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Determination of estrone and 17α‐ethinylestradiol in digested sludge by ultrasonic liquid extraction and high‐performance liquid chromatography with fluorescence detection

Published: Feb 15, 2019

Author(s): Vitória L. Louros, Diana L.D. Lima, Jorge H. Leitão, Valdemar I. Esteves, Helena G. Nadais

Journal: Journal of Separation Science

Abstract Estrone, 17β‐estradiol and 17α‐ethinylestradiol are increasingly recognised as important micropollutants to be monitored in wastewater treatment plants. These estrogens are retained onto sludge due to their high adsorption and since they are largely used in land applications, the monitoring of these chemicals in sludge samples is of great importance. This study describes a method for the determination of estrone and 17α‐ethinylestradiol in fresh sludge samples. After spiking fresh...

thumbnail image: Determination of estrone and 17ethinylestradiol in digested sludge by ultrasonic liquid extraction and highperformance liquid chromatography with fluorescence detection

Fat suppression for ultrashort echo time imaging using a single‐point Dixon method

Published: Feb 15, 2019

Author(s): Hyungseok Jang, Michael Carl, Yajun Ma, Saeed Jerban, Tan Guo, Wei Zhao, Eric Y. Chang, Jiang Du

Journal: NMR in Biomedicine

Purpose In ultrashort echo time (UTE) imaging, fat suppression can improve short T2* contrast but can also reduce short T2* signals. The conventional two‐point Dixon (2p‐Dixon) method does not perform well due to short T2* decay. In this study, we propose a new method to suppress fat for high contrast UTE imaging of short T2 tissues, utilizing a single‐point Dixon (1p‐Dixon) method. Methods The proposed method utilizes dual‐echo UTE imaging, where UTE is followed by the second TE, chosen...

thumbnail image: Fat suppression for ultrashort echo time imaging using a singlepoint Dixon method

Ultra‐high‐pressure‐assisted extraction of wedelolactone and isodemethylwedelolactone from Ecliptae Herba and purification by high‐speed counter‐current chromatography

Published: Feb 15, 2019

Author(s): Hongwei Zhao, Supan Cheng, Longfei Zhang, Hongjing Dong, Yongqing Zhang, Xiao Wang

Journal: Biomedical Chromatography

Abstract Ultra‐high‐pressure extraction combined with high‐speed counter‐current chromatography was employed to extract and purify wedelolactone and isodemethylwedelolactone from Ecliptae Herba. The operating conditions of ultra‐high‐pressure extraction were optimized using an orthogonal experimental design. The optimal conditions were 80% aqueous methanol solvent, 200 MPa pressure, 3 min extraction time and 1:20 (g/mL) solid–liquid ratio for extraction of wedelolactone and...

thumbnail image: Ultrahighpressureassisted extraction of wedelolactone and isodemethylwedelolactone from Ecliptae Herba and purification by highspeed countercurrent chromatography

Determination of a novel antifibrotic small molecule GDC‐3280 in human plasma and urine by liquid chromatography tandem mass spectrometry to support its first‐in‐human clinical trial

Published: Feb 15, 2019

Author(s): Jianshuang Wang, Michael Van Parys, Lin Pan, Yuan Chen, Dorothy Cheung, Janine McKnight, Dennis Milanowski, Xiao Ding, Brian Dean

Journal: Biomedical Chromatography

Abstract A specific and robust LC–MS/MS method was developed and validated for the quantitative determination of GDC‐3280 in human plasma and urine. The nonspecific binding associated with urine samples was overcome by the addition of CHAPS. The sample volume was 25 μL for either matrix, and supported liquid extraction was employed for analyte extraction. d6‐GDC‐3280 was used as the internal standard. Linear standard curves (R2 0.9956) were established from 5.00 to 5000 ng/mL in both...

thumbnail image: Determination of a novel antifibrotic small molecule GDC3280 in human plasma and urine by liquid chromatography tandem mass spectrometry to support its firstinhuman clinical trial

Microbial transformation of ambrisentan to its glycosides by Cunninghamella elegans

Published: Feb 15, 2019

Author(s): Rafaela Sponchiado, Julia Medeiros Sorrentino, Natália Olegário, Sendy Sales Oliveira, Leticia Malgarim Cordenonsi, Gustavo Pozza Silveira, Alexandre M. Fuentefria, Andreas S. L. Mendez, Martin Steppe, Cássia V. Garcia

Journal: Biomedical Chromatography

Abstract The purpose of this paper is to describe the glycosylation of ambrisentan (AMB) by cultures of Cunninghamella elegans ATCC 9245. AMB is an endothelin receptor antagonist, which is used to treat pulmonary arterial hypertension. Filamentous fungi are morphologically complex and may exhibit different forms depending on the species and the nature of the culture medium. A biotransformation study was conducted to investigate the ability of C. elegans to metabolize AMB. Parameters were...

thumbnail image: Microbial transformation of ambrisentan to its glycosides by Cunninghamella elegans

Characterization and screening of metals, metalloids and biomarkers in crude oil by ICP–MS/OES, and GC–MS techniques after digestion by microwave‐induced combustion

Published: Feb 15, 2019

Author(s): Abdul Karim‐Talaq Mohammad, Abdullah Thamer Hameed, Mohammed Affan Alhamdany, Khaldun Mohammad Al Azzam, Gaidaa Abd Alkareem Talk

Journal: Biomedical Chromatography

Abstract A method for digestion of light and medium Iraqi crude oils (Basrah and Khanaken oils) using microwave‐induced combustion (MIC) in closed vessels is described for the determination of Hg, Au, Cu, Al, Ca, Co, K, Mg, Si and Sr by inductively coupled plasma optical emission spectrometry (ICP–OES) and Mo, Ti, Mn, Li, Se−1, Rb, Ag, Ba, Pb, As, Cd, Cr, Fe, Ni, V and Zn by inductively coupled plasma mass spectrometry (ICP–MS). Upon using MIC it was possible to obtain lower limits of...

thumbnail image: Characterization and screening of metals metalloids and biomarkers in crude oil by ICPMSOES and GCMS techniques after digestion by microwaveinduced combustion

Evaluation of ForenSeq™ Signature Prep Kit B on predicting eye and hair coloration as well as biogeographical ancestry by using Universal Analysis Software (UAS) and available web‐tools

Published: Feb 15, 2019

Author(s): Vishakha Sharma, Krupa Jani, Pavan Khosla, Erin Butler, Donald Siegel, Elisa Wurmbach

Journal: ELECTROPHORESIS

Abstract This study examined 266 individuals from various populations including African American, East Asian, South Asian, European, and mixed populations to evaluate the ForenSeq™ Signature Prep Kit Primer Mix B. Focus was placed on phenotypic and biogeographical ancestry predictions by Illumina's Universal Analysis Software (UAS). These outcomes were compared to those obtained through web‐tools developed at the Erasmus Medical Center (EMC) and available from the Forensic Resource/Reference...

thumbnail image: Evaluation of ForenSeq Signature Prep Kit B on predicting eye and hair coloration as well as biogeographical ancestry by using Universal Analysis Software UAS and available webtools

Count‐rate, linearity, and performance of new backgammon detector technology

Published: Feb 14, 2019

Author(s): Hamish A. Melia, Jonathan W. Dean, Lucas F. Smale, Alexis J. Illig, Christopher T. Chantler

Journal: X-Ray Spectrometry

The meander wire backgammon technology has high levels of flux and spatial linearity across a wide range of energies. One of the attractive features of these technologies is the stability of response and robustness under long X‐ray exposure, compactness, and portability. A key problem historically has been the limited range of count‐rate for processing to the optimum resolution. We report dramatic advances in this and other areas appropriate for high‐accuracy experiments including tests of...

thumbnail image: Countrate linearity and performance of new backgammon detector technology

X‐ray fluorescence analysis of samples simulating blood collected from uranium‐contaminated wounds

Published: Feb 14, 2019

Author(s): Yukie Izumoto, Tsugufumi Matsuyama, Kota Ishii, Yasuhiro Sakai, Yoshiyuki Oguri, Hiroshi Yoshii

Journal: X-Ray Spectrometry

Personnel working in nuclear fuel handling facilities incur a finite risk of injury and uranium contamination in any resulting wounds. The accidental absorption of uranium from the likes of wounds can lead to a significant degree of internal exposure due to its hazardous nature. Although an appropriate surgical resection of tissue in the contaminated wound is useful for suppressing the additional intake of uranium, the rapid quantification of uranium in the wound is required to avoid...

thumbnail image: Xray fluorescence analysis of samples simulating blood collected from uraniumcontaminated wounds

Sensitive detection of hydroxymethylcytosine levels in normal and neoplastic cells and tissues

Published: Feb 14, 2019

Author(s): Annette M. Krais, Yoon Jung Park, Guido Reifenberger, Michael Meister, Christoph Plass, Heinz H. Schmeiser

Journal: ELECTROPHORESIS

Abstract A new sensitive analytical method using capillary electrophoresis with laser induced fluorescence (CE‐LIF) was applied for the simultaneous detection of DNA methylation and hydroxymethylation levels in human cancers of different origin. DNA hydroxymethylation, measured as 5‐hydroxymethylcytosine (5hmC) levels, was decreased in gliomas with mutation in the isocitrate dehydrogenase 1 (IDH1) gene when compared to IDH1‐wildtype gliomas. Independent from IDH1 mutation, 5hmC levels were...

thumbnail image: Sensitive detection of hydroxymethylcytosine levels in normal and neoplastic cells and tissues

Redox Proteomic Analysis Reveals Oxidative Modifications of Proteins by Increased Levels of Intracellular Reactive Oxygen Species during Hypoxia Adaptation of Aspergillus fumigatus

Published: Feb 13, 2019

Author(s): Elena Shekhova, Lia Ivanova, Thomas Krüger, Maria C. Stroe, Juliane Macheleidt, Olaf Kniemeyer, Axel A. Brakhage

Journal: PROTEOMICS

Abstract Aspergillus fumigatus faces abrupt changes in oxygen concentrations at the site of infection. An increasing number of studies has demonstrated that elevated production of intracellular reactive oxygen species (ROS) under low oxygen conditions plays a regulatory role in modulating cellular responses for adaptation to hypoxia. To learn more about this process in A. fumigatus, intracellular ROS production during hypoxia has been determined. The results confirm increased amounts of...

thumbnail image: Redox Proteomic Analysis Reveals Oxidative Modifications of Proteins by Increased Levels of Intracellular Reactive Oxygen Species during Hypoxia Adaptation of Aspergillus fumigatus

Identification of Rabbit Oviductal Fluid Proteins Involved in Pre‐Fertilization Processes by Quantitative Proteomics

Published: Feb 13, 2019

Author(s): Hans Yu, Lena Hackenbroch, Florian R. L. Meyer, Judith Reiser, Ebrahim Razzazi‐Fazeli, Katharina Nöbauer, Urban Besenfelder, Claus Vogl, Gottfried Brem, Corina Mayrhofer

Journal: PROTEOMICS

Abstract Oviductal fluid (ODF) proteins modulate and support reproductive processes in the oviduct. In the present study, proteins involved in the biological events that precede fertilization have been identified in the rabbit ODF proteome, isolated from the ampulla and isthmus of the oviduct at different time points within 8 h after intrauterine insemination. A workflow is used that integrates lectin affinity capture with stable‐isotope dimethyl labeling prior to nanoLC‐MS/MS analysis. In...

thumbnail image: Identification of Rabbit Oviductal Fluid Proteins Involved in PreFertilization Processes by Quantitative Proteomics

Cationic surfactant regulated synthesis of Au nanorods for sensitive detection of negatively charged colorants by surface‐enhanced Raman spectroscopy

Published: Feb 13, 2019

Author(s): Miao Qin, Pan Li, Xia Zhou, Jun Zhu, Hongyan Wang, Liangbao Yang

Journal: Journal of Raman Spectroscopy

Abstract Although surface‐enhanced Raman spectroscopy (SERS) has recently emerged as a powerful analytical tool, its widespread use is hindered by several inherent problems (e.g., low reproducibility) that need to be solved before further progress is possible. Herein, we used dodecyltrimethylammonium bromide (DTAB), N‐dodecyl‐N‐2‐hydroxyethyl‐N,N‐dimethylammonium bromide (C12HDAB), and N‐dodecyl‐N,N‐2‐dihydroxyethyl‐N‐methylammonium bromide (C12DHAB) as templates for the seed‐mediated growth...

thumbnail image: Cationic surfactant regulated synthesis of Au nanorods for sensitive detection of negatively charged colorants by surfaceenhanced Raman spectroscopy

In situ full view of the Portland cement hydration by confocal Raman microscopy

Published: Feb 13, 2019

Author(s): Manuel Torres‐Carrasco, Adolfo Campo, Miguel A. Rubia, Encarnación Reyes, Amparo Moragues, Jose F. Fernández

Journal: Journal of Raman Spectroscopy

Abstract The study of the hydration reactions of Portland cement is well documented by conventional techniques such as X‐ray diffraction, differential thermal and thermogravimetric analysis, or NMR, for instance. However, a complete view of all the phases present in the reactions is elusive. In this study, by using an in situ analysis through confocal Raman microscopy (CRM), the reaction of the initial phases (C2S, C3S, and C3A) to form new crystalline phases (portlandite, ettringite, and...

thumbnail image: In situ full view of the Portland cement hydration by confocal Raman microscopy

Metabolic profiling of synthetic cannabinoid 5F‐ADB by human liver microsome incubations and urine samples using high‐resolution mass spectrometry

Published: Feb 13, 2019

Author(s): Oya Yeter, Yeter Erol Ozturk

Journal: Drug Testing and Analysis

Abstract 5F‐ADB (methyl 2‐{[1‐(5‐fluoropentyl)‐1H‐indazole‐3‐carbonyl] amino}‐3,3‐dimethylbutanoate) is a frequently abused new synthetic cannabinoid that has been sold since at least the end of 2014 on the drug market and has been classified as an illicit drug in most European countries, as well as Turkey, Japan, and the United States. In this study, the in vitro metabolism of 5F‐ADB was investigated by using pooled human liver microsomes (HLMs) assay and liquid chromatography‐high‐resolution...

thumbnail image: Metabolic profiling of synthetic cannabinoid 5FADB by human liver microsome incubations and urine samples using highresolution mass spectrometry

Diagram, valence‐to‐core, and hypersatellite Kβ X‐ray transitions in metallic chromium

Published: Feb 13, 2019

Author(s): Faisal Zeeshan, Joanna Hoszowska, Jean‐Claude Dousse, Dimosthenis Sokaras, Tsu‐Chien Weng, Roberto Alonso‐Mori, Matjaz Kavčič, Mauro Guerra, Jorge Miguel Sampaio, Fernando Parente, Paul Indelicato, José Pires Marques, José Paulo Santos

Journal: X-Ray Spectrometry

We report on measurements of the Kβ diagram, valence‐to‐core (VtC), and hypersatellite X‐ray spectra induced in metallic Cr by photon single and double K‐shell ionization. The experiment was carried out at the Stanford Synchrotron Radiation Lightsource using the seven‐crystal Johann‐type hard X‐ray spectrometer of the beamline 6‐2. For the Kβ diagram and VtC transitions, the present study confirms the line shape features observed in previous works, whereas the Khβ hypersatellite transition was...

thumbnail image: Diagram valencetocore and hypersatellite K Xray transitions in metallic chromium

Advances in the histopathological characterization of breast tissue using combined X‐ray fluorescence and X‐ray diffraction data in a multivariate analysis approach

Published: Feb 13, 2019

Author(s): Eric M. Johnston, Erica Dao, Michael J. Farquharson

Journal: X-Ray Spectrometry

Previous studies have shown that the combination of X‐ray fluorescence and X‐ray diffraction data can be used as a histopathological characterization tool for breast tissue. Recent advances in energy‐dispersive X‐ray fluorescence techniques have allowed for benchtop systems to produce useful results in a reasonable time frame, allowing for clinical implementation to be realized. Using a polarized energy‐dispersive X‐ray fluorescence and energy‐dispersive X‐ray diffraction system optimized for...

Read More $thumbnail image: Advances in the histopathological characterization of breast tissue using combined Xray fluorescence and Xray diffraction data in a multivariate analysis approach$

Fe3O4/reduced graphene oxide‐carbon nanotubes composite for the magnetic solid‐phase extraction and HPLC determination of sulfonamides in milk

Published: Feb 13, 2019

Author(s): Yingying Feng, Xiaopeng Hu, Faqiong Zhao, Baizhao Zeng

Journal: Journal of Separation Science

Abstract A novel magnetic adsorbent Fe3O4/reduced graphene oxide‐carbon nanotubes, was prepared by one‐pot solvothermal synthesis method. It was characterized by scanning electron microscopy, X‐ray powder diffraction and vibrating sample magnetometry. The diameter of Fe3O4 microparticles was about 350 nm, which were covered by carbon nanotubes and reduced graphene oxide sheets, while carbon nanotubes inserted between the reduced graphene oxide sheets effectively prevented their aggregation....

thumbnail image: Fe3O4reduced graphene oxidecarbon nanotubes composite for the magnetic solidphase extraction and HPLC determination of sulfonamides in milk

DIY XES—development of an inexpensive, versatile, and easy to fabricate XES analyzer and sample delivery system

Published: Feb 13, 2019

Author(s): Scott C. Jensen, Brendan Sullivan, Daniel A. Hartzler, Yulia Pushkar

Journal: X-Ray Spectrometry

The application of X‐ray emission spectroscopy (XES) has grown substantially with the development of X‐ray free‐electron lasers, third and fourth generation synchrotron sources, and high‐power benchtop sources. By providing the high X‐ray flux required for XES, these sources broaden the availability and application of this method of probing electronic structure. As the number of sources increase, so does the demand for X‐ray emission detection and sample delivery systems that are cost...

thumbnail image: DIY XESdevelopment of an inexpensive versatile and easy to fabricate XES analyzer and sample delivery system

Recent studies of docking and molecular dynamics simulation for liquid‐phase enantioseparations

Published: Feb 12, 2019

Author(s): Paola Peluso, Alessandro Dessì, Roberto Dallocchio, Victor Mamane, Sergio Cossu

Journal: ELECTROPHORESIS

Abstract Liquid‐phase enantioseparations have been fruitfully applied in several fields of science. Various applications along with technical and theoretical advancements contributed to increase significantly the knowledge in this area. Nowadays, chromatographic techniques, in particular HPLC on chiral stationary phase, are considered as mature technologies. In the last thirty years, CE has been also recognized as one of the most versatile technique for analytical scale separation of...