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Luisa Matos Do Canto, Catalin Marian, Rency S Varghese, Jaeil Ahn, Patricia A Da Cunha, Shawna Willey, Mary Sidawy, Janice D Rone, Amrita K Cheema, George Luta, Mohammad R Nezami Ranjbar, Habtom W Ressom, Bassem R Haddad
Identification of new biomarkers for breast cancer remains critical in order to enhance early detection of the disease and improve its prognosis. Towards this end, we performed an untargeted metabolomic analysis of breast ductal fluid using an ultra-performance liquid chromatography coupled with a quadrupole time-of-light (UPLC-QTOF) mass spectrometer. We investigated the metabolomic profiles of breast tumors using ductal fluid samples collected by ductal lavage (DL). We studied fluid from both the affected breasts and the unaffected contralateral breasts (as controls) from 43 women with confirmed unilateral breast cancer...
October 13, 2016: International Journal of Oncology
Chiguru Vishnuvardhan, Saibaba Baikadi, Roshan M Borkar, R Srinivas, N Satheeshkumar
Silodosin (SLD) is a novel α1-adrenoceptor antagonist which has shown promising clinical efficacy and safety in patients with benign prostatic hyperplasia (BPH). However, lack of information about metabolism of SLD prompted us to investigate metabolic fate of SLD in rats. To identify in vivo metabolites of SLD, urine, feces and plasma were collected from Sprague-Dawley rats after its oral administration. The samples were prepared using an optimized sample preparation approach involving protein precipitation followed by solid-phase extraction and then subjected to LC/HR-MS/MS analysis...
October 2016: Journal of Mass Spectrometry: JMS
Hong-Ping Wang, You-Bo Zhang, Xiu-Wei Yang, Da-Qing Zhao, Ying-Ping Wang
BACKGROUND: Ginsenosides are the characteristic and principal components which manifest a variety of the biological and pharmacological activities of the roots and rhizomes of Panax ginseng (GRR). This study was carried out to qualitatively and quantitatively determine the ginsenosides in the cultivated and forest GRR. METHODS: A rapid and sensitive ultra-high-performance liquid chromatography coupled with diode-array detector and quadrupole/time of flight tandem mass spectrometry (UPLC-DAD-QTOF-MS/MS) was applied to the qualitative analysis of ginsenosides and a 4000 QTRAP triple quadrupole tandem mass spectrometer (HPLC-ESI-MS) was applied to quantitative analysis of 19 ginsenosides...
October 2016: Journal of Ginseng Research
Xin-Fang Xu, Xian-Long Cheng, Qing-Hua Lin, Sha-Sha Li, Zhe Jia, Ting Han, Rui-Chao Lin, Dan Wang, Feng Wei, Xiang-Ri Li
BACKGROUND: Mountain-cultivated ginseng (MCG) and cultivated ginseng (CG) both belong to Panax ginseng and have similar ingredients. However, their pharmacological activities are different due to their significantly different growth environments. METHODS: An ultra-performance liquid chromatography/quadrupole time-of-flight mass spectrometry (UPLC-QTOF-MS/MS)-based approach was developed to distinguish MCG and CG. Multivariate statistical methods, such as principal component analysis and supervised orthogonal partial-least-squares discrimination analysis were used to select the influential components...
October 2016: Journal of Ginseng Research
Kathrin Stavenhagen, Hannes Hinneburg, Daniel Kolarich, Manfred Wuhrer
The vast heterogeneity of protein glycosylation, even of a single glycoprotein with only one glycosylation site, can give rise to a set of macromolecules with different physicochemical properties. Thus, the use of orthogonal approaches for comprehensive characterization of glycoproteins is a key requirement. This chapter describes a universal workflow for site-specific N- and O-glycopeptide analysis. In a first step glycoproteins are treated with Pronase to generate glycopeptides containing small peptide sequences for enhanced glycosylation site assignment and characterization...
2017: Methods in Molecular Biology
Ramanujam Saravanan, Muthuvel Bharathselvi, Aravind C Babu, Jyothirmay Biswas, Konerirajapuram N Sulochana
PURPOSE: Eales' disease (ED), an enigmatic inflammatory disease affects peripheral retinal veins and thereby vision, in males. This study was aimed at identifying and deciphering the role of a novel 88 kDa protein reported in the serum and vitreous of patients with ED. EXPERIMENTAL DESIGN: The purified 88 kDa protein was identified by UPLC coupled ESI-QTOF-MS. The identified proteins were quantified in the serum from 20 ED patients and controls (age and sex matched), respectively by ELISA...
October 14, 2016: Proteomics. Clinical Applications
Andrea E Steuer, Elena Williner, Sandra Staeheli, Thomas Kraemer
Increasing numbers of new psychoactive substances (NPS) among them fentanyl derivatives has been reported by the European monitoring centre for drugs and drug addiction (EMCDDA). Butyrfentanyl is a new fentanyl derivative whose potency ratio was found to be seven compared to morphine and 0.13 compared to fentanyl. Several case reports on butyrfentanyl intoxications have been described. Little is known about its pharmacokinetic properties including its metabolism. However, knowledge of metabolism is essential for analytical detection in clinical and forensic toxicology...
October 13, 2016: Drug Testing and Analysis
Efficient N Ncube, Paul A Steenkamp, Ntakadzeni E Madala, Ian A Dubery
Centella asiatica is a perrenial herb that grows in tropical regions with numerous medicinal properties mostly attributed to the presence of pentacyclic triterpenoids. Interestingly, this plant also possess a significant amount of phenylpropanoid-derived chlorogenic acids (CGAs) that have recently been reported to confer neuroprotective properties. In a biotechnological attempt to increase the biosynthesis of CGA-derivatives in cultured Centella cells, acibenzolar-S-methyl was applied as a xenobiotic inducer in combination with quinic acid and shikimic acid as precursor molecules...
2016: Frontiers in Plant Science
Borbála Antal, Ákos Kuki, Lajos Nagy, Tibor Nagy, Miklós Zsuga, Márta M-Hamvas, Gábor Vasas, Sándor Kéki
Direct analysis in real time mass spectrometry (DART-MS) was applied as a rapid method for the discrimination of the spices and traditional medicines cumin (Cuminum cyminum L.), caraway (Carum carvi L.), and fennel (Foeniculum vulgare Mill.). The seeds of these plants were analyzed without sample preparation by DART ion source coupled with quadrupole time-of-flight (QTOF) tandem mass spectrometry. The relatively clean DART spectra showed characteristic patterns, fingerprints, for each herb. It was found that a marker compound can be assigned to each species that can identify unambiguously these plants...
2016: Analytical Sciences: the International Journal of the Japan Society for Analytical Chemistry
Jordyn M Wolfand, Gregory H LeFevre, Richard G Luthy
Fipronil is a recalcitrant phenylpyrazole-based pesticide used for flea/tick treatment and termite control that is distributed in urban aquatic environments via stormwater and contributes to stream toxicity. We discovered that fipronil is rapidly metabolized (t1/2 = 4.2 d) by the white rot fungus Trametes versicolor to fipronil sulfone and multiple previously unknown fipronil transformation products, lowering fipronil concentration by 96.5%. Using an LC-QTOF-MS untargeted metabolomics approach, we identified four novel fipronil fungal transformation products: hydroxylated fipronil sulfone, glycosylated fipronil sulfone, and two compounds with unresolved structures...
October 12, 2016: Environmental Science. Processes & Impacts
Yan Jiang, Feng-Jie Liu, Yu-Mei Wang, Hui-Jun Li
Although natural products (NPs) from ethnomedical plants have played a vital role in modern drug discovery, separation and purification of bioactive compounds from plant extract is still challenging. In this study, a dereplication strategy using HPLC-QTOF-MS was employed to rapidly discover and highly targeted isolate the novel hepatoprotective triterpenoid saponins from the methanol extract of Celosiae Semen. Firstly, four known saponins, i.e. celosin H, celosin I, celosin J, and pseudoginsenoside RT1 were selected as model compounds, and their fragmentation patterns in ESI-QTOF-MS/MS were characterized...
October 3, 2016: Journal of Pharmaceutical and Biomedical Analysis
Inamullah Hakeem Said, Rohan Lakshmidas Shah, Matthias S Ullrich, Nikolai Kuhnert
A liquid chromatography-mass spectrometry-based method for the quantification of intracellular concentrations of dietary phenolics in bacteria was developed. Using this assay, the time-dependent uptake of quercetin and two of its glycosides into gut microbiota model organisms (Escherichia coli and Bifidobacterium bifidum) under aerobic and anaerobic conditions was studied. For the first time, quantitative data on the uptake of dietary phenols were obtained indicating a time-dependent differential uptake of the dietary compounds...
September 14, 2016: Food & Function
M Gabriela Gallego, Tamara Rodríguez, Isaac Rodríguez, María Pilar Almajano
The extracts (0.5% [w/w]) from Caesalpinia spinosa or tara (CS) and Caesalpinia decapetala (CD) leaves were evaluated for their ability to inhibit lipid oxidation using oil-in-water (O/W) emulsions as the model system. Liquid chromatography (LC) combined with mass spectrometry (MS), using a hybrid quadrupole time-of-flight (QTOF) mass spectrometer, was employed for (1) the identification of potential antioxidant species in the extracts and (2) to follow their evolution through aging of the emulsions. CS extracts, containing esters and conjugated forms of gallic acid (GA), turned out to be more effective than CD, rich in flavonoid species, in stabilizing the O/W emulsions...
October 5, 2016: Journal of Food Science
Yinjun Yang, Xinguang Sun, Jinjun Liu, Liping Kang, Sibao Chen, Baiping Ma, Baolin Guo
A simple, accurate and reliable high performance liquid chromatography coupled with photodiode array detection (HPLC-DAD) method was developed and then successfully applied for simultaneous quantitative analysis of eight compounds, including chlorogenic acid (1), (R/S)-flavanomarein (2), butin-7-O-β-d-glucopyranoside (3), isookanin (4), taxifolin (5), 5,7,3',5'-tetrahydroxyflavanone-7-O-β-d-glucopyranoside (6), marein (7) and okanin (8), in 23 batches of snow chrysanthemum of different seed provenance and from various habitats...
September 30, 2016: Molecules: a Journal of Synthetic Chemistry and Natural Product Chemistry
Lingxi Li, Shuting Zhang, Yan Cui, Yuanyuan Li, Lanxin Luo, Peiyu Zhou, Baoshan Sun
In this work, an efficient method for preparative separation of procyanidins from raw cacao bean extract by high-speed counter-current chromatography (HSCCC) was developed. Under the optimized solvent system of n-hexane-ethyl acetate-water (1:50:50, v/v/v) with a combination of head-tail and tail-head elution modes, various procyanidins fractions with different polymerization degrees were successfully separated. UPLC, QTOF-MS and (1)H NMR analysis verified that these fractions contained monomer up to pentamer respectively...
September 27, 2016: Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences
Shuna Jin, Chengwu Song, Shuailong Jia, Sen Li, Yang Zhang, Cheng Chen, Yulin Feng, Yong Xu, Chaomei Xiong, Yi Xiang, Hongliang Jiang
Turmeric and curcuminoids are used as natural food coloring and functional food additives in various parts of the world. In this study, ninety-six curcuminoids were fully characterized using a targeted curcuminoid profile, which established by integrated use of two complementary LC-MS/MS platforms (liquid chromatography-quadrupole time of flight mass spectrometry (LC-QTOF-MS/MS) and liquid chromatography-quadrupole linear ion trap mass spectrometry (LC-QTRAP-MS/MS)). The curcuminoid profile was represented in the form of a multiple reaction monitoring (MRM) mode based on LC-QTRAP-MS/MS analysis...
September 27, 2016: Journal of Pharmaceutical and Biomedical Analysis
Vinod Bhatt, Sushila Sharma, Neeraj Kumar, Upendra Sharma, Bikram Singh
The current study presents isolation and characterization of twelve compounds including catechin (1), isovitexin (2), hesperidin (3), psoralin (4), eudesmin (5), kobusin (6), fargesin (7), sesamin (8), asarinin (9), planispine-A (10), α-sanshool (11) and vitexin (12), from the leaves of Zanthoxylum armatum. Further, two rapid and simple ultra performance liquid chromatography-diode array detection (UPLC-DAD) methods were developed for the simultaneous quantitative determination of isolated compounds from Z...
September 26, 2016: Journal of Pharmaceutical and Biomedical Analysis
Kevin S Jewell, Per Falås, Arne Wick, Adriano Joss, Thomas A Ternes
The biotransformation of diclofenac during wastewater treatment was investigated. Attached growth biomass from a carrier-filled compartment of a hybrid-MBBR at the wastewater treatment plant (WWTP) in Bad Ragaz, Switzerland was used to test the biotransformation. Laboratory-scale incubation experiments were performed with diclofenac and carriers and high-resolution LC-QTof-MS was implemented to monitor the biotransformation. Up to 20 diclofenac transformation products (TPs) were detected. Tentative structures were proposed for 16 of the TPs after characterization by MS(2) fragmentation and/or inferring the structure from the transformation pathway and the molecular formula given by the high resolution ionic mass...
November 15, 2016: Water Research
Radhiah Khairon, Noraziah Mohamad Zin, Mariati Abdul Rahman, Dayang Fredalina Basri
The aim of this study is to analyze the differential proteins in MRSA ATCC 33591 treated with aqueous extract from Q. infectoria gall. Protein extracts were obtained from MRSA cells by sonication and were separated by 2D polyacrylamide gels. Protein spots of interest were extracted from the gels and identified using LC-ESI-QTOF MS. The concentration of Q. infectoria extract used for 2D-gel electrophoresis was subinhibitory concentration. Minimum inhibitory concentration (MIC) value of the extract against MRSA was 19...
2016: International Journal of Proteomics
Draženka Stipaničev, Zrinka Dragun, Siniša Repec, Katerina Rebok, Maja Jordanova
Target screening of 463 organic contaminants in surface water using ultra high performance liquid chromatography quadrupole time-of-flight mass spectrometry (UHPLC-QTOF-MS) with direct injection was performed in spring of 2015 in northern Macedonia, at six sampling sites in four rivers belonging to Vardar basin: Kriva, Zletovska, Bregalnica and Vardar. The aim of the study was to differentiate between various types of organic contamination characteristic for different types of anthropogenic activities, such as mining, agriculture, and urbanization...
September 26, 2016: Ecotoxicology and Environmental Safety
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