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Study of the forced degradation behavior of prasugrel hydrochloride by liquid chromatography with mass spectrometry and liquid chromatography with NMR detection and prediction of the toxicity of the characterized degradation products

Published: Jul 31, 2015

Author(s): Dilip Kumar Singh, Archana Sahu, Tarun Handa, Mallikarjun Narayanam, Saranjit Singh

Journal: Journal of Separation Science

Prasugrel was subjected to forced degradation studies under conditions of hydrolysis (acid, base, and neutral), photolysis, oxidation, and thermal stress. The drug showed liability in hydrolytic as well as oxidative conditions, resulting in a total of four degradation products. In order to characterize the latter, initially mass fragmentation pathway of the drug was established with the help of mass spectrometry/time‐of‐flight, multiple...

Read More thumbnail image: Study of the forced degradation behavior of prasugrel hydrochloride by liquid chromatography with mass spectrometry and liquid chromatography with NMR detection and prediction of the toxicity of the characterized degradation products

Hollow‐fiber liquid‐phase microextraction coupled with miniature capillary electrophoresis for the trace analysis of four aliphatic aldehydes in water samples

Published: Jul 31, 2015

Author(s): Ying Li, Fan Yi, Yiliang Zheng, Yu Wang, Jiannong Ye, Qingcui Chu

Journal: Journal of Separation Science

An environmentally friendly method for the trace analysis of four aliphatic aldehydes as water disinfection byproducts has been developed based on hollow‐fiber liquid‐phase microextraction followed by miniature capillary electrophoresis with amperometric detection. After derivatization with 2‐thiobarbituric acid, four aliphatic aldehydes (formaldehyde, acetaldehyde, propylaldehyde, and butyraldehyde) became detectable by the amperometric...

Read More thumbnail image: Hollowfiber liquidphase microextraction coupled with miniature capillary electrophoresis for the trace analysis of four aliphatic aldehydes in water samples

Development of a method using high‐performance liquid chromatographic fingerprint and multi‐ingredients quantitative analysis for the quality control of Yangxinshi Pian

Published: Jul 31, 2015

Author(s): Yerui Li, Kai Yang, Qiyuan Shi, Bowen Liu, Ye Jin, Xuesong Liu, Zuolin Jiang, Lianjun Luan, Yongjiang Wu

Journal: Journal of Separation Science

A simple and reliable method of high‐performance liquid chromatography with diode array detection method was developed for fingerprint analysis and simultaneous determination of six compounds including puerarin, salvianolic acid B, berberine hydrochloride, palmatine chloride, dehydrocorydaline, and icariin in the Chinese medicine preparation Yangxinshi Pian. The separation was performed on an Agilent Eclipse XDB‐C18 reserved‐phase column...

Read More thumbnail image: Development of a method using highperformance liquid chromatographic fingerprint and multiingredients quantitative analysis for the quality control of Yangxinshi Pian

Development of an impurity‐profiling method for source identification of spilled benzene series compounds by gas chromatography with mass spectrometry: Toluene as a case study

Published: Jul 31, 2015

Author(s): Bin Han, Junhui Chen, Li Zheng, Tao Zhou, Jingxi Li, Xiaoru Wang, Jiangtao Wang

Journal: Journal of Separation Science

In this study, an impurity profiling method was established for the source identification of spilled benzene series compounds. Toluene was used as a case study to demonstrate the feasibility of this approach. Gas chromatography with mass spectrometry was applied for identification and quantification of the impurities including ethyl benzene, p‐xylene, m‐xylene, and o‐xylene in toluene. Impurities in toluene were detected at very low levels by...

Read More thumbnail image: Development of an impurityprofiling method for source identification of spilled benzene series compounds by gas chromatography with mass spectrometry Toluene as a case study

Dielectrophoretic immobilization of proteins: Quantification by atomic force microscopy

Published: Jul 30, 2015

Author(s): Eva‐Maria Laux, Xenia Knigge, Frank F. Bier, Christian Wenger, Ralph Hölzel

Journal: ELECTROPHORESIS

The combination of alternating electric fields with nanometer‐sized electrodes allows the permanent immobilization of proteins by dielectrophoretic force. Here, atomic force microscopy is introduced as a quantification method, and results are compared with fluorescence microscopy. Experimental parameters, for example the applied voltage and duration of field application, are varied systematically, and the influence on the amount of...

Read More thumbnail image: Dielectrophoretic immobilization of proteins Quantification by atomic force microscopy

Measurement of L subshell fluorescence yields of some rare earth elements using synchrotron radiation

Published: Jul 30, 2015

Author(s): Krishnananda, Santosh Mirji, Mutturaj Hosamani, N. M. Badiger, M. K. Tiwari, G. S. Lodha

Journal: X-Ray Spectrometry

The L subshell fluorescence yields ω1, ω2 and ω3 of Gd, Tb and Ho have been measured using Indus‐2 synchrotron radiation. The L X‐ray photons generated in the elemental targets by 10 and 11 keV synchrotron radiation have been measured using silicon drift detector that has an energy resolution of 130 eV at 5.9 keV. The measured values of ω1, ω2 and ω3 have been compared with theoretical values, semi‐empirical fitted values and other experimental...

Read More thumbnail image: Measurement of L subshell fluorescence yields of some rare earth elements using synchrotron radiation

Multielement analysis in serum of healthy population of the metropolitan region of Rio de Janeiro in Brazil by SRTXRF

Published: Jul 30, 2015

Author(s): Catarine G. L. Canellas, Silvia M. F. Carvalho, Roberta G. Leitão, Alfredo V. B. Bellido, Marcelino J. Anjos, Ricardo T. Lopes

Journal: X-Ray Spectrometry

The determination of multielemental concentrations in physiological fluids is of considerable interest in clinical chemistry. Since it has been established these levels in human serum can be utilized as indicators for several pathological conditions. The multielement composition determination in human serum is important for the investigation of their role in human physiology and metabolism. From this research, more detailed studies on the...

Read More thumbnail image: Multielement analysis in serum of healthy population of the metropolitan region of Rio de Janeiro in Brazil by SRTXRF

Multiparametric MRI as an early biomarker of individual therapy effects during concomitant treatment of brain tumours

Published: Jul 30, 2015

Author(s): Benjamin Lemasson, Audrey Bouchet, Cécile Maisin, Thomas Christen, Géraldine Le Duc, Chantal Rémy, Emmanuel L. Barbier, Raphaël Serduc

Journal: NMR in Biomedicine

The aim of this study was to determine the ability of multiparametric MRI to identify the early effects of individual treatment, during combined chemo‐radiotherapy on brain tumours. Eighty male rats bearing 9L gliosarcomas were randomized into four groups: untreated, anti‐angiogenic therapy (SORA group), microbeam radiation therapy (MRT group) and both treatments (MRT+SORA group). Multiparametric MRI (tumour volume,...

Read More thumbnail image: Multiparametric MRI as an early biomarker of individual therapy effects during concomitant treatment of brain tumours

Raman micro‐spectroscopy for quantitative thickness measurement of nanometer thin polymer films

Published: Jul 30, 2015

Author(s): Barbara M. Liszka, Aufried T. M. Lenferink, Geert‐Jan Witkamp, Cees Otto

Journal: Journal of Raman Spectroscopy

The sensitivity of far‐field Raman micro‐spectroscopy was investigated to determine quantitatively the actual thickness of organic thin films. It is shown that the thickness of organic films can be quantitatively determined down to 3 nm with an error margin of 20% and down to 1.5 nm with an error margin of 100%. Raman imaging of thin‐film surfaces with a far‐field optical microscope establishes the distribution of a polymer with a lateral...

Read More thumbnail image: Raman microspectroscopy for quantitative thickness measurement of nanometer thin polymer films

Concurrent determination of olanzapine, risperidone and 9‐hydroxyrisperidone in human plasma by ultra performance liquid chromatography with diode array detection method: application to pharmacokinetic study

Published: Jul 30, 2015

Author(s): M. Siva Selva Kumar, M. Ramanathan

Journal: Biomedical Chromatography

Abstract A simple and sensitive ultra‐performance liquid chromatography (UPLC) method has been developed and validated for simultaneous estimation of olanzapine (OLZ), risperidone (RIS) and 9‐hydroxyrisperidone (9‐OHRIS) in human plasma in vitro. The sample preparation was performed by simple liquid–liquid extraction technique. The analytes were chromatographed on a Waters Acquity H class UPLC system using isocratic mobile phase conditions at a...

Read More thumbnail image: Concurrent determination of olanzapine risperidone and 9hydroxyrisperidone in human plasma by ultra performance liquid chromatography with diode array detection method application to pharmacokinetic study

Resolution and quantification of arginine, monomethylarginine, asymmetric dimethylarginine, and symmetric dimethylarginine in plasma using HPLC with internal calibration

Published: Jul 30, 2015

Author(s): Matthew S. Alkaitis, Glenn Nardone, Jessica H. Chertow, Hans C. Ackerman

Journal: Biomedical Chromatography

Abstract NG,NG‐dimethyl‐l‐arginine (asymmetric dimethylarginine, ADMA),NG‐monomethyl‐l‐arginine (l‐NMMA) and NG,NG’‐dimethyl‐l‐arginine (symmetric dimethylarginine, SDMA) are released during hydrolysis of proteins containing methylated arginine residues. ADMA and l‐NMMA inhibit nitric oxide synthase by competing with l‐arginine substrate. All three methylarginine derivatives also inhibit arginine transport. To enable investigation of methylarginines ...

Read More thumbnail image: Resolution and quantification of arginine monomethylarginine asymmetric dimethylarginine and symmetric dimethylarginine in plasma using HPLC with internal calibration

The profiling and identification of the metabolites of 8‐prenylkaempferol and a study on their distribution in rats by high‐performance liquid chromatography with diode array detection combined with electrospray ionization ion trap time‐of‐flight multistage mass spectrometry

Published: Jul 29, 2015

Author(s): Li‐Man Ma, Feng Xu, Feng‐Chun Li, Jing‐Zhe Wang, Ming‐Ying Shang, Guang‐Xue Liu, Shao‐Qing Cai

Journal: Biomedical Chromatography

Abstract 8‐Prenylkaempferol is a prenylflavonoid that has various bioactivities and benefits for human health. A high‐performance liquid chromatography with a diode array detector combined with electrospray ionization ion trap time‐of‐flight multistage mass spectrometry (HPLC‐DAD‐ESI‐IT‐TOF‐MSn) method was established to profile and identify the metabolites of 8‐prenylkaempferol in rat in vivo and in vitro, and to study the distribution of...

Read More thumbnail image: The profiling and identification of the metabolites of 8prenylkaempferol and a study on their distribution in rats by highperformance liquid chromatography with diode array detection combined with electrospray ionization ion trap timeofflight multistage mass spectrometry

Aptamer‐based detection and quantitative analysis of human immunoglobulin E in capillary electrophoresis with chemiluminescence detection

Published: Jul 29, 2015

Author(s): Yan‐Ming Liu, Jun‐Tao Cao, Ying‐Ying Liu, Jing‐Jing Zhang, Min Zhou, Ke‐Jing Huang, Yong‐Hong Chen, Shu‐Wei Ren

Journal: ELECTROPHORESIS

A novel aptamer‐based CE with chemiluminescence (CL) assay was developed for highly sensitive detection of human immunoglobulin E (IgE). The IgE aptamer was conjugated with gold nanoparticles (AuNPs) to form AuNPs‐aptamer that could specifically recognize the IgE to produce an AuNPs‐aptamer‐IgE complex. The mixture of the AuNPs‐aptamer‐IgE complex and the unbounded AuNPs‐aptamer could be effectively separated by CE and sensitively...

Read More thumbnail image: Aptamerbased detection and quantitative analysis of human immunoglobulin E in capillary electrophoresis with chemiluminescence detection

Quantitative NMRI and NMRS identify augmented disease progression after loss of ambulation in forearms of boys with Duchenne muscular dystrophy

Published: Jul 27, 2015

Author(s): Claire Wary, Noura Azzabou, Céline Giraudeau, Julien Le Louër, Marie Montus, Thomas Voit, Laurent Servais, Pierre Carlier

Journal: NMR in Biomedicine

Quantitative NMRI and 31P NMRS indices are reported in the forearms of 24 patients with Duchenne muscular dystrophy (DMD) (6–18 years, 14 non‐ambulant) amenable to exon 53 skipping therapy and in 12 age‐matched male controls (CONT). Examinations carried out at 3 T comprised multi‐slice 17‐echo measurements of muscle water T2 and heterogeneity, three‐point Dixon imaging of fat fraction in flexor and extensor muscles (FLEX, EXT), and non‐localised ...

Read More thumbnail image: Quantitative NMRI and NMRS identify augmented disease progression after loss of ambulation in forearms of boys with Duchenne muscular dystrophy

Study of the spectro‐chemical signatures of cobalt–manganese layered oxides (asbolane–lithiophorite and their intermediates) by Raman spectroscopy

Published: Jul 27, 2015

Author(s): C. Burlet, Y. Vanbrabant

Journal: Journal of Raman Spectroscopy

In this study, Raman microspectroscopy is applied to investigate two manganese oxide phases: lithiophorite [(Al,Li)Mn4+O2(OH)2] and asbolane [(Ni,Co)xMn4+(O,OH)4·nH2O], along with their intermediates (‘asbolane–lithiophorite intermediates’: ALI). These oxides typically incorporate variable concentrations of Co, Ni, Cu and Li. They represent a group of economically interesting phases that are difficult to identify and characterize with classical X‐ray...

Read More thumbnail image: Study of the spectrochemical signatures of cobaltmanganese layered oxides asbolanelithiophorite and their intermediates by Raman spectroscopy

In situ ambient and high‐temperature Raman spectroscopic studies of nyerereite (Na,K) 2 Ca(CO 3 ) 2 : can hexagonal zemkorite be stable at earth‐surface conditions?

Published: Jul 27, 2015

Author(s): A. V. Golovin, A. V. Korsakov, A. N. Zaitsev

Journal: Journal of Raman Spectroscopy

In this study we present Raman spectroscopy data obtained from a naturally occurring orthorhombic nyerereite (Na,K)2Ca(CO3)2 from the Oldoinyo Lengai volcano (Tanzania) at ambient and high temperature. Nyerereite was heated up to 300 °C, 400 °C and 500 °C, and is believed to have been transformed at high temperatures to hexagonal β‐ and γ‐phases similar to zemkorite, (Na,K)2Ca(CO3)2. There are no major differences in the chemical composition of natural...

Read More thumbnail image: In situ ambient and hightemperature Raman spectroscopic studies of nyerereite NaK 2 CaCO 3  2  can hexagonal zemkorite be stable at earthsurface conditions

Statistically rigorous analysis of imaging SIMS data in the presence of detector saturation

Published: Jul 27, 2015

Author(s): Lev D. Gelb, Layla A. Bakhtiari, Amy V. Walker

Journal: Surface and Interface Analysis

We present a new strategy for analyzing imaging time‐of‐flight SIMS data sets affected by detector saturation. Rather than attempt to correct the measured data to remove saturation, we incorporate the detector behavior into the statistical basis of the analysis. This is performed within the framework of maximum a posteriori reconstruction. The proposed approach has several advantages over previous techniques. No approximations are involved...

Read More thumbnail image: Statistically rigorous analysis of imaging SIMS data in the presence of detector saturation

Effects of Mn 2+ on the chrome‐free colored Ti/Zr‐based conversion coating on 6063 aluminum alloy

Published: Jul 27, 2015

Author(s): Aihua Yi, WenFang Li, Jun Du, SongLin Mu

Journal: Surface and Interface Analysis

The conversion coating with golden color and improved corrosion resistance had been prepared by adding Mn2+ in the Ti/Zr conversion coating solution. Comparing with that of conversion coating without Mn2+, the optimal treatment time of this conversion coating was much shorter and the corrosion resistance was obviously improved. The effect of Mn2+ on the formation of golden Ti/Zr conversion coating was thoroughly investigated by means of energy dispersive X‐ray...

Read More thumbnail image: Effects of Mn 2 on the chromefree colored TiZrbased conversion coating on 6063 aluminum alloy

Retention behavior of resorcinarene‐based cavitands on C 8 and C 18 stationary phases

Published: Jul 27, 2015

Author(s): Endre Bartó, Ibolya Prauda, Ferenc Kilár, Ibolya Kiss, Attila Felinger

Journal: Journal of Separation Science

The understanding of the retention behavior of large molecules is an area of interest in liquid chromatography. Resorcinarene‐based cavitands are cavity‐shaped cyclic oligomers that can create host–guest interactions. We have investigated the chromatographic behavior of two types of cyclic tetramers as analytes in high‐performance liquid chromatography. The experiments were performed at four different temperatures (15, 25, 35, 45°C) on...

Read More thumbnail image: Retention behavior of resorcinarenebased cavitands on C 8 and C 18 stationary phases

Elution–extrusion counter‐current chromatography for the separation of two pairs of isomeric monoterpenes from Paeoniae Alba Radix

Published: Jul 27, 2015

Author(s): Chu Chu, Shidi Zhang, Shengqiang Tong, Xingnuo Li, Qingyong Li, Jizhong Yan

Journal: Journal of Separation Science

In this work, a simple and efficient protocol for the rapid separation of two pairs of isomeric monoterpenes from Paeoniae Alba Radix was developed by combining macroporous resin and elution–extrusion counter‐current chromatography. The crude extract was firstly subjected to a D101 macroporous resin column eluted with water and a series of different concentrations of ethanol. Then, effluents of 30 and 95% ethanol were collected as sample...

Read More thumbnail image: Elutionextrusion countercurrent chromatography for the separation of two pairs of isomeric monoterpenes from Paeoniae Alba Radix
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