaneously making use of diazepam as the internal standard (IS) had been developed and validated. A simple protein precipitation by acetonitrile ...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 25, 2018 Category: Drugs & Pharmacology Source Type: research

Development and validation of a new UHPLC method for related proteins in insulin and insulin analogues as an alternative to the European Pharmacopoeia RP-HPLC method
Publication date: Available online 23 December 2018Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Oliver Wahl, Sylvie JorajuriaAbstractThe LC methods for related proteins prescribed in the European Pharmacopoeia monographs for insulins and insulin analogues are very similar and present some drawbacks including long run time and low resolution. LC to UHPLC-UV geometrical transfer was attempted to overcome such drawbacks. With the new UHPLC method, additional substances were separated in bovine and porcine insulins. A UHPLC MS-compatible method was developed using a mixed-mode C18 stationary phase with c...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 25, 2018 Category: Drugs & Pharmacology Source Type: research

A high-performance liquid chromatography-tandem mass spectrometry method for the determination of BGB-283, a novel RAF kinase and EGFR inhibitor, in human plasma and urine and its application in clinical pharmacokinetic study
Publication date: Available online 24 December 2018Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Xueting Yao, Ling Song, Yang Liu, Huanhuan Wang, Jie Liu, Ji Jiang, Dongyang Liu, Pei HuAbstractBGB-283, a novel BRAF kinase and EGFR inhibitor, showed favorable efficacy and safety in treating patients with different cancer types harboring mutations in BRAF, KRAS and NRAS. In order to support the clinical pharmacokinetic study, a sensitive high performance liquid chromatography-tandem mass spectrometry (HPLC–MS/MS) method was developed and validated to determine BGB-283 concentration in human plasma...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 25, 2018 Category: Drugs & Pharmacology Source Type: research

Study of aldehyde oxidase with phthalazine as substrate using both off-line and on-line capillary electrophoresis
Publication date: 20 February 2019Source: Journal of Pharmaceutical and Biomedical Analysis, Volume 165Author(s): Shengyun Huang, Getu Kahsay, Erwin Adams, Ann Van SchepdaelAbstractAn optimized and economical capillary electrophoretic method for both off-line and on-line study of the enzyme aldehyde oxidase and its substrate phthalazine was developed. The separation of the substrate phthalazine and its metabolite 1-phthalazinone was achieved using micellar electrokinetic chromatography (MEKC) with sodium dodecyl sulphate in the background electrolyte (BGE). The BGE consists of 25 mM sodium phosphate buffer containin...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 25, 2018 Category: Drugs & Pharmacology Source Type: research

Determination of polycyclic aromatic hydrocarbons in lipstick by gas-chromatography coupled to mass spectrometry: A case history
Publication date: 20 February 2019Source: Journal of Pharmaceutical and Biomedical Analysis, Volume 165Author(s): Gabriella Roda, Sebastiano Arnoldi, Eleonora Casagni, Michele Dei Cas, Laura Silva, Marina CariniAbstractA suitable extraction protocol based on an liquid-liquid extraction with hexane/dimethyl sulfoxide and a GC/MS method were developed and validated to determine the concentration of six prohibited Polycyclic Aromatic Hydrocarbons (PAHs; benzo[a]pyrene; dibenz[a,h]anthracene; benz[a]anthracene; benzo[j]fluoranthene; benzo[k]fluoranthene; chrysene) in lipsticks commissioned by a cosmetic company to a manufactur...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 25, 2018 Category: Drugs & Pharmacology Source Type: research

Identification and structural characterization of hydrolytic degradation products of alvimopan by LC/QTOF/MS/MS and NMR studies
Publication date: 20 February 2019Source: Journal of Pharmaceutical and Biomedical Analysis, Volume 165Author(s): Shandilya Mahamuni Baira, Srinivas R., M.V.N. Kumar TalluriAbstractAlvimopan (ALV), a peripherally acting mu-opioid receptor (PAM-OR) antagonist used for the treatment of postoperative ileus, was examined for its degradation behaviour under different stress conditions. A total of five degradation products (DP1-DP5) were formed and identified using high-performance liquid chromatography (HPLC) method. Primarily, complete fragmentation pathways of the protonated drug and its degradation products (DP1-DP5) were el...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 25, 2018 Category: Drugs & Pharmacology Source Type: research

Bioanalytical method validation: new FDA guidance vs. EMA guideline. Better or worse?
Publication date: 20 February 2019Source: Journal of Pharmaceutical and Biomedical Analysis, Volume 165Author(s): Michał Kaza, Marta Karaźniewicz-Łada, Katarzyna Kosicka, Anna Siemiątkowska, Piotr J. RudzkiAbstractBioanalysis concerns the identification and quantification of analytes in various biological matrices. Validation of any analytical method helps to achieve reliable results that are necessary for proper decisions on drug dosing and patient safety. In the case of bioanalytical methods, validation additionally covers steps of pharmacokinetic and toxicological studies – such as sample collection, handling,...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 25, 2018 Category: Drugs & Pharmacology Source Type: research

Generic gas chromatography flame ionization detection method using hydrogen as the carrier gas for the analysis of solvents in pharmaceuticals
In this study, a simple and efficient generic/universal GC-FID method using H2 as the carrier gas has been developed with the capability of baseline resolution of over 30 of the most commonly used solvents in development and manufacturing with a method run time of less than eight minutes. The use of this method for the separation and analysis of solvents within a pharmaceutical manufacturing process is demonstrated with additional method validation data presented using five different diluents as a means to increase flexibility for the chromatographer. Furthermore, it is the recommendation of the authors that the current co...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 21, 2018 Category: Drugs & Pharmacology Source Type: research

Quantitative determination of the antimalarials artemether and lumefantrine in biological samples: A review
Publication date: 20 February 2019Source: Journal of Pharmaceutical and Biomedical Analysis, Volume 165Author(s): Luisa Avelar Resende, Pedro Henrique Reis da Silva, Christian FernandesAbstractMalaria is a worldwide health issue, with 216 million cases reported in 2016. Due to the widespread resistance of Plasmodium falciparum to conventional drugs, the first line treatment recommended by World Health Organization for uncomplicated malaria is artemisinin-based combined therapy (ACT), which combines two drugs with different mechanisms of action. The association of artemether and lumefantrine is the most common ACT used in t...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 20, 2018 Category: Drugs & Pharmacology Source Type: research

Development of stability-indicating HPLC method and accelerated stability studies for osmotic and pulsatile tablet formulations of Clopidogrel Bisulfate
Publication date: 20 February 2019Source: Journal of Pharmaceutical and Biomedical Analysis, Volume 165Author(s): Priti R. Deshmukh, Vinod L. Gaikwad, Preeti K. Tamane, Kakasaheb R. Mahadik, Ravindra N. PurohitAbstractThe purpose of the present study is to develop a simple, rapid and sensitive stability-indicating high-performance liquid chromatography (HPLC) method for Clopidogrel Bisulfate (CBS) and further extending it for assessment of CBS stability in osmotic and pulsatile tablet formulations tested under accelerated conditions. A stability-indicating HPLC method for quantitative determination of CBS in gastro-retenti...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 20, 2018 Category: Drugs & Pharmacology Source Type: research

Isolation, identification, characterization, synthesis and quality control strategy of new process-related impurities in ambrisentan
Publication date: 20 February 2019Source: Journal of Pharmaceutical and Biomedical Analysis, Volume 165Author(s): Wei-Dong Feng, Song-Ming Zhuo, Fu-Li ZhangAbstractAmbrisentan is a highly selective endothelin-A receptor antagonist for the treatment of pulmonary arterial hypertension (PAH). The analysis of the process-related impurities will help not only to optimize the process parameters but also to develop reasonable analytical methods and set the quality standard for a quality control strategy in pharmaceutical manufacturing. During the manufacture of ambrisentan, five unknown impurities were detected in pilot batches r...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 20, 2018 Category: Drugs & Pharmacology Source Type: research

Zwitterionic-hydrophilic interaction liquid chromatography for l-ascorbic acid 2-phosphate magnesium, a raw material in cell therapy
Publication date: 20 February 2019Source: Journal of Pharmaceutical and Biomedical Analysis, Volume 165Author(s): Xiaolong Xu, Jonas Urlaub, Magdalena Woźniczka, Evelien Wynendaele, Karen Herman, Curd Schollmayer, Bernd Diehl, Serge Van Calenbergh, Ulrike Holzgrabe, Bart De SpiegeleerAbstractl-ascorbic acid 2-phosphate magnesium (APMg) salt is a vitamin C derivative frequently used in cell culture media for research purposes. It is also used as a raw material in the GMP-manufacturing of gene-, cell- and tissue advanced therapy medicinal products (ATMPs). However, quality methods are currently lacking. Therefore, a LC meth...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 20, 2018 Category: Drugs & Pharmacology Source Type: research

Metabolic profiling analysis of corilagin in vivo and in vitro using high-performance liquid chromatography quadrupole time-of-flight mass spectrometry
This study is first report to identify phase II conjugate metabolites (except mono-methylate conjugated metabolites) of pure Ellagitannin and distribution of these metabolites in vivo. In addition, clear, detailed metabolic pathways of corilagin were shown to involve hydrolysis, methylation, glycosylation, reduction, glucuronidation and sulfation. (Source: Journal of Pharmaceutical and Biomedical Analysis)
Source: Journal of Pharmaceutical and Biomedical Analysis - December 20, 2018 Category: Drugs & Pharmacology Source Type: research

Simultaneous determination of vancomycin and creatinine in plasma applied to volumetric absorptive microsampling devices using liquid chromatography-tandem mass spectrometry
Publication date: 20 February 2019Source: Journal of Pharmaceutical and Biomedical Analysis, Volume 165Author(s): Nadine B. Andriguetti, Letícia L. Lisboa, Siomara R. Hahn, Lidiane R. Pagnussat, Marina V. Antunes, Rafael LindenAbstractVancomycin (VCM) is a glycopeptide antibiotic, widely used against methicillin-resistant Staphylococcus aureus infections, and its clearance is highly correlated to creatinine (CRE) clearance. Usually, VCM and CRE levels are measured in serum or plasma specimens obtained from venous blood, after phlebotomy. As the majority of hospitals in Developing Countries do not have on-site access...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 20, 2018 Category: Drugs & Pharmacology Source Type: research

Use of ESI-MS for semi-quantitative estimation of inactive precursor in no-carrier-added 131I- meta-Iodobenzylguanidine radiopharmaceutical preparation
Publication date: 20 February 2019Source: Journal of Pharmaceutical and Biomedical Analysis, Volume 165Author(s): Anupam Mathur, Soumen Das, Navin Sakhare, S.S. SachdevAbstractNo-carrier-added (nca)-131I-meta-Iodobenzylguadine (mIBG) is a clinical agent used for the therapy of Neuroendocrine tumors. It is prepared by reaction of radioiodine with precursors that are chemically different from mIBG. The precursor in few cases is structurally similar and may co-elute along during purification step. Presence of these precursors in final radiolabeled formulation may affect the clinical behaviour of the radiopharmaceutical. The p...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 20, 2018 Category: Drugs & Pharmacology Source Type: research

Impurity profiling of anticancer preclinical candidate, IIIM-290
Publication date: Available online 18 December 2018Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Vikas Kumar, Deendyal Bhurta, Ankita Sharma, Puneet Kumar, Sandip B. Bharate, Ram A. Vishwakarma, Sonali S. BharateABSTRACTIIIM-290, an orally bioavailable preclinical candidate is effective in human xenograft models of leukemia, colon and pancreatic cancer. The promising preclinical data of this lead candidate has shown its potential for clinical development. As a part of its preclinical development, impurity profiling of pilot scale batches is one of the most important component of the CMC documentation....
Source: Journal of Pharmaceutical and Biomedical Analysis - December 19, 2018 Category: Drugs & Pharmacology Source Type: research

Survey of peptide quantification methods and comparison of their reproducibility: a case study using oxytocin
In this study, the HPLC assay method using the same peptide bulk material as the standard showed the lowest inter-lab variability. The coefficient of variation (%CV) was calculated without counting the uncertainty associated with the purity assignment of the standard with mass balance. The proton qNMR method is a direct measurement of the peptide against an internal standard, which is not difficult to perform under common laboratory conditions. Because of the simpler operation and shorter analytical time, qNMR as a primary method for peptide reference standard value assignment deserves further exploration. (Source: Journal...
Source: Journal of Pharmaceutical and Biomedical Analysis - December 19, 2018 Category: Drugs & Pharmacology Source Type: research