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Journal of Pharmaceutical and Biomedical Analysis

Cristian Gómez-Canela, Teresa Sala-Comorera, Víctor Pueyo, Carlos Barata, Silvia Lacorte
Elderly people represent about the 15% of the total world population and often include a polymedicated age group with an average consumption of 5-10 pills per day. The main pharmaceuticals consumed are antianalgesics, antidiabetics, anti-parkinson compounds, anti-convulsants, drugs to treat constipation and drugs to treat cancer. In this study, we have developed a multiresidue method for the analysis of 44 selected pharmaceuticals prioritized according to the foremost consumption by the elderly in effluents from senior residences...
February 13, 2019: Journal of Pharmaceutical and Biomedical Analysis
Sara Tengattini, Federica Corana, Davide Bianchi, Giorgio Marrubini, Raffaella Colombo, Sandra Furlanetto, Marco Terreni, Caterina Temporini
A liquid chromatographic MS-compatible method was applied to the structural elucidation of Teicoplanin for identification CRS components. The method, previously developed by our group, involves the use of LiChrospher 100 RP-18 column with a mobile phase composed of ammonium formate 25 mM at pH 6.00 and acetonitrile (ACN). All the peaks with a 0.10% UV area, largely above the disregard limit of 0.15% as fixed by EMA, were considered and submitted to MS/MS fragmentation experiments. The study of MS/MS spectrum collected for Teicoplanin complex major component (namely A2-2 ) allowed to elucidate the fragmentation pathway and enabled the successful identity assignment of all the 42 detected species...
February 13, 2019: Journal of Pharmaceutical and Biomedical Analysis
Zhenqun Li, Jia Wu, Li Jia
Detection of amino acids (AAs) in blood is helpful to diagnose some diseases. In this work, a method is developed for determination of trace amounts of AAs in bovine blood by combining solid phase extraction (SPE) and capillary electrophoresis (CE). Zeolitic imidazolate framework-8 (ZIF-8) nanoparticles are prepared and used as adsorbents to simultaneously extract three AAs (tryptophan, tyrosine, phenylalanine). Under the optimum extraction conditions, the extraction efficiencies of ZIF-8 for AAs are 95.1% (tryptophan), 91...
February 13, 2019: Journal of Pharmaceutical and Biomedical Analysis
Thi Phuong Duyen Vu, Trong Quan Khong, Thi Minh Nguyet Nguyen, Young Ho Kim, Jong Seong Kang
Syzygium formosum (SF) leaves have been used for thousands of years in traditional Vietnamese medicine for the treatment of allergy or skin rash. However, the role of the phytochemical profile of SF leaves on their activities is poorly understood. Additionally, there is currently no quality control method for this herbal material, which is required by the pharmaceutical industry. Therefore, this study aimed to investigate chemical profile of SF leaves using high-performance liquid chromatography-photodiode array-tandem mass spectrometry (HPLC-PDA-ESI-MS/MS) and establish a simple and efficient HPLC method for controlling major bioactive compounds...
February 11, 2019: Journal of Pharmaceutical and Biomedical Analysis
Na Guo, Yi-Wei Jiang, Ping Kou, Zhi-Ming Liu, Thomas Efferth, Yan-Yan Li, Yu-Jie Fu
A simple and efficient method based on cloud point extraction and concentration combined with high performance liquid chromatography was developed for the simultaneous separation and determination of five target compounds (deoxynojirimycin, chlorogenic acid, rutin, isoquercitrin and astragalin) in mulberry leaves samples. Firstly, to obtain a high extraction rate, the ultrasound assisted extraction was developed on acid modified Triton X-114 system. Under the optimal conditions, the total maximum extraction yields of five target compounds reached 20...
February 10, 2019: Journal of Pharmaceutical and Biomedical Analysis
Elumalai Sambandan, Thenmozhi Kathavarayan, Senthilkumar Sellappan, Jentaie Shiea, Vinoth Kumar Ponnusamy
The present study focuses on identifying the degradation profile and pathways of unknown impurities from beclomethasone dipropionate (BDP) topical cream formulation reported under accelerated stability conditions. Six degradation impurities were observed during the accelerated stability testing of BDP topical cream formulation, and these thermally labile degradation impurities were primarily identified using a simple, effective and mass compatible isocratic reversed-phase high-performance liquid chromatography with ultraviolet detection method...
February 10, 2019: Journal of Pharmaceutical and Biomedical Analysis
Joshua Rutowski, Fanyi Zhong, Mengyang Xu, Jiangjiang Zhu
Traditional strategies in developing novel drugs to treat antibiotic-resistant S. aureus have not been very successful to date, therefore, there is an urgent need for creative usage of existing agents that can treat and control S. aureus infection. This study demonstrated that a combination of glucose and a sublethal dose of antibiotic can reduce the survivability of S. aureus in a glucose concentration-dependent manner. Mass spectrometry-based targeted metabolic profiling detected massive metabolic profile shift of both methicillin-susceptible and resistant S...
February 8, 2019: Journal of Pharmaceutical and Biomedical Analysis
John Meijer, Tom van den Berg, Robert Huls, Vincent Hofstede, Willem Niesing, Cas van den Beld, Walter Krauwinkel
Mirabegron is the first registered β3-adrenoceptor agonist for treatment of overactive bladder as an alternative to antimuscarinics. Previously four liquid chromatography-tandem mass spectrometry assays were published to determine mirabegron and eight metabolites (M5, M8, M11-M16) in human plasma. In order to support paediatric development, the assays were further optimized to reduce the required blood volume and increase the sensitivity. The assays were miniaturized by using 96-well supported liquid extraction plates (mirabegron, M5, M16) or 96-well mixed-mode cation exchange solid phase extraction plates (M8, M11-M15) and a more sensitive MS-system was used...
February 7, 2019: Journal of Pharmaceutical and Biomedical Analysis
Zeyun Li, Songfeng Zhao, Yongliang Yuan, Lizhen Zhang, Zhizhen Song, Xin Tian, Xiaojian Zhang
Motolimod (VTX-2337) is an agonist of toll-like receptor 8 (TLR8) with potential immune-stimulating and antineoplastic activities. The purpose of this study was to investigate the in vitro metabolic profiles of VTX-2337. The average in vitro T1/2 values were 6.93, 8.71, 7.39, 2.85, and 10.58 min in the liver microsomes of mouse, rat, dog, monkey and human respectively, suggesting that VTX-2337 suffered from extensive metabolism. The metabolites were further profiled and identified by using ultra-high performance liquid chromatography coupled with diode array detector and Q-Exactive-Orbitrap tandem mass spectrometer (UHPLC-DAD-Q-Exactive-Orbitrap-MS) operated in positive ion mode...
February 7, 2019: Journal of Pharmaceutical and Biomedical Analysis
Shengyuan Wu, Liai Lan, Jingjing Jiang, Xianting Ding, Chih-Ming Ho, Yuefen Lou, Guorong Fan
Tuberculosis is one of the top concerns in the world and acutely threatens human health. A new potent candidate regimen containing pyrazinamide (PZA), ethambutol (EMB), protionamide (PTO) and clofazimine (CFZ) was proposed by Parabolic Response Surface/Feedback System Control (FSC/PRS) system and showed excellent outcomes in vitro and vivo studies. Here, a convenient liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) method was developed for the simultaneously determination of four compounds in beagle dog plasma...
February 6, 2019: Journal of Pharmaceutical and Biomedical Analysis
Ziwei Li, Jun Zhang, Yufeng Zhang, Zhong Zuo
Simvastatin is known as a pro-drug, which could be hydrolyzed by esterases to its active form, simvastatin acid. Although pharmacokinetics of simvastatin and simvastatin acid have been widely studied, hydrolysis of simvastatin to simvastatin acid during blood sampling and plasma preparation has been overlooked in the previous studies, leading to underestimation of simvastatin concentration and overestimation of simvastatin acid concentration in plasma. Since both efficacy and adverse drug reaction of simvastatin are highly dependent on simvastatin and simvastatin acid concentrations in vivo, accurate assessment of the two compounds are critical in their pharmacokinetic and pharmacodynamic studies...
February 6, 2019: Journal of Pharmaceutical and Biomedical Analysis
Huang-Qin Zhang, Pei Liu, Jin-Ao Duan, Ling Dong, Er-Xin Shang, Da-Wei Qian, Ping Xiao, Ming Zhao, Wei-Wen Li
Trichosanthin (root of Trichosanthes kirilowii Maxim.) has received much attention, but T. kirilowii has received little systematic analysis. A comprehensive evaluation of flavones and triterpenes in nine different parts of T. kirilowii would, thus, be of value to fully understand the potential medicinal properties of T. kirilowii. A hierarchical extraction-simultaneous determination method was established, which based on different types of components had different response on the MS detector. The hierarchical extraction method extracted 3, 29-dibenzoyl rarounitriol solely, which response lowly on the MS detector in the mixture of one step extract, in order to obtain accurate results in the next UHPLC-MS/MS assay...
February 6, 2019: Journal of Pharmaceutical and Biomedical Analysis
Jaewan Jung, Kyunghoon Lee, Jongwon Oh, Rihwa Choi, Hye In Woo, Hyung-Doo Park, Cheol-In Kang, Yae-Jean Kim, Soo-Youn Lee
Teicoplanin is a glycopeptide antibiotic used for treatment of severe Gram-positive bacterial infection. The aim of this study was to develop and validate a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for therapeutic drug monitoring (TDM) of teicoplanin and to review our clinical experience. We established an LC-MS/MS method to analyze serum concentration of teicoplanin using simple protein precipitation with a 5 min run time for each sample. The linearity, lower limit of quantitation, detection accuracy, precision, carryover, matrix effect, and extraction recovery were evaluated...
February 4, 2019: Journal of Pharmaceutical and Biomedical Analysis
Jing Chen, Chao Ye, Xiaomin Hu, Caihua Huang, Zheng Yang, Pengyang Li, Aiming Wu, Xiaolin Xue, Donghai Lin, Huimin Yang
Dyslipidemia is known as a common clinical disease that affects the health of millions of people around the world. The treatment of dyslipidemia with traditional Chinese medicine (TCM) is generally based on the accurate identification of disease syndromes. TCM syndromes are judged by traditional four-diagnosis method, which is subjective and fuzzy. Additionally, the judgment of TCM syndromes highly depend on doctors' own clinical experience. In this present study, we used nuclear magnetic resonance (NMR)-based serum metabolomics patterns to figure out the metabolic characteristics of different syndromes in patients with dyslipidemia...
February 4, 2019: Journal of Pharmaceutical and Biomedical Analysis
Bharathi Avula, Amar G Chittiboyina, Ji-Yeong Bae, Saqlain Haider, Yan-Hong Wang, Mei Wang, Jianping Zhao, Patricia A Deuster, Ikhlas A Khan
A previously unidentified purported botanical ingredient was found in dietary supplements marketed for anabolic benefits. In an attempt to assess the 'naturalness' of a group of steroid-like compounds called laxogenins, a UHPLC-QToF method was developed. Several dietary supplements claim to contain 5α-hydroxy laxogenin, which is a derivative of a naturally occurring spirostane-type steroid, laxogenin. Although laxogenin has been isolated from the rhizomes of Smilax sieboldii, 5α-hydroxy laxogenin has not been isolated or reported from any natural source...
February 1, 2019: Journal of Pharmaceutical and Biomedical Analysis
Amruta Tambe, Priyankai Mokashi, Nancy Pandita
Acetyl- Keto-β-boswellic acid (AKBA) is a pentacyclic triterpenic acid found in gum resin of Boswellia serrata. Even though it is shown to have anti-inflammatory activity, its bioavailability gets limited due to its poor aqueous solubility and permeability. The present study, hence, deals in enhancement of the intestinal absorption of AKBA from total boswellic acid fraction (TA fraction) using cyclodextrin (CD) and poloxamer solid dispersion (PXM SDs) formulations. Absorption studies were performed using the everted gut sac model prepared from rat jejunum...
February 1, 2019: Journal of Pharmaceutical and Biomedical Analysis
Natalia Korytowska, Aleksandra Wyczałkowska-Tomasik, Agnieszka Wiśniewska, Leszek Pączek, Joanna Giebułtowicz
p-Cresol is a protein-bound uremic retention solute that originates in the intestine through bacterial metabolism and accumulates throughout the body in case of kidney failure. To date, there has been no method to analyze unconjugated p-cresol concentration in the blood with a limit of detection lower than 75 pg. Thus, the aim of this study was to develop and validate a novel liquid chromatography-tandem mass spectrometry method for the determination of unconjugated p-cresol in plasma with a lower detection limit than what has been determined using previously described methods...
January 31, 2019: Journal of Pharmaceutical and Biomedical Analysis
Amy Smart, Ben de Lacy Costello, Paul White, Matthew Avison, Claire Batty, Claire Turner, Raj Persad, Norman Ratcliffe
Antibiotic resistance is set to be an unprecedented threat to modern medicine. 'Sniffing' bacteria potentially offers a rapid way to determine susceptibility. A successful proof-of-principle study is described, using thermal desorption-gas chromatography-mass spectrometry (TDGCMS) to 'smell' cephalexin and ciprofloxacin resistant and sensitive Urinary Tract Infection (UTI)-causing bacteria. 578 peaks at unique retention times were detected from 86 chromatograms of 18 bacterial isolates (E. coli, K. pneumoniae and P...
January 31, 2019: Journal of Pharmaceutical and Biomedical Analysis
V V S R N Anji Karun Mutha, V V RavichandraReddy, Prabhakar S Achanta, Deviprasad Rendedula, Chakravarthy Chandra, Nagul Meera Shaik, Muralidharan Kaliyaperumal, Raghu Babu Korupolu, Susheela Bai Gajbhiye, Chidananda Swamy Rumalla
Thiocolchicoside is a natural product analogue often used for its spasmolytic action. To know more about its stability under various stress conditions, the drug was stirred in acid, base and peroxide solutions. In acid hydrolysis, two products were obtained and in both, the glucose got cleaved. In one of them the acetyl group also got cleaved. A set of two diastereomers were formed during the peroxide mediated hydrolysis. The base mediated hydrolysis resulted in formation of three novel degradants. They have six membered rings in their structures instead of a seven membered cycloheptatrienone...
January 31, 2019: Journal of Pharmaceutical and Biomedical Analysis
Mariana Gallo, Sara Matteucci, Nadine Alaimo, Erica Pitti, Maria V Orsale, Vincenzo Summa, Daniel O Cicero, Edith Monteagudo
A new methodology based on Nuclear Magnetic Resonance (NMR) was developed to determine plasma protein binding (PPB) of drug candidates in drug discovery programs. A strong correlation was found between the attenuation of NMR signals of diverse drugs in the presence of different plasma concentrations and their fraction bound (fb ) reported in the literature. Based on these results, a protocol for a rapid calculation of fb of small molecules was established. The advantage of using plasma instead of purified recombinant proteins and the possibility of pool analysis to increase throughput were also evaluated...
January 31, 2019: Journal of Pharmaceutical and Biomedical Analysis
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