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The advances of electromigration techniques applied for alkaloid analysis
Published: Jul 1, 2013
Author(s): Szymon Dziomba, Mariusz Belka, Piotr Kowalski, Alina Plenis, Tomasz Bączek
Journal: Biomedical Chromatography
ABSTRACT Alkaloids are natural products of metabolism found mainly in plants. Their diversified pharmacological activities as medical agents and extensive occurrence in nutritional products demand the development of reliable and sensitive analytical tools. This review presents the developments in the field of electromigration techniques and specifically capillary and microchip electrophoresis. We include the main aspects of interest...
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Screening and determination for potential α ‐glucosidase inhibitory constituents from Dalbergia odorifera T. Chen using ultrafiltration‐LC/ESI‐MS n
Published: Jul 1, 2013
Author(s): Chunfang Zhao, Yongqiang Liu, Dengli Cong, Hui Zhang, Jiajia Yu, Ying Jiang, Xiuyue Cui, Jiaming Sun
Journal: Biomedical Chromatography
ABSTRACT In the present study, it was demonstrated that ethyl acetate soluble fraction partitioned from heartwood of Dalbergia odorifera T. Chen (HEF) had a remarkable inhibitory effect on α‐glucosidase. Therefore HEF was selected as a starting material for screening the potential α‐glucosidase inhibitors using ultrafiltration liquid chromatography/mass spectrometry (UF‐LC/MS). Twenty‐six compounds were identified with analysis of LC/MS. UF assay indicated...
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Laser wavelength dependence of background fluorescence in Raman spectroscopic analysis of synovial fluid from symptomatic joints
Published: Jul 1, 2013
Author(s): Shan Yang, Bolan Li, Mikhail N. Slipchenko, Anna Akkus, Nora G. Singer, Yener N. Yeni, Ozan Akkus
Journal: Journal of Raman Spectroscopy
Gout is a disease process where the nucleation and growth of crystals in the synovial fluid of joints elicit painful arthritis‐like symptoms. Raman spectroscopy is evolving as a potential diagnostic tool in identifying such crystals; however, attainment of sufficient Raman signal while overcoming the background fluorescence remains as a major challenge. The current study focused on assessing whether excitation in 532–700 nm range will...
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Characterization and quantification of 10‐hydroxycamptothecine in Camptotheca acuminate and its medicinal preparation by liquid chromatography–ion trap mass spectrometry
Published: Jul 1, 2013
Author(s): Qinhua Chen, Guangmin Pan, Lin Xiong, Hongsheng He, Hangdong Yang
Journal: Biomedical Chromatography
ABSTRACT A rapid and sensitive method for the identification and quantification of 10‐hydroxycamptothecine (HCPT) in Camptotheca acuminata Decne is described. The HCPT standard solution was directly infused into the ion trap mass spectrometers (IT/MS) for collecting the MSn spectra. The electrospray ionization (ESI) mass spectral fragmentation pathway of HCPT was proposed and the ESI‐MSn fragmentation behavior of HCPT was deduced in detail. The major...
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Determination of 3‐ α ‐hydroxytibolone in human plasma by LC‐MS/MS: application for a pharmacokinetic study after administration of a tibolone formulation
Published: Jul 1, 2013
Author(s): Fabiana Fernandes de Santana e Silva Cardoso, Isabela Costa César, Iram Moreira Mundim, Leonardo de Souza Teixeira, Enikson Pontes Silva, Ricardo Rodrigues Bonfim, Sandro Antônio Gomes, Denys Pires Ferreira, Aderimar Rogério Batista Lopes, Helifas Duarte Pascoal, Weidson Carlo Souza, Gerson Antônio Pianetti
Journal: Biomedical Chromatography
ABSTRACT A new method was developed for the quantitation of 3‐α‐hydroxy tibolone, in human plasma, after oral administration of a tablet formulation containing tibolone (2.5 mg). 3‐α‐Hydroxy tibolone was extracted by a liquid–liquid procedure, using cyproterone acetate as internal standard and chlorobutane as extraction solvent. After extraction, samples were submitted to a derivatization step with p‐toluenesulfonyl isocyanate. A mobile phase consisting of...
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Efficient chromatographic separation of intact proteins derivatized with a fluorogenic reagent for proteomics analysis
Published: Jul 1, 2013
Author(s): Tomoko Ichibangase, Itaru Yazawa, Kazuhiro Imai
Journal: Biomedical Chromatography
ABSTRACT To achieve more efficient separation of intact proteins for proteomics applications, three columns of differing diameters (4.0, 4.6 and 6.0 mm internal diameter) were chosen for comparison and investigated to identify optimal conditions. The column with the largest diameter gave the largest peak capacity, showing the efficient separation of intact proteins, such as two protein standards, glutathione S‐transferase and...
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Quantitative determination of d‐ and l‐threo enantiomers of methylphenidate in brain tissue by liquid chromatography–mass spectrometry
Published: Jul 1, 2013
Author(s): Carolyn C. Combs, Erin L. Hankins, Cara L. Copeland, Stacy D. Brown, Brooks B. Pond
Journal: Biomedical Chromatography
ABSTRACT Methylphenidate, a psychostimulant used for the treatment of attention deficit hyperactivity disorder and narcolepsy, is administered as a 50:50 racemic mixture, despite the fact that d‐methylphenidate has been shown to have greater pharmacologic activity. This paper presents a validated LC‐MS/MS approach to separation and quantification of methylphenidate enantiomers using a vancomycin column and triethylammonium acetate...
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Validation of a new HPLC‐UV method for determination of the antibiotic linezolid in human plasma and in bronchoalveolar lavage
Published: Jul 1, 2013
Author(s): Serena Fortuna, Gennaro De Pascale, Enzo Ragazzoni, Massimo Antonelli, Pierluigi Navarra
Journal: Biomedical Chromatography
ABSTRACT A rapid and selective HPLC‐UV method was developed for the quantification of linezolid (LNZ) in human plasma and bronchoalveolar lavage (BAL) at the concentrations associated with therapy. Plasma samples were extracted by solid‐phase extraction followed by evaporation to dryness and reconstitution in mobile phase solution. The chromatographic separation was carried out on a C18 column with an isocratic mobile phase...
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Simultaneous quantitative analyses of indole and oxindole alkaloids of Uncaria Hook in rat plasma and brain after oral administration of the traditional Japanese medicine Yokukansan using high‐performance liquid chromatography with tandem mass spectrometr
Published: Jul 1, 2013
Author(s): Hirotaka Kushida, Miwako Fukutake, Masahiro Tabuchi, Takao Katsuhara, Hiroaki Nishimura, Yasushi Ikarashi, Masanao Kanitani, Yoshio Kase
Journal: Biomedical Chromatography
ABSTRACT Uncaria Hook (UH) alkaloids are involved in the beneficial effects of Yokukansan. However, the pharmacokinetics of UH alkaloids after oral administration of Yokukansan has not yet been sufficiently investigated. Therefore, we developed and validated a sensitive and specific high‐performance liquid chromatography with tandem mass spectrometry (LC/MS/MS) method for the simultaneous quantitation of seven UH alkaloids...
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Modification of cysteine residues by cyclopentenone prostaglandins: Interplay with redox regulation of protein function
Published: Jul 1, 2013
Author(s): Clara L. Oeste, Dolores Pérez‐Sala
Journal: Mass Spectrometry Reviews
Abstract Cyclopentenone prostaglandins (cyPG) are endogenous lipid mediators involved in the resolution of inflammation and the regulation of cell proliferation and cellular redox status. Upon exogenous administration they have shown beneficial effects in models of inflammation and tissue injury, as well as potential antitumoral actions, which have raised a considerable interest in their study for the...
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Quantitative analysis of heavy elements and semi‐quantitative evaluation of heavy mineral compositions of sediments in Japan for construction of a forensic soil database using synchrotron radiation X‐ray analyses
Published: Jun 28, 2013
Author(s): Izumi Nakai, Shunsuke Furuya, Willy Bong, Yoshinari Abe, Keiichi Osaka, Takuya Matsumoto, Masayoshi Itou, Atsuyuki Ohta, Toshio Ninomiya
Journal: X-Ray Spectrometry
We have started to construct a nationwide forensic soil sediment database for Japan, based on the heavy mineral and trace heavy element compositions of stream sediments collected at 3024 points across Japan. The data were measured by high‐resolution synchrotron radiation X‐ray powder diffraction (SR‐XRD) and high‐energy SR X‐ray fluorescence analysis (XRF) using the SR source of SPring‐8, the SR radiation facility in Japan. The automated...
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High‐resolution imaging of magnetisation transfer and nuclear Overhauser effect in the human visual cortex at 7 T
Published: Jun 26, 2013
Author(s): Olivier Mougin, Matthew Clemence, Andrew Peters, Alain Pitiot, Penny Gowland
Journal: NMR in Biomedicine
The aim of this study was to optimise a pulse sequence for high‐resolution imaging sensitive to the effects of conventional macromolecular magnetisation transfer (MTm) and nuclear Overhauser enhancement (NOE), and to use it to investigate variations in these parameters across the cerebral cortex. A high‐spatial‐resolution magnetisation transfer‐prepared turbo field echo (MT‐TFE) sequence was designed to have high sensitivity to MTm and...
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Electrochemically controlled detection of adrenaline on poly(2‐aminobenzylamine) thin films by surface plasmon resonance spectroscopy and quartz crystal microbalance
Published: Jun 26, 2013
Author(s): Sopis Chuekachang, Rapiphun Janmanee, Akira Baba, Sukon Phanichphant, Saengrawee Sriwichai, Kazunari Shinbo, Keizo Kato, Futao Kaneko, Nobuko Fukuda, Hirobumi Ushijima
Journal: Surface and Interface Analysis
In this study, we present an electrochemically controlled surface plasmon resonance (EC‐SPR) biosensor to detect adrenaline on poly(2‐aminobenzylamine) (P2ABA) thin films. The P2ABA thin films are stable and display electroactivity in a neutral PBS solution. Specific detection of adrenaline was performed on P2ABA thin films because the benzylamine groups in the P2ABA structure could specifically react with adrenalines. Adrenaline was...
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Advanced hyphenated chromatographic‐mass spectrometry in mycotoxin determination: Current status and prospects
Published: Jun 26, 2013
Author(s): Peiwu Li, Zhaowei Zhang, Xiaofeng Hu, Qi Zhang
Journal: Mass Spectrometry Reviews
Abstract Mass spectrometric techniques are essential for advanced research in food safety and environmental monitoring. These fields are important for securing the health of humans and animals, and for ensuring environmental security. Mycotoxins, toxic secondary metabolites of filamentous fungi, are major contaminants of agricultural products, food and feed, biological samples, and the environment as a whole....
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Salbutamol extraction from urine and its stability in different solutions: identification of methylation products and validation of a quantitative analytical method
Published: Jun 26, 2013
Author(s): Bruno Carius Garrido, Mayra Leal Chrisóstomo Silva, Ricardo Moreira Borges, Monica Costa Padilha, Francisco Radler Aquino Neto
Journal: Biomedical Chromatography
ABSTRACT Salbutamol is commonly used in asthma treatment, being considered a short‐effect bronchodilator. This drug poses special interest in certain fields of chemical analysis, such as food, clinical and doping analyses, in which it needs to be analyzed with quantitative precision and accuracy. Salbutamol, however, is known to degrade under certain conditions and this is critical if quantitative results must be generated. The...
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In vivo MRI analysis of depth‐dependent ultrastructure in human knee cartilage at 7 T
Published: Jun 25, 2013
Author(s): Nikita Garnov, Wilfried Gründer, Gregor Thörmer, Robert Trampel, Robert Turner, Thomas Kahn, Harald Busse
Journal: NMR in Biomedicine
Signal intensities of T2‐weighted magnetic resonance images depend on the local fiber arrangement in hyaline cartilage. The aims of this study were to determine whether angle‐sensitive MRI at 7 T can be used to quantify the cartilage ultrastructure of the knee in vivo and to assess potential differences with age. Ten younger (21–30 ) and ten older (55–76 years old) healthy volunteers were imaged with a T2‐weighted spin‐echo...
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Determination of the stress biomarker corticosterone in serum of tumor‐bearing mice by surrogate‐based liquid chromatography–tandem mass spectrometry
Published: Jun 25, 2013
Author(s): Lei Kang, Tao Jiang, Xinxing Ge, Liang Peng, Ying Xie, Xin Luan, Huafang Li, Zhengxing Rong, Hong Qi, Hongzhuan Chen
Journal: Biomedical Chromatography
ABSTRACT A simple, robust and specific liquid chromatography tandem mass spectrometry (LC‐MS/MS) method was developed and validated to determine the concentration of corticosterone (Cort) which is usually regarded as a stress biomarker in mouse serum. Since Cort is an endogenous hormone, a ‘surrogate analyte’ strategy was adopted using the stable isotope‐deuterated corticosterone as a surrogate of the authentic analyte to generate...
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Using microbubbles as an MRI contrast agent for the measurement of cerebral blood volume
Published: Jun 24, 2013
Author(s): Shin‐Lei Peng, Fu‐Nien Wang, Chung‐Hsin Wang, Hsu‐Hsia Peng, Chih‐Tien Lu, Chih‐Kuang Yeh
Journal: NMR in Biomedicine
The susceptibility differences at the gas–liquid interface of microbubbles (MBs) allow their use as an intravascular susceptibility contrast agent for in vivo MRI. However, the characteristics of MBs are very different from those of the standard gadolinium‐diethylenetriaminepentaacetic acid (Gd‐DPTA) contrast agent, including the size distribution and hemodynamic properties, which could influence MRI outcomes. Here, we investigate...
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Enhancing the [ 13 C]bicarbonate signal in cardiac hyperpolarized [1‐ 13 C]pyruvate MRS studies by infusion of glucose, insulin and potassium
Published: Jun 24, 2013
Author(s): Mette Hauge Lauritzen, Christoffer Laustsen, Sadia Asghar Butt, Peter Magnusson, Lise Vejby Søgaard, Jan Henrik Ardenkjær‐Larsen, Per Åkeson, C. Laustsen, J. H. Ardenkjær‐Larsen, J. H. Ardenkjær‐Larsen
Journal: NMR in Biomedicine
A change in myocardial metabolism is a known effect of several diseases. MRS with hyperpolarized 13C‐labelled pyruvate is a technique capable of detecting changes in myocardial pyruvate metabolism, and has proven to be useful for the evaluation of myocardial ischaemia in vivo. However, during fasting, the myocardial glucose oxidation is low and the fatty acid oxidation (β‐oxidation) is high, which complicates the interpretation of pyruvate metabolism...
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Characterization of synthetic routes to ‘Bromo‐DragonFLY’ and benzodifuranyl isopropylamine homologues utilizing ketone intermediates. Part 1: Synthesis of ketone precursors
Published: Jun 24, 2013
Author(s): Richard E. O'Connor, John J. Keating
Journal: Drug Testing and Analysis
Bromo‐DragonFLY (BDF) and many of its analogues are misused as recreational drugs due to their potency as psychoactive substances. To date, none of the published routes to these designer amphetamines have exploited a ketone intermediate. It is well known that benzyl methyl ketone (BMK) can be employed as a precursor in the synthesis of amphetamine. Similarly, it is reasonable to assume that ketone precursors may potentially be utilized in...
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