EarlyView Articles
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Drug concentrations in post‐mortem femoral blood compared with therapeutic concentrations in plasma
Published: Jul 23, 2013
Author(s): Terhi Launiainen, Ilkka Ojanperä
Journal: Drug Testing and Analysis
Therapeutic drug concentrations measured in plasma are of limited value as reference intervals for interpretation in post‐mortem (PM) toxicology. In this study, drug concentration distributions were studied in PM femoral venous blood from 57 903 Finnish autopsy cases representing all causes of death during an 11‐year period. Cause‐of‐death information was obtained from death certificates issued by forensic pathologists. Median, mean, and...
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LC/MS/MS analysis of the endogenous dimethyltryptamine hallucinogens, their precursors, and major metabolites in rat pineal gland microdialysate
Published: Jul 23, 2013
Author(s): Steven A. Barker, Jimo Borjigin, Izabela Lomnicka, Rick Strassman
Journal: Biomedical Chromatography
ABSTRACT We report a qualitative liquid chromatography–tandem mass spectrometry (LC/MS/MS) method for the simultaneous analysis of the three known N,N‐dimethyltryptamine endogenous hallucinogens, their precursors and metabolites, as well as melatonin and its metabolic precursors. The method was characterized using artificial cerebrospinal fluid (aCSF) as the matrix and was subsequently applied to the analysis of rat brain pineal...
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A validated HPLC‐PDA method for identification and quantification of two bioactive alkaloids, ephedrine and cryptolepine, in different Sida species
Published: Jul 23, 2013
Author(s): Arnab Chatterjee, Satyanshu Kumar, Sunil K. Chattopadhyay
Journal: Biomedical Chromatography
ABSTRACT A simple, rapid, accurate and reproducible reverse‐phase HPLC method has been developed for the identification and quantification of two alkaloids ephedrine and cryptolepine in different extracts of Sida species using photodiode array detection. Baseline separation of the two alkaloids was achieved on a Waters RP‐18 X‐terra column (250 × 4.6 mm, 5 µm) using a solvent system consisting of a mixture of water containing 0.1%...
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Development and validation of a stability‐indicating assay including the isolation and characterization of degradation products of metaxalone by LC‐MS
Published: Jul 23, 2013
Author(s): R. Nageswara Rao, Hassan Farah, Prafulla Kumar Sahu, Muthumani Janarthan, Ch. Gangu Naidu
Journal: Biomedical Chromatography
ABSTRACT A stability‐indicating reverse‐phase high‐performance liquid chromatography–mass spectrometric method was developed and validated for the assay of metaxalone through forced degradation under acidic, alkaline, photo, oxidative and peroxide stress conditions. Separation of degradation products was accomplished on a reverse‐phase Phenomenex C18 (250 × 4.6 mm, 5 µm) column thermostated at 25°C using 10 mM aqueous ammonium acetate: methanol...
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Chemical effects of high‐resolution Yb Lγ 4 emission spectra: a possible probe for chemical analysis
Published: Jul 23, 2013
Author(s): Hisashi Hayashi, Noriko Kanai, Naomi Kawamura, Yasuhiro H. Matsuda, Kentaro Kuga, Satoru Nakatsuji, Tetsuro Yamashita, Shigeo Ohara
Journal: X-Ray Spectrometry
An ‘eccentric’ X‐ray emission, YbLγ4, was measured for Yb metal, Yb2O3, YbF3, β‐YbAlB4, YbNi3Al9, and YbNi3Ga9 with a resolution of ~0.9 eV. Peak splitting of the YbLγ4 line was observed in all the recorded spectra and was attributed to the two components originating from the LS coupling of the Yb5p hole, the Yb5p1/2 (LIOII: Lγ4′) and Yb5p3/2 components (LIOIII: Lγ4). The spectra were substantially different depending on the chemical environment of Yb. The position of the...
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Click chemistry immobilization strategies in the development of strong cation exchanger chiral stationary phases for HPLC
Published: Jul 22, 2013
Author(s): Denise Wolrab, Peter Frühauf, Michal Kohout, Wolfgang Lindner
Journal: Journal of Separation Science
Enantioseparation of chiral amines with HPLC has developed into a widely used analytical and preparative tool. Chiral basic molecules, which act as cationic species upon protonation, are suited for an enantioselective cation exchange process. Novel strong cation exchangers (SCX) based on different 3,5‐disubstituted benzoic acids functionalized with trans‐(R,R)‐ and trans‐(S,S)‐2‐aminocyclohexanesulfonic acid as the chiral selector (SO) and ion...
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Travelling wave ion mobility and negative ion fragmentation for the structural determination of N ‐linked glycans
Published: Jul 22, 2013
Author(s): David J. Harvey, Charlotte A. Scarff, Matthew Edgeworth, Max Crispin, Christopher N. Scanlan, Frank Sobott, Sarah Allman, Kavitha Baruah, Laura Pritchard, James H. Scrivens
Journal: ELECTROPHORESIS
Travelling wave ion mobility was investigated for its ability to separate N‐glycans from other compounds and for resolution of isomers. Charged glycans, exemplified by sialylated complex N‐glycans released from bovine fetuin and ionised by electrospray, could be separated from residual glycopeptides allowing the minor, more highly sialylated compounds to be detected where their ions were obscured by ions from other compounds in different charge...
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Efficient excitation of Raman coherence by a gradient force
Published: Jul 21, 2013
Author(s): Dongxia Ma, Yuri V. Rostovtsev
Journal: Journal of Raman Spectroscopy
The vibrational molecular excitation by strong laser fields have been studied. Starting with the molecular Hamiltonian, we derive the vibrational excitation rate due to a gradient of laser field and show that the rate can be two to three orders of magnitude larger than the regular Raman rates. The developed theory contributes to understanding of interaction of powerful laser pulses with molecular systems, and it might be used in...
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Pump power dependence in resonance femtosecond stimulated Raman spectroscopy
Published: Jul 21, 2013
Author(s): Joohyun Lee, J. Reddy Challa, David W. McCamant
Journal: Journal of Raman Spectroscopy
Femtosecond stimulated Raman spectroscopy (FSRS) has emerged as a powerful new technique that is capable of obtaining resonance Raman spectra of fluorescent species and transient photochemical intermediates. Unlike related transient infrared absorption techniques, the FSRS signal is quite sensitive to the laser power utilized in the vibrational probing event. In particular, FSRS spectra are highly sensitive to the intensity of the...
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LC‐ESI‐MS/MS analysis and pharmacokinetics of jolkinolide B, a potential antitumor active component isolated from Euphorbia fischeriana , in rat plasma
Published: Jul 19, 2013
Author(s): Yang Li, Xiao‐Li Liu, Zhen‐Gang Cai, Si‐Xi Zhang
Journal: Biomedical Chromatography
ABSTRACT A simple, specific and reproducible liquid chromatography–electrospray ionization mass spectrometry was developed and validated for the determination of jolkinolide B, a potential antitumor active component isolated from Euphorbia fischeriana, in rat plasma. Chromatographic separation was achieved on a Venusil MP‐C18 column using an isocratic elution. Jolkinolide B and osthole (internal standard) were monitored by positive electrospray ...
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Toward sub‐micro‐XRF working at nanometer range using capillary optics
Published: Jul 19, 2013
Author(s): M. Dehlinger, C. Fauquet, F. Jandard, A. Bjeoumikhov, S. Bjeoumikhova, R. Gubzhokov, A. Erko, I. Zizak, D. Pailharey, S. Ferrero, B. Dahmani, D. Tonneau
Journal: X-Ray Spectrometry
Capillary optics are used for X‐ray fluorescence micro‐analysis using the Cu Kα line provided by a rotating anode. The excitation beam is focused using a polycapillary lens on a Co–Ti sample. Cylindrical glass capillaries of various diameters are fitted to the X‐ray detector (Energy Dispersive X‐Ray (EDX) analyzer) and displaced along the irradiated zone of the sample. The fluorescence is studied as a function of capillary position. Good...
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A direct sensitivity comparison between flow‐modulated comprehensive 2D and 1D GC in untargeted and targeted MS‐based experiments
Published: Jul 19, 2013
Author(s): Peter Q. Tranchida, Flavio A. Franchina, Mariosimone Zoccali, Ivana Bonaccorsi, Francesco Cacciola, Luigi Mondello
Journal: Journal of Separation Science
The present contribution is focused on the measurement of the analytical sensitivity attained in untargeted/targeted MS/MS experiments, performed using flow‐modulator comprehensive 2D and 1D GC. The comprehensive 2D experiment was performed by diverting part of the high flow (circa 80%) to flush the accumulation loop (about 28 mL/min) to waste, to reduce the gas flow entering the ion source. 1D analyses were performed through: (i)...
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Preparation of polyhedral oligomeric silsesquioxane based hybrid monoliths by ring‐opening polymerization for capillary LC and CEC
Published: Jul 19, 2013
Author(s): Hui Lin, Zhenbin Zhang, Jing Dong, Zhongshan Liu, Junjie Ou, Hanfa Zou
Journal: Journal of Separation Science
A new organic–inorganic hybrid monolith was prepared by the ring‐opening polymerization of octaglycidyldimethylsilyl polyhedral oligomeric silsesquioxane (POSS) with 1,4‐butanediamine (BDA) using 1‐propanol, 1,4‐butanediol, and PEG 10 000 as a porogenic system. Benefiting from the moderate phase separation process, the resulting poly(POSS‐co‐BDA) hybrid monolith possessed a uniform microstructure and exhibited excellent performance in chromatographic...
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Highly stable surface modification of hypercrosslinked monolithic capillary columns and their application in hydrophilic interaction chromatography
Published: Jul 19, 2013
Author(s): Veronika Škeříková, Jiří Urban
Journal: Journal of Separation Science
A two‐step surface modification of poly(styrene‐co‐vinylbenzyl chloride‐co‐divinylbenzene) monolithic stationary phases, including hypercrosslinking and thermally initiated surface grafting of [2‐(methacryloyloxy)ethyl]dimethyl(3‐sulfopropyl)ammonium hydroxide, has been used to prepare capillary columns for the isocratic separation of small polar compounds in hydrophilic interaction chromatography (HILIC). The prepared monolithic columns...
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Rapid and simple LC‐MS/MS screening of 64 novel psychoactive substances using dried blood spots
Published: Jul 19, 2013
Author(s): Lars Ambach, Ana Hernández Redondo, Stefan König, Wolfgang Weinmann
Journal: Drug Testing and Analysis
The range of novel psychoactive substances (NPS) including phenethylamines, cathinones, piperazines, tryptamines, etc. is continuously growing. Therefore, fast and reliable screening methods for these compounds are essential and needed. The use of dried blood spots (DBS) for a fast straightforward approach helps to simplify and shorten sample preparation significantly. DBS were produced from 10 µl of whole blood and extracted offline with...
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Variability of cannabis potency in the Venice area (Italy): A survey over the period 2010–2012
Published: Jul 19, 2013
Author(s): Luca Zamengo, Giampietro Frison, Chiara Bettin, Rocco Sciarrone
Journal: Drug Testing and Analysis
Cannabis is the most widely used illicit substance globally, with an estimated annual prevalence in 2010 of 2.6–5.0% of the adult population. Concerns have been expressed about increases in the potency of cannabis products. A high tetrahydrocannabinol (THC) content can increase anxiety, depression, and psychotic symptoms, and can increase the risk of dependence and adverse effects on the respiratory and cardiovascular systems in regular...
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Expanding analytical possibilities concerning the detection of stanozolol misuse by means of high resolution/high accuracy mass spectrometric detection of stanozolol glucuronides in human sports drug testing
Published: Jul 19, 2013
Author(s): Wilhelm Schänzer, Sven Guddat, Andreas Thomas, Georg Opfermann, Hans Geyer, Mario Thevis
Journal: Drug Testing and Analysis
Anabolic‐androgenic steroids (AAS) represent one of the most frequently detected classes of prohibited substances in doping controls. Due to their long‐lasting beneficial effects on athletic performance, utmost retrospectivity via urine analysis is desirable and accomplished by targeting long‐term metabolites of the respective drugs. In case of stanozolol, a substantial variety of metabolites has enabled the identification of numerous...
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An unusual case of risperidone instability in a fatality presenting an analytical and interpretative challenge
Published: Jul 19, 2013
Author(s): Kerry Taylor, Simon Elliott
Journal: Drug Testing and Analysis
This paper describes the detection and characterization of unusual metabolite/breakdown products of the anti‐psychotic drug risperidone in post‐mortem blood and urine as part of a toxicological investigation into an unexpected death of a male suffering from paranoid schizophrenia prescribed risperidone and previously paroxetine. Compounds detected in the post‐mortem blood and urine specimens were shown to be benzisoxazole ring scission...
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Protein purification by aminosquarylium cyanine dye‐affinity chromatography
Published: Jul 19, 2013
Author(s): M. S. Silva, V. C. Graça, L. V. Reis, P. F. Santos, P. Almeida, J. A. Queiroz, F. Sousa
Journal: Biomedical Chromatography
ABSTRACT The most selective purification method for proteins and other biomolecules is affinity chromatography. This method is based on the unique biological‐based specificity of the biomolecule–ligand interaction and commonly uses biological ligands. However, these ligands may present some drawbacks, mainly because of their cost and lability. Dye‐affinity chromatography overcomes the limitations of biological ligands and is widely...
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Development of HPLC/fluorescence detection method for chiral resolution of dansylated benzimidazoles derivatives
Published: Jul 19, 2013
Author(s): Emmanuelle Lipka, Julie Charton, Claude Vaccher
Journal: Biomedical Chromatography
ABSTRACT The development of high performance liquid chromatography method on amylose‐based stationary phase (Chiralpak AD) with n‐hexane–2‐propanol (90:10, v/v) as mobile phase allowed the enantioseparation of non‐dansylated and dansylated benzimidazole derivatives, prepared from potent‐AMPK activators, to be achieved. Using both fluorescence and ultraviolet detection, limits of detection and quantification were determined. Fluorescence...
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