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One degradation phenomenon that occurs in artworks is the formation of metal oxalates on their surfaces. In order to gain
insight into the inclination of pigments to produce oxalates, nine pigments including Na, Ca, Fe, Pb and Cu cations were selected
to react with oxalic acid solutions at different concentrations (1 M, 0.1 M, 0.01 M and 0.005 M). Micro-Raman spectroscopy
was used to detect the different reaction products. Pigments containing calcium (calcite, gypsum and Volterra gypsum) showed
a high tendency to form weddellite as well as whewellite, especially at high acidic concentrations; among copper-based pigments
(malachite, azurite, verdigris), the formation of moolooite was observed for high concentrations of acid and down to the lowest
concentration (0.005 M) in the case of verdigris. Lead oxalate was detected on lead white. No iron oxalates were observed
for hematite; the formation of calcium oxalate crystals was observed instead. Ultramarine blue reacted to produce elemental
sulfur. According to the results obtained, calcite and verdigris showed the highest reactivity in oxalic acid environments,
resulting in a high tendency to form calcium and copper oxalates, even at very low acidic concentrations; this behavior seems
to arise from the high solubilities of these pigments in acidic environments.
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3583-1
Authors
A. Zoppi, Università di Firenze Dipartimento di Chimica, Polo Scientifico e Tecnologico Via della Lastruccia 3, Sesto Fiorentino 50019 Firenze Italy
C. Lofrumento, Università di Firenze Dipartimento di Chimica, Polo Scientifico e Tecnologico Via della Lastruccia 3, Sesto Fiorentino 50019 Firenze Italy
N. F. C. Mendes, Università di Firenze Dipartimento di Chimica, Polo Scientifico e Tecnologico Via della Lastruccia 3, Sesto Fiorentino 50019 Firenze Italy
E. M. Castellucci, Università di Firenze Dipartimento di Chimica, Polo Scientifico e Tecnologico Via della Lastruccia 3, Sesto Fiorentino 50019 Firenze Italy
The Raman spectroscopic analysis of several stone samples with applied red pigments obtained from an archaeological excavation
of an Augustinian friary discovered during the construction of an extension to Hull Magistrates Court in 1994 has revealed
a surprising diversity of composition. Cinnabar, red lead and haematite have all been identified alone or in admixture; the
cinnabar is exceptional in that it has only been found heavily adulterated with red ochre and red lead, as the other two pigments
are found alone. There are signatures of limewash putty, which has been applied to the stone substrate prior to the painting,
which is characteristic of the Roman method of wall painting, and there are no traces of gypsum found in the specimens studied.
This evidence indicates an early mediaeval method of stone decoration.
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3568-0
Authors
Howell G. M. Edwards, University of Bradford Division of Chemical & Forensic Sciences, School of Life Sciences Bradford BD7 1DP UK
Emma M. Newton, University of Bradford Division of Chemical & Forensic Sciences, School of Life Sciences Bradford BD7 1DP UK
Sonia O’Connor, University of Bradford Division of Archaeological, Geography and Environmental Sciences, School of Life Sciences Bradford BD7 1DP UK
D. Evans, The Old School Humber Archaeological Partnership Northumberland Avenue Hull HU2 0LN UK
This study describes a modification to tricine sodium dodecyl sulphate polyacrylamide gel electrophoresis to make it more
effective for the separation of low molecular mass proteins and for coupling with inductively coupled plasma mass spectrometry
(ICP-MS). The modified method employs low-percentage polyacrylamide gels (7–10%) (w/v) and low reagent concentrations that
provide efficient separations, good quantitation and low matrix levels that are compatible with ICP-MS. Using phosphopeptides
as a model system, and offline analysis, we obtained recoveries of 73% (w/v) in a 9% gel compared with 55% in a conventional
16% gel. Online coupling was achieved by modification of a standard commercially available gel electroelution apparatus and
casting of the gel into a 7.3-cm-long tube. Online separation of a digest of β-casein was demonstrated with recovery of the
mono- and tetraphosphopeptides, which were identified by comparison with peptide standards. A mass balance study with the
standards yielded recoveries of 95% for tetraphosphopeptides and 48% for monophosphopeptides. The factors affecting the separations
and recoveries are discussed in detail. The detection limits for 10-µL samples of the mono- and tetraphosphopeptides were
0.7 µM (7 pmol) and 0.2 µM (2 pmol) respectively.
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3588-9
Authors
Syed R. Haider, Loughborough University Centre for Analytical Science, Department of Chemistry Leicestershire LE11 3TU UK
Helen J. Reid, Loughborough University Centre for Analytical Science, Department of Chemistry Leicestershire LE11 3TU UK
Barry L. Sharp, Loughborough University Centre for Analytical Science, Department of Chemistry Leicestershire LE11 3TU UK
The uranyl sulphate mineral zippeite was studied by Raman spectroscopy. The phase purity of the sample was initially checked
by X-ray powder diffraction and its chemical composition was defined by electron microprobe (wavelength dispersive spectroscopy,
WDS) analysis. The Raman spectroscopy research focused on the low wavenumber and uranyl stretching vibration regions. Vibration
bands down to 50 cm–1 were tentatively assigned. The U–O bond lengths were calculated based on empirical relations. Inferred values are consistent
with those obtained from the crystal structure analysis of synthetic zippeite. Number of bands was interpreted on the basis
of factor group analysis.
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3577-z
Authors
Jakub Plášil, National Museum Department of Mineralogy and Petrology Václavské nám. 68 115 79 Prague 1 Czech Republic
Elena Buixaderas, Academy of Sciences of the Czech Republic Department of Dielectrics, Institute of Physics Na Slovance 2 182 21 Prague 8 Czech Republic
Jiří Čejka, National Museum Natural History Museum Václavské nám. 68 115 79 Prague 1 Czech Republic
Jiří Sejkora, National Museum Department of Mineralogy and Petrology Václavské nám. 68 115 79 Prague 1 Czech Republic
Jan Jehlička, Charles University in Prague Institute of Geochemistry, Mineralogy and Mineral Resources, Faculty of Science Albertov 6 128 43 Prague 2 Czech Republic
Milan Novák, Masaryk University Department of Geological Science, Faculty of Science Kotlářská 2 611 37 Brno Czech Republic
This paper deals with the development and optimization of an analytical procedure using ultrafiltration and a flow-injection
system, and its application in in-situ experiments to characterize the lability and availability of metal species in humic-rich
hydrocolloids. The on-line system consists of a tangential flow ultrafiltration device equipped with a 3-kDa filtration membrane.
The concentration of free ions in the filtrate was determined by atomic-absorption spectrometry, assuming that metals not
complexed by aquatic humic substances (AHS) were separated from the complexed species (M–AHS) retained by the membrane. For
optimization, exchange experiments using Cu(II) solutions and AHS solutions doped with the metal ions Ni(II), Mn(II), Fe(III),
Cd(II), and Zn(II) were carried out to characterize the stability of the metal–AHS complexes. The new procedure was then applied
in-situ at a tributary of the Ribeira do Iguape river (Iguape, São Paulo State, Brazil) and evaluated using the ions Fe(III)
and Mn(II), which are considered to be essential constituents of aquatic systems. From the exchange between metal–natural
organic matter (M–NOM) and the Cu(II) ions it was concluded that Cu(II) concentrations >485 μg L−1 were necessary to obtain maximum exchange of the complexes Mn–NOM and Fe–NOM, corresponding to 100% Mn and 8% Fe. Moreover,
the new analytical procedure is simple and opens up new perspectives for understanding the complexation, transport, stability,
and lability of metal species in humic-rich aquatic environments.
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3547-5
Authors
Danielle Goveia, UNESP – Universidade Estadual Paulista Departamento de Engenharia Ambiental 18087-180 Sorocaba SP Brazil
Fabiana Aparecida Lobo, UNESP – Universidade Estadual Paulista Departamento de Engenharia Ambiental 18087-180 Sorocaba SP Brazil
Peter Burba, ISAS – Institute for Analytical Sciences 44013 Dortmund Germany
Leonardo Fernandes Fraceto, UNESP – Universidade Estadual Paulista Departamento de Engenharia Ambiental 18087-180 Sorocaba SP Brazil
Newton Luiz Dias Filho, UNESP – Universidade Estadual Paulista Departamento de Física e Química 15385-000 Ilha Solteira SP Brazil
André Henrique Rosa, UNESP – Universidade Estadual Paulista Departamento de Engenharia Ambiental 18087-180 Sorocaba SP Brazil
Poly(2-N-carbazolylethyl acrylate) with terminal trimethoxysilyl groups was prepared as an organic phase and immobilized onto silica.
The retention behavior of the column packed with this carbazole-based polymer-immobilized silica (Sil-CEA) was investigated
by using various estrogenic steroids and corticoids in both reversed-phase and normal-phase liquid chromatography. As a result,
complete separation was confirmed for eight kinds of steroids with Sil-CEA. The most specific separation with Sil-CEA can
be emphasized by the high separation factor (e.g., α = 1.39 in methanol–water (7:3, v/v) at 35 °C) for 17α and 17β-estradiols, one of the most difficult pairs of isomers in chromatographic separation, whereas
for two kinds of commercially available polymeric ODS columns as references α = 1.01, only, under the same conditions. Because the excellent separation and retention order with Sil-CEA was maintained
even in a normal-phase mobile phase such as a hexane–2-propanol, it is estimated that the CEA phase has multiple interaction
mechanisms through stronger interactions such as dipole–dipole, carbonyl–π, and hydrogen bonding interactions than the hydrophobic
effect expected with ODS.
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3601-3
Authors
Abul K. Mallik, Kumamoto University Department of Applied Chemistry and Biochemistry, Faculty of Engineering 2-39-1 Kurokami Kumamoto Japan
Kaori Shingo, Kumamoto University Department of Applied Chemistry and Biochemistry, Faculty of Engineering 2-39-1 Kurokami Kumamoto Japan
Usha Ghimire Gautam, Kumamoto University Department of Applied Chemistry and Biochemistry, Faculty of Engineering 2-39-1 Kurokami Kumamoto Japan
Tsuyoshi Sawada, Kumamoto University Department of Applied Chemistry and Biochemistry, Faculty of Engineering 2-39-1 Kurokami Kumamoto Japan
Makoto Takafuji, Kumamoto University Department of Applied Chemistry and Biochemistry, Faculty of Engineering 2-39-1 Kurokami Kumamoto Japan
Hirotaka Ihara, Kumamoto University Department of Applied Chemistry and Biochemistry, Faculty of Engineering 2-39-1 Kurokami Kumamoto Japan
Superporous monolithic hydrogels (cryogel monoliths) are elastic, sponge-like materials that can be prepared in an aqueous
medium through a cryotropic gelation technique. These monoliths show interesting properties for the development of high-throughput
solid-phase extraction supports to treat large volumes of aqueous samples. In this work, a cryogel-supported molecularly imprinted
solid-phase extraction approach for the endocrine disruptor bisphenol A (BPA) from river water and wine samples is presented.
An imprinted polymer with molecular recognition properties for BPA was prepared in acetonitrile by thermal polymerization
of a mixture of 4,4′-dihydroxy-2,2-diphenyl-1,1,1,3,3,3-trifluoropropane as a mimic template of BPA, 4-vinylpyridine and trimethylolpropane
trimethacrylate in a molar ratio of 1 + 6 + 6. Fine imprinted particles (<10 μm) were embedded in a poly-acrylamide-co-N,N′-methylenbisacrylamide cryogel obtained by ammonium persulfate-induced cryopolymerization at −18 °C. The resulting monolithic
gel was evaluated for its use as a sorbent support in an off-line solid-phase extraction approach to recover BPA from dilute
aqueous samples with minimum pre-loading work-up. The optimized extraction protocol resulted in a reliable MISPE method suitable
to selectively extract and preconcentrate BPA from river water and red wine samples, demonstrating the practical feasibility
of cryogel-trapped imprinted polymers as solid-phase extraction materials
Figure Superporous poly-acrylamide-co-N,N'-methylen-bis-acrylamide cryogels embedding micron-sized imprinted particles were used
to set up a method for efficient solid phase extraction of the endocrine disruptor bisphenol A from river water and wine samples
with minimum pre-loading work-up
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3591-1
Authors
Claudio Baggiani, University of Torino Laboratory of Bioanalytical Chemistry, Department of Analytical Chemistry via Giuria 5 10125 Turin Italy
Patrizia Baravalle, University of Torino Laboratory of Bioanalytical Chemistry, Department of Analytical Chemistry via Giuria 5 10125 Turin Italy
Cristina Giovannoli, University of Torino Laboratory of Bioanalytical Chemistry, Department of Analytical Chemistry via Giuria 5 10125 Turin Italy
Laura Anfossi, University of Torino Laboratory of Bioanalytical Chemistry, Department of Analytical Chemistry via Giuria 5 10125 Turin Italy
Gianfranco Giraudi, University of Torino Laboratory of Bioanalytical Chemistry, Department of Analytical Chemistry via Giuria 5 10125 Turin Italy
In the present study, we have evaluated the effectiveness of a passive sampler for polar organic chemicals to accumulate a
group of widespread and hazardous tumor-promoting toxins produced in cyanobacterial water blooms—microcystins (MC). The previously
optimized configuration of the sampler based on polycarbonate membrane and Oasis HLB sorbent (2.75 mg/cm2) was validated under various exposure scenarios in laboratory and field. Calibration of the passive sampler conducted under
variable conditions and concentrations of MC revealed linearity of the sampling up to 4 weeks. The sampling rates of microcystins
for two different exposure scenarios were derived (e.g., MC-LR: Rs = 0.017 L/day under static and 0.087 L/d under turbulent conditions). Rs values were further used for calculations of time-weighted average concentrations in natural water. Improved sensitivity
and selectivity of the in-house-made sampler was observed in comparison with the commercially available Polar Organic Compound
Integrative Sampler (POCIS). Comparisons of grab and passive sampling methods were performed during cyanobacterial water bloom
season in the Brno reservoir, Czech Republic in 2008. Data obtained by passive sampling provided a more relevant picture of
the situation and enabled better assessment of potential risks. The present study demonstrated that the modification of POCIS
is suitable for monitoring of occurrence and retrospective estimations of microcystin water concentrations, especially with
respect to the control of drinking water quality.
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3578-y
Authors
Jiří Kohoutek, The Academy of Sciences of the Czech Republic Institute of Botany Lidická 25/27 657 20 Brno Czech Republic
Blahoslav Maršálek, The Academy of Sciences of the Czech Republic Institute of Botany Lidická 25/27 657 20 Brno Czech Republic
Luděk Bláha, The Academy of Sciences of the Czech Republic Institute of Botany Lidická 25/27 657 20 Brno Czech Republic
T. Hianik, X. Wang, V. Tashlitsky, T. Oretskaya, S. Ponikova, M. Antalik, J. S. Ellis, M. Thompson
(Paper from Analyst)
T. Hianik, Analyst, 2010, DOI: 10.1039/c0an00070a
To cite this article before page numbers are assigned, use the DOI form of citation above.
The content of this RSS Feed (c) The Royal Society of Chemistry
Angela Walter, Susann Erdmann, Thomas Bocklitz, Elke-Martina Jung, Nadine Vogler, Denis Akimov, Benjamin Dietzek, Petra Rosch, Erika Kothe, Jurgen Popp
(Paper from Analyst)
Angela Walter, Analyst, 2010, DOI: 10.1039/b921101b
To cite this article before page numbers are assigned, use the DOI form of citation above.
The content of this RSS Feed (c) The Royal Society of Chemistry
Most methods for the analysis of oligosaccharides from biological sources require a glycan derivatization step: glycans may
be derivatized to introduce a chromophore or fluorophore, facilitating detection after chromatographic or electrophoretic
separation. Derivatization can also be applied to link charged or hydrophobic groups at the reducing end to enhance glycan
separation and mass-spectrometric detection. Moreover, derivatization steps such as permethylation aim at stabilizing sialic
acid residues, enhancing mass-spectrometric sensitivity, and supporting detailed structural characterization by (tandem) mass
spectrometry. Finally, many glycan labels serve as a linker for oligosaccharide attachment to surfaces or carrier proteins,
thereby allowing interaction studies with carbohydrate-binding proteins. In this review, various aspects of glycan labeling,
separation, and detection strategies are discussed.
Figure MALDI-FTICR-MS of 2AA-labeled total plasma N-glycans
Content Type Journal Article
Category Review
DOI 10.1007/s00216-010-3532-z
Authors
L. R. Ruhaak, Leiden University Medical Center Biomolecular Mass Spectrometry Unit, Department of Parasitology P.O. Box 9600 2300RC Leiden The Netherlands
G. Zauner, Leiden University Medical Center Biomolecular Mass Spectrometry Unit, Department of Parasitology P.O. Box 9600 2300RC Leiden The Netherlands
C. Huhn, Leiden University Medical Center Biomolecular Mass Spectrometry Unit, Department of Parasitology P.O. Box 9600 2300RC Leiden The Netherlands
C. Bruggink, Leiden University Medical Center Biomolecular Mass Spectrometry Unit, Department of Parasitology P.O. Box 9600 2300RC Leiden The Netherlands
A. M. Deelder, Leiden University Medical Center Biomolecular Mass Spectrometry Unit, Department of Parasitology P.O. Box 9600 2300RC Leiden The Netherlands
M. Wuhrer, Leiden University Medical Center Biomolecular Mass Spectrometry Unit, Department of Parasitology P.O. Box 9600 2300RC Leiden The Netherlands
This paper describes determination of the deoxynivalenol and ergosterol in samples from different varieties of barley and,
consequently, malt produced from this barley. In total, 20 samples of barley and 20 samples of barley malt were analyzed.
The alkaline hydrolysis with consequent extraction into hexane was applied to obtain the ergosterol from cereals. Extraction
to acetonitrile/water and subsequent solid-phase extraction (SPE) were used for deoxynivalenol. The determination of the samples
was performed on high-performance liquid chromatography using UV detection (ergosterol) and mass spectrometric detection (deoxynivalenol).
The influence of the malting process on the production of two compounds of interest was assessed from obtained results. Ergosterol
concentration ranged 0.88–15.87 mg/kg in barley and 2.63–34.96 mg/kg in malt, where its content increased to 95% compared
to samples before malting. The malting process was observed as having a significant effect on ergosterol concentration (P = 0.07). The maximum concentration of deoxynivalenol was found to be 641 µg/kg in barley and 499 µg/kg in malt. Its concentration
was lower than the legislative limit for unprocessed cereals (1,250 µg/kg). The statistic effect of the malting process on
deoxynivalenol production was not found. Linear correlation between ergosterol and deoxynivalenol content was found to be
very low (barley R = 0.02, malt R = 0.01). The results revealed that it is not possible to consider the ergosterol content as the indicator of deoxynivalenol
contamination of naturally molded samples.
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3585-z
Authors
Vlastimil Dohnal, University of J.E. Purkynje in Usti nad Labem Department of Chemistry, Faculty of Science Ceske mladeze 8 400 96 Usti nad Labem Czech Republic
Alena Jezkova, Mendel University of Agriculture and Forestry in Brno Department of Food Technology, Faculty of Agronomy Zemedelská 1 613 00 Brno Czech Republic
Lucie Pavlikova, Mendel University of Agriculture and Forestry in Brno Department of Food Technology, Faculty of Agronomy Zemedelská 1 613 00 Brno Czech Republic
Kamil Musilek, University of J.E. Purkynje in Usti nad Labem Department of Chemistry, Faculty of Science Ceske mladeze 8 400 96 Usti nad Labem Czech Republic
Daniel Jun, University of J.E. Purkynje in Usti nad Labem Department of Chemistry, Faculty of Science Ceske mladeze 8 400 96 Usti nad Labem Czech Republic
Kamil Kuca, University of J.E. Purkynje in Usti nad Labem Department of Chemistry, Faculty of Science Ceske mladeze 8 400 96 Usti nad Labem Czech Republic
Based on several alerts from European countries over the last years concerning spices, we have been encouraged to establish
an accurate method for the determination of dyes, aflatoxins and pesticides in various types of spices using reversed-phase
(RP) liquid chromatography–tandem mass spectrometry interfaced with electrospray (LC–ESI–MS/MS). A simple sample treatment
procedure entailing the use of an extraction step with acetonitrile without further cleanup has been developed. A C18 column
with an aqueous ammonium formate/methanol mixture as the mobile phase was used, and gradient elution was performed. Mass spectral
acquisition was done in positive ion mode by applying multiple reaction monitoring of at least two fragmentation transitions
per compound to provide a high degree of selectivity. The method was in-house validated in terms of linearity, sensitivity,
repeatability, recovery and selectivity on six kinds of spices. Satisfactory results in the majority of the cases were obtained
for all analytes and matrices, with practical limits of quantitation acceptable for routine monitoring purposes. Extraction
recoveries for most of the compounds ranged from 60% to 140% at spiking levels of 0.05 and 0.5 mg kg−1. The applicability of the method for the simultaneous determination of dyes, aflatoxins and pesticides in several types of
spices was demonstrated, and the method successfully applied to a limited number of products from the local market.
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3526-x
Authors
C. Ferrer Amate, University of Almería Community Reference Laboratory (DG SANCO) for Residues of Pesticides in Fruits and Vegetables, Pesticide Residue Research Group, Department of Hydrogeology and Analytical Chemistry 04120 La Cañada de San Urbano Almería Spain
H. Unterluggauer, Austrian Agency for Health and Food Safety (AGES) GmbH Technikerstrasse 70 6020 Innsbruck Austria
R. J. Fischer, Austrian Agency for Health and Food Safety (AGES) GmbH Technikerstrasse 70 6020 Innsbruck Austria
A. R. Fernández-Alba, University of Almería Community Reference Laboratory (DG SANCO) for Residues of Pesticides in Fruits and Vegetables, Pesticide Residue Research Group, Department of Hydrogeology and Analytical Chemistry 04120 La Cañada de San Urbano Almería Spain
S. Masselter, Austrian Agency for Health and Food Safety (AGES) GmbH Technikerstrasse 70 6020 Innsbruck Austria
In the present article, a novel microfluidic immunosensor coupled with electrochemical detection for anti-gliadin IgG antibody
quantification is proposed. This device represents an important tool for a fast, simple, sensitive, and automated diagnostic
for celiac disease, which is carried out through detection of anti-gliadin IgG antibodies present in human serum samples.
Celiac disease (CD) is an autoimmune disease generated by gluten protein fractions called prolamins. This pathology affects
about one in 250 people around the world, produces intestinal inflammation, villous atrophy, and crypt hyperplasia, which
causes a range of symptoms including altered bowel habits, malnutrition and weight loss. Our immunosensor consists of a Plexiglas
device coupled to a gold electrode, with a central channel containing 3-aminopropyl-modified controlled pore glass (AP-CPG).
The quantification of anti-gliadin IgG antibodies was carried out using a heterogeneous, non-competitive enzyme-linked immunosorbent
assay (ELISA) in which IgG antibodies bound to gliadin protein, immobilized on AP-CPG, were determined by alkaline phosphatase
(AP) enzyme-labeled second antibodies specific to human IgG. The p-aminophenyl phosphate (p-APP) was converted to p-aminophenol (p-AP) by AP, and the electroactive product was quantified on a gold electrode at 0.250 V. The calculated detection limits for
electrochemical detection and the ELISA procedure were 0.52 and 2.72 UR mL−1, respectively, and the within- and between-assay coefficients of variation were below 5.8%. The optimized procedure was applied
to the determination of anti-gliadin IgG antibodies in human serum samples.
Content Type Journal Article
Category Paper in Forefront
DOI 10.1007/s00216-010-3589-8
Authors
Sirley V. Pereira, Universidad Nacional de San Luis, CONICET INQUISAL, Departamento de Química Chacabuco 917 D5700BWS San Luis Argentina
Julio Raba, Universidad Nacional de San Luis, CONICET INQUISAL, Departamento de Química Chacabuco 917 D5700BWS San Luis Argentina
Germán A. Messina, Universidad Nacional de San Luis, CONICET INQUISAL, Departamento de Química Chacabuco 917 D5700BWS San Luis Argentina
Influencing the endurance in elite sports is one of the key points in modern sports science. Recently, a new class of prohibited
substances reached in the focus of doping control laboratories and their misuse was classified as gene doping. The adenosine
monophosphate activated protein kinase activator 5-amino-4-imidazolecarboxyamide ribonucleoside (AICAR) was found to significantly
enhance the endurance even in sedentary mice after treatment. Due to endogenous production of AICAR in healthy humans, considerable
amounts were present in the circulation and, thus, were excreted into urine. Considering these facts, the present study was
initiated to fix reference values of renally cleared AICAR in elite athletes. Therefore a quantitative analytical method by
means of isotope-dilution liquid chromatography (analytical column: C6-phenyl) coupled to tandem mass spectrometry, after
a sample preparation consisting of a gentle dilution of native urine, was developed. Doping control samples of 499 athletes
were analysed, and AICAR concentrations in urine were determined. The mean AICAR value for all samples was 2,186 ng/mL with
a standard deviation of 1,655 ng/mL. Concentrations were found to differ depending on gender, type of sport and type of sample
collection (in competition/out of competition). The method was fully validated for quantitative purposes considering the parameters
linearity, inter- (12%, 7% and 10%) and intraday precision (14%, 9% and 12%) at low, mid and high concentration, robustness,
accuracy (approx. 100%), limit of quantification (100 ng/mL), stability and ion suppression effects, employing an in-house
synthesised 13C5-labelled AICAR as internal standard.
Urinary AICAR concentrations (ng/mL)
Content Type Journal Article
Category Paper in Forefront
DOI 10.1007/s00216-010-3560-8
Authors
Andreas Thomas, German Sport University Cologne Institute of Biochemistry, Center for Preventive Doping Research Am Sportpark Müngersdorf 50933 Cologne Germany
Simon Beuck, German Sport University Cologne Institute of Biochemistry, Center for Preventive Doping Research Am Sportpark Müngersdorf 50933 Cologne Germany
Jens Christian Eickhoff, Colorado State University Department of Statistics Fort Collins CO 80523-1877 USA
Sven Guddat, German Sport University Cologne Institute of Biochemistry, Center for Preventive Doping Research Am Sportpark Müngersdorf 50933 Cologne Germany
Oliver Krug, German Sport University Cologne Institute of Biochemistry, Center for Preventive Doping Research Am Sportpark Müngersdorf 50933 Cologne Germany
Matthias Kamber, Federal Office of Sports Department of Doping Prevention 3000 Bern Switzerland
Wilhelm Schänzer, German Sport University Cologne Institute of Biochemistry, Center for Preventive Doping Research Am Sportpark Müngersdorf 50933 Cologne Germany
Mario Thevis, German Sport University Cologne Institute of Biochemistry, Center for Preventive Doping Research Am Sportpark Müngersdorf 50933 Cologne Germany
Toxaphene is a complex technical mixture that has been found ubiquitously in the environment but has caused issues for analysis,
especially of individual congeners. This paper reports the elution order of 26 major toxaphene congeners on three gas chromatographic
columns. The three different stationary phases generally had similar elution orders for the toxaphene congeners, but fewer
co-elutions occurred on a low-bleed, low-polarity column. These congeners (except for two that co-eluted and were not added
to the calibration mixture) were examined in air particulate matter standard reference materials (SRMs), 1648a, 1649a, and
1649b as well as SRM 3067 toxaphene in methanol for assignment of reference values. SRM 3067 had mass fractions an order of
magnitude greater than the air particulate SRMs, which ranged from 0.568 ± 0.018 ng g−1 dry mass (B9-2006 in SRM 1648a) to 12.9 ± 0.20 ng g−1 dry mass (B9-715 (P 58) in SRM 1649a). The three air particulate SRMs all had different mass fractions and proportions of
congeners relative to the sum of the toxaphene congeners. SRM 3067 may be useful as a technical mixture toxaphene congener
calibrant. SRMs 1648a and 1649b will serve as reference materials for the analysis of 21 (three congeners were not included
due to values below the detection limit or a potential polychlorinated biphenyl co-elution) toxaphene congeners in atmospheric
particulate samples.
Figure Comparison (mean±SD) of proportions of toxaphene congeners to the sum of the congeners in air particulate matter SRMs 1649a,
1649b, and 1648a and compared to SRM 3067 toxaphene in methanol. Among the air particulate matter SRMs, all congeners were
significantly different (P≤0.0006) with most significantly different among all three SRMs (a indicates an SRM with greater proportion than the others
for that congener). The comparisons between the air particulate matter SRMs and SRM 3067 were significant (P<0.002) except as indicated by n.s.
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3512-3
Authors
Stacy S. Vander Pol, National Institute of Standards and Technology Analytical Chemistry Division, Hollings Marine Laboratory 331 Fort Johnson Road Charleston SC 29412 USA
John R. Kucklick, National Institute of Standards and Technology Analytical Chemistry Division, Hollings Marine Laboratory 331 Fort Johnson Road Charleston SC 29412 USA
Stefan D. Leigh, National Institute of Standards and Technology Statistical Engineering Division Gaithersburg MD 20899 USA
Barbara J. Porter, National Institute of Standards and Technology Analytical Chemistry Division Gaithersburg MD 20899 USA
Michele M. Schantz, National Institute of Standards and Technology Analytical Chemistry Division Gaithersburg MD 20899 USA
A fluorescent single-domain antibody (fluobody), a fusion protein of a green fluorescent protein extracted from Aequorea coerulescens (AcGFP), a mutant that has been codon-optimized for mammalian expression, and a single-chain variable fragment antibody (scFv),
against plumbagin (5-hydroxy-2-methyl-1,4-naphthoquinone; PL) was successfully constructed and expressed in Escherichia coli. The expressed fluobody was purified, refolded, and characterized to develop a speedy, simple, and sensitive fluorescence-linked
immunosorbent assay (FLISA) for the determination of PL. In this study, two kinds of fluobody containing PL-scFv at the N-terminus
of AcGFP (N fluobody) or the C-terminus of AcGFP (C fluobody) were constructed with flexible amino acid linker (Gly4Ser)2 between PL-scFv and AcGFP for comparative purposes. Characterization of the fluobodies revealed that the C fluobody has better
properties as a probe for FLISA than the N fluobody because the fluorescence intensity of C fluobody was 18-fold higher than
that of N fluobody. Moreover, C fluobody exhibited a fourfold-higher binding affinity than the N fluobody. More interestingly,
the limit of detection for PL measurement in FLISA (24 ng mL−1) was improved to eightfold higher than that in conventional ELISA (0.2 μg mL−1), indicating that a sensitive immunoassay could be developed by using fluobody instead of monoclonal antibody or scFv.
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3535-9
Authors
Seiichi Sakamoto, Kyushu University Department of Pharmacognosy, Graduate School of Pharmaceutical Sciences 3-1-1 Maidashi, Higashi-ku Fukuoka 812-8582 Japan
Futoshi Taura, Kyushu University Department of Pharmacognosy, Graduate School of Pharmaceutical Sciences 3-1-1 Maidashi, Higashi-ku Fukuoka 812-8582 Japan
Benyakan Pongkitwitoon, Kyushu University Department of Pharmacognosy, Graduate School of Pharmaceutical Sciences 3-1-1 Maidashi, Higashi-ku Fukuoka 812-8582 Japan
Waraporn Putalun, Khon Kaen University Faculty of Pharmaceutical Sciences Khon Kaen 40002 Thailand
Ryota Tsuchihashi, Fukuoka University Department of Pharmacognosy, Faculty of Pharmaceutical Sciences 8-19-1 Nanakuma, Jonan-ku Fukuoka 814-0180 Japan
Junei Kinjo, Fukuoka University Department of Pharmacognosy, Faculty of Pharmaceutical Sciences 8-19-1 Nanakuma, Jonan-ku Fukuoka 814-0180 Japan
Hiroyuki Tanaka, Kyushu University Department of Pharmacognosy, Graduate School of Pharmaceutical Sciences 3-1-1 Maidashi, Higashi-ku Fukuoka 812-8582 Japan
Satoshi Morimoto, Kyushu University Department of Pharmacognosy, Graduate School of Pharmaceutical Sciences 3-1-1 Maidashi, Higashi-ku Fukuoka 812-8582 Japan
Asbestos fibers are an important cause of serious health problems and respiratory diseases. The presence, structural coordination,
and oxidation state of iron at the fiber surface are potentially important for the biological effects of asbestos because
iron can catalyze the Haber–Weiss reaction, generating the reactive oxygen species ⋅OH. Literature results indicate that the
surface concentration of Fe(III) may play an important role in fiber-related radical formation. Amphibole asbestos were analyzed
by X-ray photoelectron spectroscopy (XPS) and Mössbauer spectroscopy, with the aim of determining the surface vs. bulk Fe(III)/Fetot ratios. A standard reference asbestos (Union Internationale Contre le Cancer crocidolite from South Africa) and three fibrous
tremolite samples (from Italy and USA) were investigated. In addition to the Mössbauer spectroscopy study of bulk Fe(III)/Fetot ratios, much work was dedicated to the interpretation of the XPS Fe2p signal and to the quantification of surface Fe(III)/Fetot ratios. Results confirmed the importance of surface properties because this showed that fiber surfaces are always more oxidized
than the bulk and that Fe(III) is present as oxide and oxyhydroxide species. Notably, the highest difference of surface/bulk
Fe oxidation was found for San Mango tremolite—the sample that in preliminary cytotoxicity tests (MTT assay) had revealed
a cell mortality delayed with respect to the other samples.
Content Type Journal Article
Category Paper in Forefront
DOI 10.1007/s00216-010-3576-0
Authors
Marzia Fantauzzi, Centro Grandi Strumenti Università di Cagliari Dipartimento di Chimica Inorganica e Analitica, INSTM Research Unit 09100 Cagliari Italy
Alessandro Pacella, Sapienza Università di Roma Dipartimento di Scienze della Terra Piazzale Aldo Moro 5 00185 Rome Italy
Davide Atzei, Centro Grandi Strumenti Università di Cagliari Dipartimento di Chimica Inorganica e Analitica, INSTM Research Unit 09100 Cagliari Italy
Antonio Gianfagna, Sapienza Università di Roma Dipartimento di Scienze della Terra Piazzale Aldo Moro 5 00185 Rome Italy
Giovanni B. Andreozzi, Sapienza Università di Roma Dipartimento di Scienze della Terra Piazzale Aldo Moro 5 00185 Rome Italy
Antonella Rossi, Centro Grandi Strumenti Università di Cagliari Dipartimento di Chimica Inorganica e Analitica, INSTM Research Unit 09100 Cagliari Italy
Lorenz H. Fischer, Sergey M. Borisov, Michael Schaeferling, Ingo Klimant, Otto S. Wolfbeis
(Paper from Analyst)
Lorenz H. Fischer, Analyst, 2010, DOI: 10.1039/b927255k
To cite this article before page numbers are assigned, use the DOI form of citation above.
The content of this RSS Feed (c) The Royal Society of Chemistry
Ana Gonzalez-Antuna, Pablo Rodriguez-Gonzalez, Giuseppe Centineo, J. Ignacio Garcia Alonso
(Paper from Analyst)
Ana Gonzalez-Antuna, Analyst, 2010, DOI: 10.1039/b924432h
To cite this article before page numbers are assigned, use the DOI form of citation above.
The content of this RSS Feed (c) The Royal Society of Chemistry
The extraction of six sulfonamides (sulfadiazine, sulfadimidine, sulfathiazole, sulfachloropiridazine, sulfadimethoxine, and
sulfaquinoxaline) from soils with different physicochemical characteristics and at several aging times was investigated. Conventional
mechanical shaking, microwave-assisted extraction, ultrasound probe-assisted extraction and pressurized liquid extraction
techniques were evaluated. The four techniques provided similar results when applied to freshly contaminated soils. However,
microwave-assisted extraction was the most suitable to extract sulfonamide aged residues from soils. Microwave-assisted extraction
was applied to eight soils aged for 3 months, using acetonitrile:buffer pH 9 (20:80) as the extraction solvent, and recoveries
ranged from 15–25% for STZ to 42–64% for SDM.
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3580-4
Authors
J. Raich-Montiu, Universitat de Barcelona Departament de Química Analítica Martí i Franquès 1 08028 Barcelona Spain
J. L. Beltrán, Universitat de Barcelona Departament de Química Analítica Martí i Franquès 1 08028 Barcelona Spain
M. D. Prat, Universitat de Barcelona Departament de Química Analítica Martí i Franquès 1 08028 Barcelona Spain
M. Granados, Universitat de Barcelona Departament de Química Analítica Martí i Franquès 1 08028 Barcelona Spain
Due to their unique optical and electronic properties, quantum dots (QDs) have been widely used in a variety of biosensors
for sensitive detection of biomarkers and small molecules. However, single QD exhibits dynamic fluctuation of fluorescence
intensity (i.e., blinking) with the transition between on and off states, which adversely influences the development of QD-based
optical biosensors. Therefore, the methods for efficient evaluation of on-state QD are especially important and highly desirable.
In this paper, a novel and unique approach based on single-molecule two-color coincidence detection is developed to simply
and accurately evaluate the on-state QDs in a microfluidic flow. Our results demonstrate that improved QDs in the on state
are detected in a microfluidic flow in comparison with that in the Brownian motion state, thus paving the way to the development
of single QD-based biosensors for sensitive detection of low-abundance biomolecules. This single-molecule two-color coincidence
detection has been applied for the homegeneous detection of nucleic acids in a microfluidic flow with the detection sensitivity
of 5.0 fM.
Figure Representative traces of fluorescence bursts from the 525Bead–655QD complex in the Brownian motion state. The fluorescence
signals of the 655QDs were shown in red; the fluorescence signals of the 525Beads were shown in blue
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3555-5
Authors
Chun-yang Zhang, Chinese Academy of Sciences Institute of Biomedical Engineering and Health Technology, Shenzhen Institutes of Advanced Technology Shenzhen 518055 China
Kun Yang, Chinese Academy of Sciences Institute of Biomedical Engineering and Health Technology, Shenzhen Institutes of Advanced Technology Shenzhen 518055 China
A method for the determination of polycyclic aromatic hydrocarbons (PAHs) in liquid pyrolysate of biomass (bio-oil) was developed
with attention to greenness along with accuracy. Bio-oil obtained from preparative pyrolysis at 500 °C of poplar wood as representative
biomass matrix was dissolved into acetonitrile (ACN). An aliquot of the ACN solution (0.1 mg bio-oil) was added with water
(20% v/v) and spiked with perdeuterated standards, then PAHs were extracted with n-hexane and separated from phenolic interferents by silica gel solid-phase extraction (SPE). All 16 priority PAHs were detected
at concentrations between 7.7 µg g−1 (naphthalene) and 0.1 µg g−1 (benz[a]anthracene) with RSD in the 6–23% range. Recovery of perdeuterated acenaphthene, phenanthrene and chrysene was 84, 93 and
90%, respectively. Results obtained from the analysis of bio-oil were used to evaluate the performance of analytical pyrolysis
conducted with a heated platinum filament in off-line configuration. Two sampling procedures were compared: (1) sorption onto
silica gel followed by elution with n-hexane (Py-SPE), (2) dynamic solid-phase micro-extraction followed by fibre cleanup with aqueous ammonia (Py-SPME). Emission
levels of priority PAHs could be determined by Py-SPE with RSD in the 13–45% range, while Py-SPME was unsatisfactory for quantitation.
Emission levels determined by Py-SPE fell in the 6.4–0.1 µg g−1 range slightly higher than those calculated from bio-oil analysis. Both Py methods were adequate for screening purposes to
assess the effect of catalysts on PAH formation. In particular, they agreed to show that the content of PAHs expected in bio-oil
increased dramatically when pyrolysis was conducted over HZSM-5 zeolite.
Figure PAHs in the pyrolysate of poplar wood: novel procedures of bio-oil analysis and analytical pyrolysis of biomass
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3563-5
Authors
Daniele Fabbri, Università di Bologna Laboratorio di Scienze Ambientali “R. Sartori”, Centro Interdipartimentale di Ricerca in Scienze Ambientali (C.I.R.S.A.) via Sant’ Alberto 163 48123 Ravenna Italy
Alessio Adamiano, Università di Bologna Laboratorio di Scienze Ambientali “R. Sartori”, Centro Interdipartimentale di Ricerca in Scienze Ambientali (C.I.R.S.A.) via Sant’ Alberto 163 48123 Ravenna Italy
Cristian Torri, Università di Bologna Laboratorio di Scienze Ambientali “R. Sartori”, Centro Interdipartimentale di Ricerca in Scienze Ambientali (C.I.R.S.A.) via Sant’ Alberto 163 48123 Ravenna Italy
Porous polymer monoliths have emerged as unique materials for many applications, including liquid-chromatographic analyses
at an unrivaled speed, solid-phase extraction, and enzyme immobilization in capillary and microfluidic chip format. This article
reviews the state of the art in the preparation of monoliths in narrow-bore capillaries and microfluidic chips and their miniaturization
under conditions of spatial confinement. New developments in their preparation mainly using free radical polymerization techniques
with a focus on morphological aspects in view of homogeneous porous materials are described. The suitability of monoliths
for analysis of both large and small molecules is also discussed.
Content Type Journal Article
Category Trends
DOI 10.1007/s00216-010-3550-x
Authors
Ivo Nischang, Johannes Kepler University Linz Institute of Polymer Chemistry Welser Strasse 42 4060 Leonding Austria
Oliver Brueggemann, Johannes Kepler University Linz Institute of Polymer Chemistry Welser Strasse 42 4060 Leonding Austria
Frantisek Svec, E.O. Lawrence Berkeley National Laboratory The Molecular Foundry Berkeley CA 94720 USA
Organophosphate esters (OPEs), utilized as flame retarding agents and/or plasticizers, are almost ubiquitous in environmental
compartments, and biota and foods could be contaminated by bioaccumulation or during the treatment processes. A multiresidue
method is proposed for the determination of 13 OPEs in fish tissues: analytes were simultaneously extracted and purified using
the matrix solid phase dispersion technique and then determined by gas chromatography with nitrogen–phosphorus detection.
The main parameters affecting extraction yield and selectivity, such as the type of dispersant material, clean-up co-sorbent,
rinse and elution solvents, were evaluated to obtain lipid-free extracts and quantitative recoveries for OPEs. Under optimal
conditions, 0.5 g of samples was dispersed with 2 g Florisil and 1 g anhydrous sodium sulphate and transferred to a solid
phase extraction cartridge containing 1 g alumina. The lipids were removed using 5 mL n-hexane/dichloromethane (1:1) and analytes were recovered with 10 mL n-hexane/acetone (6:4) and directly analysed. The method developed provided recoveries between 70 and 110% for different kinds
of fish, and the day-to-day variability was between 1 and 9%. This procedure constitutes the first analytical method for the
analysis of OPEs in a food matrix and it is applicable to analyse a large number of samples to evaluate the occurrence and
sources of OPEs in biota and foods.
Figure GC-NPD chromatograms of the MSPD extracts from spiked salmon sample
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3548-4
Authors
Luca Campone, Università degli Studi di Salerno Dipartimento di Scienze Farmaceutiche (DIFARMA) Via Ponte Don Melillo 84084 Fisciano (SA) Italy
Anna Lisa Piccinelli, Università degli Studi di Salerno Dipartimento di Scienze Farmaceutiche (DIFARMA) Via Ponte Don Melillo 84084 Fisciano (SA) Italy
Conny Östman, Stockholm University Department of Analytical Chemistry 106 91 Stockholm Sweden
Luca Rastrelli, Università degli Studi di Salerno Dipartimento di Scienze Farmaceutiche (DIFARMA) Via Ponte Don Melillo 84084 Fisciano (SA) Italy
Cocoa is well-known to be rich in flavan-3-ols. Previous analyses have established that alkaline treatment of cocoa beans
results in epimerization of (−)-epicatechin to (−)-catechin and (+)-catechin to (+)-epicatechin. Now, the question is whether
both epimers can be absorbed by the human organism. This paper describes sample preparation and an HPLC method for chiral
determination of (+)/(−)-catechin from sulfated and glucuronidated metabolites in human plasma. The sample preparation includes
enzymatic hydrolysis of the catechin metabolites, and solid-phase extraction (SPE). A PM-γ-cyclodextrin column is used with
a coulometric electrode-array detection (CEAD) system. The recovery of catechin ranges from 89.9 to 96.8%. The limit of detection
is 5.9 ng mL−1 for (−)-catechin and 6.8 ng mL−1 for (+)-catechin, and the limit of quantification is 12.8 ng mL−1 for (−)-catechin and 16.9 ng mL−1 for (+)-catechin. The relative standard deviation of the method ranges from 0.9 to 1.5%. This method was successfully applied
to human plasma after consumption of a cocoa drink. In one human self-experiment, (+)-catechin and (−)-catechin were found
in human plasma, but metabolism of the two enantiomers differed.
Figure Separation of (+)/(-)-catechin in human plasma
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3542-x
Authors
Christina Ritter, University of Bonn Institute of Nutrition and Food Sciences Endenicher Allee 11–13 53115 Bonn Germany
Benno F. Zimmermann, University of Bonn Institute of Nutrition and Food Sciences Endenicher Allee 11–13 53115 Bonn Germany
Rudolf Galensa, University of Bonn Institute of Nutrition and Food Sciences Endenicher Allee 11–13 53115 Bonn Germany
Linear alkylbenzene sulfonates (LAS), nonylphenol ethoxylates (NPE; sum of nonylphenol, nonylphenol monoethoxylate, and nonylphenol
diethoxylate), and di-(2-ethylhexyl)phthalate (DEHP) are the most problematic organic pollutants in sludge owing to their
high concentrations and the concentration limits of 2,600, 50, and 100 mg/kg, respectively, proposed in the European Union
directive draft for land application of sludge. In this paper, an analytical method for the simultaneous determination of
the C10, C11, C12, and C13 LAS homologues, the nonylphenolic compounds nonylphenol, nonylphenol monoethoxylate, and nonylphenol diethoxylate, and di(2-ethylhexyl)phthalate
in compost and compost-amended soil is proposed. The method is based on sonication-assisted extraction, cleanup by solid-phase
extraction, and determination by high-performance liquid chromatography with diode-array and fluorescence detectors. The mean
recoveries of LAS, NPE, and DEHP were 83, 87, and 79%, respectively, in compost samples, and 77, 96, and 99%, respectively,
in compost-amended soil samples. The limits of detection and quantification in compost samples were lower than 6.77 and 22.3 mg/kg
dry matter, respectively, for LAS; lower than 7.34 and 22.8 mg/kg dry matter, respectively, for NPE; and 0.78 and 1.18 mg/kg
dry matter, respectively, for DEHP. The limits of detection and quantification in compost-amended soil samples were lower
than 0.03 and 0.10 mg/kg dry matter, respectively, for LAS; lower than 0.04 and 0.12 mg/kg dry matter, respectively, for NPE;
and 0.03 and 0.10 mg/kg dry matter, respectively, for DEHP. The method was successfully applied to compost and compost-amended
soil samples from Seville (south of Spain).
Figure Sampling in a compost pile
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3509-y
Authors
M. M. González, University of Seville Department of Analytical Chemistry C/ Virgen de África 7 41011 Seville Spain
J. L. Santos, University of Seville Department of Analytical Chemistry C/ Virgen de África 7 41011 Seville Spain
I. Aparicio, University of Seville Department of Analytical Chemistry C/ Virgen de África 7 41011 Seville Spain
E. Alonso, University of Seville Department of Analytical Chemistry C/ Virgen de África 7 41011 Seville Spain
Fourier transform Raman spectroscopy and chemometric tools have been used for exploratory analysis of pure corn and cassava
starch samples and mixtures of both starches, as well as for the quantification of amylose content in corn and cassava starch
samples. The exploratory analysis using principal component analysis shows that two natural groups of similar samples can
be obtained, according to the amylose content, and consequently the botanical origins. The Raman band at 480 cm−1, assigned to the ring vibration of starches, has the major contribution to the separation of the corn and cassava starch
samples. This region was used as a marker to identify the presence of starch in different samples, as well as to characterize
amylose and amylopectin. Two calibration models were developed based on partial least squares regression involving pure corn
and cassava, and a third model with both starch samples was also built; the results were compared with the results of the
standard colorimetric method. The samples were separated into two groups of calibration and validation by employing the Kennard-Stone
algorithm and the optimum number of latent variables was chosen by the root mean square error of cross-validation obtained
from the calibration set by internal validation (leave one out). The performance of each model was evaluated by the root mean
square errors of calibration and prediction, and the results obtained indicate that Fourier transform Raman spectroscopy can
be used for rapid determination of apparent amylose in starch samples with prediction errors similar to those of the standard
method.
Figure Raman spectroscopy has been successfully applied to the determination of the amylose content in cassava and corn starches
by means of multivariate calibration analysis.
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3566-2
Authors
Mariana R. Almeida, Universidade Federal de Juiz de Fora Núcleo de Espectroscopia e Estrutura Molecular (NEEM), Departamento de Química 36036-330 Juiz de Fora MG Brazil
Rafael S. Alves, Universidade Federal de Juiz de Fora Núcleo de Espectroscopia e Estrutura Molecular (NEEM), Departamento de Química 36036-330 Juiz de Fora MG Brazil
Laura B. L. R. Nascimbem, Instituto de Química, UNICAMP Laboratório de Quimiometria em Química Analítica (LAQQA) cx. Postal 6154 13083-970 Campinas SP Brazil
Rodrigo Stephani, Gemacom Comércio e Serviços LTDA 36092-050 Juiz de Fora MG Brazil
Ronei J. Poppi, Instituto de Química, UNICAMP Laboratório de Quimiometria em Química Analítica (LAQQA) cx. Postal 6154 13083-970 Campinas SP Brazil
Luiz Fernando C. de Oliveira, Universidade Federal de Juiz de Fora Núcleo de Espectroscopia e Estrutura Molecular (NEEM), Departamento de Química 36036-330 Juiz de Fora MG Brazil
This paper describes a method for determination of 27 mycotoxins and other secondary metabolites in maize silage. The method
focuses on analytes which are known to be produced by common maize and maize-silage contaminants. A simple pH-buffered sample
extraction was developed on the basis of a very fast and simple method for analysis of multiple pesticide residues in food
known as QuEChERS. The buffering effectively ensured a stable pH in samples of both well-ensiled maize (pH < 4) and of hot
spots with fungal infection (pH > 7). No further clean-up was performed before analysis using liquid chromatography–tandem
mass spectrometry. The method was successfully validated for determination of eight analytes qualitatively and 19 quantitatively.
Matrix-matched calibration standards were used giving recoveries ranging from 37% to 201% with the majority between 60% and
115%. Repeatability (5–27% RSDr) and intra-laboratory reproducibility (7–35% RSDIR) was determined. The limit of detection (LOD) for the quantitatively validated analytes ranged from 1 to 739 µg kg−1. Validation results for citrinin, fumonisin B1 and fumonisin B2 were unsatisfying. The method was applied to 20 selected silage samples and alternariol monomethyl ether, andrastin A, alternariol,
citreoisocoumarin, deoxynivalenol, enniatin B, fumigaclavine A, gliotoxin, marcfortine A and B, mycophenolic acid, nivalenol,
roquefortine A and C and zearalenone were detected.
Maize silage fed to cows can be contaminated with mycotoxins from pre- and post-harvest fungi. Several metabolites were detected
by LC-MS/MS; including zearalenone and mycophenolic acid from Fusarium (red) and Penicillium (green) infections, respectively.
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3545-7
Authors
R. R. Rasmussen, Technical University of Denmark National Food Institute, Division of Food Chemistry Mørkhøj Bygade 19 DK-2860 Søborg Denmark
I. M. L. D. Storm, Technical University of Denmark Center for Microbial Biotechnology, Department of Systems Biology Building 221 DK-2800 Kgs. Lyngby Denmark
P. H. Rasmussen, Technical University of Denmark National Food Institute, Division of Food Chemistry Mørkhøj Bygade 19 DK-2860 Søborg Denmark
J. Smedsgaard, Technical University of Denmark National Food Institute, Division of Food Chemistry Mørkhøj Bygade 19 DK-2860 Søborg Denmark
K. F. Nielsen, Technical University of Denmark Center for Microbial Biotechnology, Department of Systems Biology Building 221 DK-2800 Kgs. Lyngby Denmark
This study investigated the occurrence of tetracyclines (TCs), namely minocycline (MIN), TC, and its epimer epitetracycline
(ETC), and doxycycline (DC), in four hospital wastewater effluents and its fate in municipal wastewater treatment plants (WWTPs),
in Coimbra, Portugal. Analytical determination was carried out by solid-phase extraction followed by liquid chromatography
with fluorescence detection. A gradient system with a mobile phase containing oxalic acid 0.02 M and acetonitrile was used.
After postcolumn derivatization with magnesium reagent, TCs were detected at λexc 386 nm and λem 500 nm. The proposed method allowed good sensitivity, accuracy, and precision. LOQs were 0.5 μg l−1 for ETC and TC and 15 and 5 μg l−1 for MIN and DC, respectively. The recovery values ranged between 66.4% and 117.1%, and intraday and interday repeatability
was lower than 6.8%. The method was successfully used to determine the presence of the above-mentioned TCs in 24 wastewater
composite samples obtained from hospital effluents and from influent and effluent of the WWTP located in Coimbra, Portugal.
MIN and TC were found in 41.7% of the samples; ETC and DC were found in 25% and 8.3% of the samples, respectively. The levels
found ranged from 6 to 531.7 μg l−1 in hospital effluents, while its concentrations in WWTP ranged from 95.8 to 915.3 μg l−1. A seasonal influence in the concentrations found has also been observed, the levels found in samples collected during spring
being higher than those observed in samples collected during autumn; however, these are only preliminary results. The WWTP
removal rate ranged between 89.5% and 100%.
Content Type Journal Article
Category Paper in Forefront
DOI 10.1007/s00216-010-3581-3
Authors
A. Pena, University of Coimbra Group of Health Surveillance, CEF, Faculty of Pharmacy Health Sciences Campus, Azinhaga de Santa Comba 3000-548 Coimbra Portugal
M. Paulo, University of Coimbra Group of Health Surveillance, CEF, Faculty of Pharmacy Health Sciences Campus, Azinhaga de Santa Comba 3000-548 Coimbra Portugal
L. J. G. Silva, University of Coimbra Group of Health Surveillance, CEF, Faculty of Pharmacy Health Sciences Campus, Azinhaga de Santa Comba 3000-548 Coimbra Portugal
M. Seifrtová, Charles University Department of Analytical Chemistry, Faculty of Pharmacy 500 38 Hradec Králové 1 Czech Republic
C. M. Lino, University of Coimbra Group of Health Surveillance, CEF, Faculty of Pharmacy Health Sciences Campus, Azinhaga de Santa Comba 3000-548 Coimbra Portugal
P. Solich, Charles University Department of Analytical Chemistry, Faculty of Pharmacy 500 38 Hradec Králové 1 Czech Republic
A highly sensitive procedure for the efficient routine control of aromatic amines derived from banned azo dyes in textile
and leather products was developed and optimized. The procedure involves the extraction and reduction of azo dyes from solid
samples following the sample preparation protocols outlined in EN 14362-1:2003, EN 14362-2:2003, and ISO/TS 17234:2003 standards,
and cleanup and concentration of aromatic amines by solid-phase extraction, with Oasis HLB and ENVI-Carb sorbents in series.
The elution was carried out with the cartridges connected in series, although the positions of the cartridges were reversed
and the ENVI-Carb cartridge was placed in the backflush mode. Extracted and concentrated aromatic amines were separated and
analyzed by liquid chromatography (LC)–tandem mass spectrometry (MS). The chromatographic separation was optimized by means
of computer-assisted method development with a special chemometric tool (the PREGA LC-MS module), developed specifically for
LC-MS systems. This system enables the unattended optimization of separations after a few priming isocratic and gradient experiments.
The optimized separation program enables accurate detection and measurement of all the 23 aromatic amines considered, at very
low quantification limits and without any notable matrix effects. Strategic sample composition was applied as an efficient
means of reducing the costs and work involved in the control of aromatic amines in finished textile and leather products.
The benefits of strategic sample composition are demonstrated by means of a case study of 20 sample specimens.
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3574-2
Authors
J. García-Lavandeira, University of Santiago de Compostela Department of Analytical Chemistry, Food Analysis Research Institute 15782 Santiago de Compostela Spain
C. Salgado-Petinal, University of Santiago de Compostela Department of Analytical Chemistry, Food Analysis Research Institute 15782 Santiago de Compostela Spain
E. Blanco, University of Santiago de Compostela Department of Analytical Chemistry, Food Analysis Research Institute 15782 Santiago de Compostela Spain
R. Cela, University of Santiago de Compostela Department of Analytical Chemistry, Food Analysis Research Institute 15782 Santiago de Compostela Spain
Magnesium (Mg) as a biodegradable metal has potential advantages as an implant material. This paper studies the effect of
magnesium ions on osteoblast (U2-OS) behavior since magnesium implants mainly dissolve as divalent magnesium ions (Mg2+). A real-time monitoring technique based on electric cell-substrate impedance sensing (ECIS) was used for measuring cell
proliferation, migration, adhesion, and cytotoxicity in magnesium-conditioned media. The impedance results show that U2-OS
proliferation and adhesion were inhibited in not only a magnesium-free medium but also in a medium with a high concentration
of magnesium. The impedance method produced more sensitive results than the output of an MTT assay. Other standard bioanalytical
tests were conducted for comparison with the ECIS method. Immunochemistry was carried out to study cell adhesion in magnesium-conditioned
media by staining using F-actin and α-tubulin and correlated cell density on the electrode with impedance. Bone tissue formation
was studied using von Kossa staining and indicated the mineralization level of cells in magnesium-conditioned media decreased
with the increase of magnesium ion concentration. Real-time PCR provided gene expression indicators of cell growth, apoptosis,
inflammation, and migration. Compared to the bioanalytical methods of immunochemistry and MTT assays, which need preparation
time and post-washing step, ECIS was able to measure cell activity in real time without any cell culture modification. In
summary, ECIS might be an effective way to study biodegradable magnesium implants.
Figure Principle of ECIS for analyzing U2-OS cell behavior under different concentrations of magnesium: a osteoblast cells are floating in the medium and the electrode impedance is small; and b osteoblast cells create a monolayer on the electrode which increases the impedance
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3521-2
Authors
YeoHeung Yun, University of Cincinnati Smart Materials Nanotechnology Laboratory, Dept. of Mechanical Engineering Smart Materials Nanotechnology Lab, 598 Rhodes Hall Cincinnati OH 45221-0072 USA
Zhongyun Dong, University of Cincinnati Department of Internal Medicine, College of Medicine Cincinnati OH 45221 USA
Zongqing Tan, University of Cincinnati Department of Internal Medicine, College of Medicine Cincinnati OH 45221 USA
Mark J. Schulz, University of Cincinnati Smart Materials Nanotechnology Laboratory, Dept. of Mechanical Engineering Smart Materials Nanotechnology Lab, 598 Rhodes Hall Cincinnati OH 45221-0072 USA
Homocysteine thiolactone modification is a unique process of posttranslational protein modification as well as a significant
clinical indicator of cardiovascular and neurovascular diseases, so we report a new method in this paper to sensitively monitor
such a modification using horse heart cytochrome c as a model protein. After the modification has been confirmed by UV–vis spectroscopy and ESI-MS, N-linked cytochrome c is then covalently assembled onto the surface of a gold electrode via the resulted homocysteine thiol group, thus electrochemical
techniques, especially differential pulse voltammetry, have been employed and proven to provide an efficient way to probe
into the modification of the protein. While the immobilized protein can exhibit well-defined voltammetric response, the signal
of the modified cytochrome c is positively correlated to the concentration of homocysteine-thiolactone. The detectable electrochemical signal can be attained
with the minimum concentration of 5 × 10−5 M homocysteine-thiolactone. Furthermore, screening of N-homocysteinylation inhibitors can be also feasible since the electrochemical waves linearly decrease with the concentration
of an inhibitor pyridoxal 5-phosphate. The limit of detection for the inhibitors can be about 1 × 10−5 M.
Figure Schematic illustration of the electrochemical method to probe into the modification of cytochrome c with homocysteine-thiolactone
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3553-7
Authors
Jing Zhao, Nanjing University Department of Biochemistry and National Key Laboratory of Pharmaceutical Biotechnology Nanjing 210093 China
Wei Zhu, Nanjing University Department of Biochemistry and National Key Laboratory of Pharmaceutical Biotechnology Nanjing 210093 China
Tao Liu, Nanjing University Department of Biochemistry and National Key Laboratory of Pharmaceutical Biotechnology Nanjing 210093 China
Jinghua Yang, Nanjing University Department of Biochemistry and National Key Laboratory of Pharmaceutical Biotechnology Nanjing 210093 China
Genxi Li, Nanjing University Department of Biochemistry and National Key Laboratory of Pharmaceutical Biotechnology Nanjing 210093 China
Development of sustainable materials requires methods capable of probing the molecular composition of samples not only at
the surface but also in depth. Static secondary ion mass spectrometry (S-SIMS) characterises the distribution of organic and
inorganic compounds at the surface. Ultra-low-angle microtomy (ULAM) has been studied as an alternative or complementing method
to the molecular depth profiling with, e.g. C60+ projectiles. Acrylate-based multilayers relevant to industrial inkjet printing have been sectioned at a cutting angle below
1°. In this way, analysis of the section over a distance of 1 µm allows a depth range in the order of a few nm in the original
sample to be achieved. Adequate procedures to optimise the ULAM step and minimise or control the cutting artefacts have been
developed. The combination of ULAM with S-SIMS has allowed a depth resolution of 10 nm to be obtained for components at a
distance of 35 μm from the surface.
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3507-0
Authors
Yannick Vercammen, MiTAC, University of Antwerp Department of Chemistry (CDE) Universiteitsplein 1 2610 Wilrijk Belgium
Roel De Mondt, MiTAC, University of Antwerp Department of Chemistry (CDE) Universiteitsplein 1 2610 Wilrijk Belgium
Arsenate [As(V)] solution reference material, National Metrology Institute of Japan (NMIJ) certified reference material (CRM)
7912-a, for speciation of arsenic species was developed and certified by NMIJ, the National Institute of Advanced Industrial
Science and Technology. High-purity As2O3 reagent powder was dissolved in 0.8 M HNO3 solution and As(III) was oxidized to As(V) with HNO3 to prepare 100 mg kg-1 of As(V) candidate CRM solution. The solution was bottled in 400 bottles (50 mL each). The concentration of As(V) was determined
by four independent analytical techniques—inductively coupled plasma mass spectrometry, inductively coupled plasma optical
emission spectrometry, graphite furnace atomic absorption spectrometry, and liquid chromatography inductively coupled plasma
mass spectrometry—according to As(V) calibration solutions, which were prepared from the arsenic standard of the Japan Calibration
Service system and whose species was guaranteed to be As(V) by NMIJ. The uncertainties of all the measurements and preparation
procedures were evaluated. The certified value of As(V) in the CRM is (99.53 ± 1.67) mg kg-1 (k = 2).
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3564-4
Authors
Tomohiro Narukawa, National Institute of Advanced Industrial Science and Technology (AIST) Environmental Standard Section, National Metrology Institute of Japan (NMIJ) Tsukuba Central 3, 1-1-1 Umezono, Tsukuba Ibaraki 305-8563 Japan
Takayoshi Kuroiwa, National Institute of Advanced Industrial Science and Technology (AIST) Environmental Standard Section, National Metrology Institute of Japan (NMIJ) Tsukuba Central 3, 1-1-1 Umezono, Tsukuba Ibaraki 305-8563 Japan
Izumi Narushima, National Institute of Advanced Industrial Science and Technology (AIST) Environmental Standard Section, National Metrology Institute of Japan (NMIJ) Tsukuba Central 3, 1-1-1 Umezono, Tsukuba Ibaraki 305-8563 Japan
Yasujiro Jimbo, National Institute of Advanced Industrial Science and Technology (AIST) Environmental Standard Section, National Metrology Institute of Japan (NMIJ) Tsukuba Central 3, 1-1-1 Umezono, Tsukuba Ibaraki 305-8563 Japan
Toshihiro Suzuki, National Institute of Advanced Industrial Science and Technology (AIST) Environmental Standard Section, National Metrology Institute of Japan (NMIJ) Tsukuba Central 3, 1-1-1 Umezono, Tsukuba Ibaraki 305-8563 Japan
Koichi Chiba, National Institute of Advanced Industrial Science and Technology (AIST) Environmental Standard Section, National Metrology Institute of Japan (NMIJ) Tsukuba Central 3, 1-1-1 Umezono, Tsukuba Ibaraki 305-8563 Japan
A simple and fast microwave-assisted-extraction (MAE) method has been evaluated as an alternative to solid-phase extraction
(SPE) for the determination of six benzodiazepines widely prescribed in European countries (alprazolam, bromazepam, diazepam,
lorazepam, lormetazepam and tetrazepam) in human plasma. For MAE optimization a Doehlert experimental design was used with
extraction time, temperature and solvent volume as influential parameters. A desirability function was employed in addition
to the simultaneous optimization of the MAE conditions. The analysis of variance showed that the solvent volume had a positive
influence on the extraction of all the analytes tested, achieving a statistically significant effect. Also, the extraction
time had a statistically significant effect on the extraction of four benzodiazepines. The selected MAE conditions—89 °C,
13 min and 8 mL of chloroform/2-propanol (4:1, v/v)—led to recoveries between 89.8 ± 0.3 and 102.1 ± 5.2% for benzodiazepines
using a high performance liquid chromatography method coupled with diode-array detection. The comparison of MAE and SPE shows
better results for MAE, with a lower number of steps in handling the sample and greater efficiency. The applicability of MAE
was successfully tested in 27 plasma samples from benzodiazepine users.
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3572-4
Authors
P. Fernández, Faculty of Medicine Institute of Legal Medicine, Forensic Toxicology Service 15782 Santiago de Compostela Spain
C. Vázquez, Faculty of Medicine Institute of Legal Medicine, Forensic Toxicology Service 15782 Santiago de Compostela Spain
R. A. Lorenzo, Faculty of Chemistry Department of Analytical Chemistry 15782 Santiago de Compostela Spain
A. M. Carro, Faculty of Chemistry Department of Analytical Chemistry 15782 Santiago de Compostela Spain
I. Álvarez, Faculty of Medicine Institute of Legal Medicine, Forensic Toxicology Service 15782 Santiago de Compostela Spain
P. Cabarcos, Faculty of Medicine Institute of Legal Medicine, Forensic Toxicology Service 15782 Santiago de Compostela Spain
The effect of repassivation on tribocorrosion behaviour of two multilayer coatings of different structures is studied experimentally
by measuring the variation of instantaneous open-circuit potential during friction. One coating consists of alternating Cr
and CrN layers, while another consists of alternated layers of CrN and ZrN. Analysis of the results showed that friction force,
i.e. the rate of the mechanical energy supplied to the material in the contact zone, has no direct influence on the tribocorrosion
behaviour; however, the wear rate does strongly influence the tribocorrosion. A simple phenomenological model of repassivation
of the multilayer coating is developed assuming “surface coverage” approach. This model establishes the relationship between
the rate of mechanical activation of material by friction and the behaviour of the open-circuit potential.
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3538-6
Authors
R. Bayón, Fundación Tekniker Avda. Otaola, 20 20600 Eibar Spain
R. Nevshupa, Fundación Tekniker Avda. Otaola, 20 20600 Eibar Spain
C. Zubizarreta, Fundación Tekniker Avda. Otaola, 20 20600 Eibar Spain
U. Ruiz de Gopegui, Fundación Tekniker Avda. Otaola, 20 20600 Eibar Spain
J. Barriga, Fundación Tekniker Avda. Otaola, 20 20600 Eibar Spain
A. Igartua, Fundación Tekniker Avda. Otaola, 20 20600 Eibar Spain
Cobalt phthalocyanine-modified screen-printed carbon electrodes (CoPC-SPCEs) have been investigated as disposable sensors
for the measurement of citric acid. The analyte was found to undergo an electrocatalytic oxidation process involving the Co2+/Co3+ redox couple. Calibration plots were found to be linear in the range 2 mM to 2.0 M; replicate determinations of a 5.2 mM
citric acid (n = 4) solution gave a coefficient of variation of 1.43%. Additions of metal ions, such as Ag+, Pb2+, Cu2+, Fe3+ and Ca2+, were found not to interfere. The effects of hesperidin, cysteine, ethylenediaminetetraacetic acid (EDTA), ascorbic, formic,
malic, malonic, tartaric, oxalic and trichloroacetic acids on the determination of citric acid were examined and, under the
conditions employed, only oxalic acid and EDTA were found to give any significant interference. The sensors were evaluated
by carrying out citric acid determinations on spiked and unspiked samples of an acid citrate dextrose (ACD) formulation, lime
flesh and juice. For lime juice, recoveries were calculated to be 96.8% (% CV = 2.7%) for a sample fortified with 5% citric
acid and for ACD 99.4% (%CV = 2.6%) when fortified at 2.30% citric acid. Further studies showed the possibility of determining
citric acid concentrations in lime juice and fruit directly, without the need for an added electrolyte. These performance
characteristics indicate that reliable data may be obtained for citric acid measurements in such samples. To our knowledge,
this is the first report on the electrocatalytic oxidation of citric acid and its application using a CoPC-SPCE.
Figure Direct measurement of citric acid in limes based on the electrocatalytic oxidation of the analyte at a screen-printed carbon
electrode modified with cobalt phthalocyanine.
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3534-x
Authors
Kevin C. Honeychurch, University of the West of England, Bristol Centre for Research in Analytical, Materials and Sensors Science Frenchay Campus, Coldharbour Lane Bristol BS16 1QY UK
Lucy Gilbert, University of the West of England, Bristol Centre for Research in Analytical, Materials and Sensors Science Frenchay Campus, Coldharbour Lane Bristol BS16 1QY UK
John P. Hart, University of the West of England, Bristol Centre for Research in Analytical, Materials and Sensors Science Frenchay Campus, Coldharbour Lane Bristol BS16 1QY UK
The development of tissue micro-array (TMA) technologies provides insights into high-throughput analysis of proteomics patterns
from a large number of archived tumour samples. In the work reported here, matrix-assisted laser desorption/ionisation–ion
mobility separation–mass spectrometry (MALDI–IMS–MS) profiling and imaging methodology has been used to visualise the distribution
of several peptides and identify them directly from TMA sections after on-tissue tryptic digestion. A novel approach that
combines MALDI–IMS–MSI and principal component analysis–discriminant analysis (PCA–DA) is described, which has the aim of
generating tumour classification models based on protein profile patterns. The molecular classification models obtained by
PCA–DA have been validated by applying the same statistical analysis to other tissue cores and patient samples. The ability
to correlate proteomic information obtained from samples with known and/or unknown clinical outcome by statistical analysis
is of great importance, since it may lead to a better understanding of tumour progression and aggressiveness and hence improve
diagnosis, prognosis as well as therapeutic treatments. The selectivity, robustness and current limitations of the methodology
are discussed.
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3554-6
Authors
Marie-Claude Djidja, Sheffield Hallam University Biomedical Research Centre Howard Street Sheffield S1 1WB UK
Emmanuelle Claude, Waters Corporation Manchester M23 9LZ UK
Marten F. Snel, Lysosomal Diseases Research Unit, SA Pathology North Adelaide SA 5006 Australia
Simona Francese, Sheffield Hallam University Biomedical Research Centre Howard Street Sheffield S1 1WB UK
Peter Scriven, University of Sheffield Academic Surgical Oncology Unit Sheffield S3 7ND UK
Vikki Carolan, Sheffield Hallam University Biomedical Research Centre Howard Street Sheffield S1 1WB UK
Malcolm R. Clench, Sheffield Hallam University Biomedical Research Centre Howard Street Sheffield S1 1WB UK
The qualitative and quantitative analysis of aflatoxin B1 in a model system (water/ethanol), in different wines and in beer using one- and two-photon-induced fluorescence is discussed.
The absorption and fluorescence properties of aflatoxin B1 depend on the solvent and pH. The two-photon-absorption cross-section was calculated for aflatoxin B1 in beer and wine (σ2 ∼ 25 GM) for excitation at 720 nm. A comparison of the one- and two-photon- induced fluorescence results showed that the
disturbance due to background emission originating from matrix constituents is significantly reduced under two-photon-excitation
conditions. The limit of detection for the one- and two-photon-induced fluorescence was determined.
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3530-1
Authors
Claudia Rasch, University of Potsdam Department of Chemistry (Physical Chemistry) Karl-Liebknecht-Str. 24–25 14476 Potsdam-Golm Germany
Maike Böttcher, University of Potsdam Department of Chemistry (Physical Chemistry) Karl-Liebknecht-Str. 24–25 14476 Potsdam-Golm Germany
Michael Kumke, University of Potsdam Department of Chemistry (Physical Chemistry) Karl-Liebknecht-Str. 24–25 14476 Potsdam-Golm Germany
Haiwei Gu, Bin Hu, Jianqiang Li, Shuiping Yang, Jing Han, Huanwen Chen
(Paper from Analyst)
Haiwei Gu, Analyst, 2010, DOI: 10.1039/b923991j
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Franco Basile, Shaofeng Zhang, Yong-Seung Shin, Barbara Drolet
(Paper from Analyst)
Franco Basile, Analyst, 2010, DOI: 10.1039/c0an00071j
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Analyst, 2010, DOI: 10.1039/c003812c
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Martina Sattlecker, Conrad Bessant, Jennifer Smith, Nick Stone
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Martina Sattlecker, Analyst, 2010, DOI: 10.1039/b920229c
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M. J. Baker, C. Clarke, D. Demoulin, J. M. Nicholson, F. M. Lyng, H. J. Byrne, C. A. Hart, M. D. Brown, N. W. Clarke, P. Gardner
(Paper from Analyst)
M. J. Baker, Analyst, 2010, DOI: 10.1039/b920385k
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Hong Lin Zhai, Ya Ting Chang, Chih Ching Wu, Jau Song Yu
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Hong Lin Zhai, Analyst, 2010, DOI: 10.1039/b927473a
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Yan Pan, Lars Konermann
(Critical Review from Analyst)
Yan Pan, Analyst, 2010, DOI: 10.1039/b924805f
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Two reference materials, at relatively low and high concentrations (GBW08404 and GBW08405), for analysis of the mass fractions
of Cd, Cr, Hg and Pb in polypropylene were developed. The reference materials were prepared by doping blank polypropylene
base material with Cd, Cr, Hg and Pb in the form of oxides, salts or pigments. Homogeneity and stability studies were performed
by inductively coupled plasma mass spectrometry. The certification of the four analytes was carried out by isotope-dilution
mass spectrometry (IDMS) with microwave-assisted digestion. Combined uncertainties were calculated from the IDMS uncertainty
evaluation budget and the uncertainty of the homogeneity. The mass fractions of Cd, Cr, Hg and Pb of the two certified reference
materials (CRMs) were from 8 to 1,000 mg kg−1. The two samples were also used in an interlaboratory comparison scheme in which National Institute of Metrology, China,
National Metrological Institute of Japan and Korea Research Institute of Standards and Science participated. The agreement
of the comparison results proved that the certification procedure of the CRMs is valid and that the certified values of Cd,
Cr, Hg and Pb are accurate and reliable.
Figure Certified reference materials for Cd, Cr, Hg and Pb in polypropylene (GBW08404 and GBW08405)
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3514-1
Authors
Liuxing Feng, National Institute of Metrology Division of Metrology in Chemistry Beijing 100013 China
Liandi Ma, National Institute of Metrology Division of Metrology in Chemistry Beijing 100013 China
Jun Wang, National Institute of Metrology Division of Metrology in Chemistry Beijing 100013 China
Hai Lu, National Institute of Metrology Division of Metrology in Chemistry Beijing 100013 China
The analysis of total carbon dioxide (TCO2) in equine plasma is conventionally done in Australia and elsewhere using Beckman Synchron EL-ISE® analysers. This instrument is no longer being manufactured and has not been supported by the supplier since December 2008.
For testing for TCO2 to continue, it is necessary to evaluate and commission alternative instrumentation. In this paper, we compare the Beckman
Synchron EL-ISE®, the Beckman Synchron CX®5, the Beckman UniCel DxC®600 and the Randox Daytona™ instruments. Results indicate that all four
instruments perform in accordance with the manufacturer’s specifications. The Beckman CX 5, DxC 600 and Randox Daytona instruments
are therefore all suitable alternatives for routine screening in a laboratory environment. Only the Randox Daytona instrument
is sufficiently ‘portable’, i.e. it can be readily transported and used on-site at a racecourse (typically in a purpose-built
modest-size laboratory vehicle). The three Beckman instruments are suitable for ‘confirmatory analysis’ using the quality-accredited
method (Racing Science Centre), but the principle of operation of the Randox Daytona instrument may preclude its use in confirmatory
analysis. Instrument costs may affect purchase decisions.
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3543-9
Authors
Mark Jarrett, Racing Science Centre P.O. Box 513 Albion Queensland 4010 Australia
D. Brynn Hibbert, University of New South Wales School of Chemistry Sydney NSW 2052 Australia
Roy Osborne, Racing Science Centre P.O. Box 513 Albion Queensland 4010 Australia
E. Bruce Young, Racing Science Centre P.O. Box 513 Albion Queensland 4010 Australia
The use of municipal biosolids as agricultural fertilisers has raised significant concerns in recent years. As part of this,
the presence of complex mixtures of pharmaceutical residues and their effects on soil ecosystems remains particularly under-researched.
This study focuses on the transfer of a selection of pharmaceutical residues from municipal sewage sludge to agricultural
topsoils and their fate therein after an accelerated 6-month rainfall event. Twelve pharmaceuticals encompassing antibiotics,
analgesics, anti-inflammatories, beta-blockers, hyperlipidaemics and stimulants were invesigated by employing a combination
of extraction techniques and liquid chromatography-tandem mass spectrometry. Both liquid- and solid-phase pharmaceutical contents
were analysed and pharmaceutical and personal care products quantified at defined timepoints to elucidate transport behaviour
and transformation potential. Results show the distribution and separation of pharmaceuticals over a 100-mm soil depth following
typical biosolid enrichment. Using experimentally determined solid–water partition coefficients (Kd) and hydrophobicity distribution ratios (Dow), mobility and modes of interaction under dynamic conditions are discussed. Finally, a brief study into the susceptibility
of soil microbes is also presented. To our knowledge, this is the first investigation of pharmaceutical and personal care
products release from amended biosolids to soils to include the factors and mechanisms governing their distribution and transformation
even over relatively shallow depths. It applies multicompartmental and mass-balanced chemical analyses as well as microbiological
approaches for a holistic view of these complex processes.
Figure Transport behaviour and fate of pharmaceuticals in biosolid enriched topsoils
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3494-1
Authors
Leon Barron, King’s College London Department of Forensic Science & Drug Monitoring, Pharmaceutical Science Division, Franklin-Wilkins Building 150 Stamford Street London SE1 9NH UK
Ekaterina Nesterenko, Dublin City University Irish Separation Science Cluster, National Centre for Sensor Research Glasnevin Dublin 9 Republic of Ireland
Kris Hart, Dublin City University School of Chemical Sciences Glasnevin Dublin 9 Republic of Ireland
Emma Power, Galway-Mayo Institute of Technology Irish Centre for Environmental Toxicology Galway Republic of Ireland
Brian Quinn, Galway-Mayo Institute of Technology Irish Centre for Environmental Toxicology Galway Republic of Ireland
Brian Kelleher, Dublin City University School of Chemical Sciences Glasnevin Dublin 9 Republic of Ireland
Brett Paull, Dublin City University Irish Separation Science Cluster, National Centre for Sensor Research Glasnevin Dublin 9 Republic of Ireland
The analytical detection of chlorophenoxycarboxylic-acid-type herbicides (2,4-D, dichloprop, MCPA, etc.) in environmental
samples is often a problem in instrumental analysis, as these compounds containing free carboxylic groups require chemical
derivatisation prior to gas chromatographic (GC) methods. Nine chlorophenoxy-acid-type herbicide active ingredients have been
derivatised successfully with trimethylsilyl N,N-dimethyl carbamate and t-butyldimethylsilyl N,N-dimethyl carbamate by forming their trimethylsilyl (TMS) and t-butyldimethylsilyl (TBDMS) esters, respectively. The detection and determination of the derivatives were performed by capillary
gas chromatography–mass spectrometry. The study included determination of retention indices, mass spectral properties and
comparison of derivatives produced. The mass spectra of TBDMS derivatives are usually dominated by very characteristic ions
[M-57]+ resulting from the cleavage of t-butyl moiety during electron impact (EI) ionisation in the mass spectrometer. Limits of detection were 5 to 100 pg applying
GC with EI-MS detection in full scan mode. The method, using SPE sample preparation, was applied for the analysis of 115 ground
water and surface water samples collected in Békés County, Hungary in 2009.
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3486-1
Authors
Erik Maloschik, Plant Protection Institute, Hungarian Academy of Sciences Department of Ecotoxicology and Environmental Analysis 1022 Budapest Herman O. u. 15 Hungary
Mária Mörtl, Plant Protection Institute, Hungarian Academy of Sciences Department of Ecotoxicology and Environmental Analysis 1022 Budapest Herman O. u. 15 Hungary
András Székács, Plant Protection Institute, Hungarian Academy of Sciences Department of Ecotoxicology and Environmental Analysis 1022 Budapest Herman O. u. 15 Hungary
A comprehensive method was developed for the simultaneous trace analysis of ten hormone antagonist pharmaceuticals (raloxifene,
exemestane, letrozole, anastrozole, mifepristone, finastride, tamoxifen, N-desmethyltamoxifen, clomiphene, and toremifene) in municipal sewage and hospital wastewater samples. The target compounds
were firstly extracted using an Oasis HLB cartridge, followed by purification by an aminopropyl cartridge, and were then analyzed
by liquid chromatography electrospray ionization tandem mass spectrometry in positive ion mode. The recoveries for the analytes
based on internal standard calibration in different test matrices ranged from 67.6 to 118.6% (with the exception of mifepristone
in clinical wastewater samples), with relative standard deviations less than 20%. The method quantification limits of the
ten pharmaceuticals were in the range 0.10–2.0 ng/L. Excluding exemestane and N-desmethyltamoxifen, eight drugs were detected at 0.20–195.0 ng/L in hospital wastewater and municipal wastewater samples
from Beijing.
Figure Analysis of hormone antagonists in clinical and municipal wastewater by liquid chromatography tandem mass spectrometry
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3531-0
Authors
Xianjun Liu, Beijing Center for Disease Control & Prevention Central Laboratory Beijing 100013 China
Jing Zhang, Beijing Center for Disease Control & Prevention Central Laboratory Beijing 100013 China
Jie Yin, Beijing Center for Disease Control & Prevention Central Laboratory Beijing 100013 China
Hejun Duan, Beijing Center for Disease Control & Prevention Central Laboratory Beijing 100013 China
Yongning Wu, China Center for Disease Control & Prevention Institute of Nutrition and Food Safety Beijing 100021 China
Bing Shao, Beijing Center for Disease Control & Prevention Central Laboratory Beijing 100013 China
A simplified method for the measurement of proteases utilising solid-phase substrates incorporating an ELISA end-point detection
step is described. Gelatin–hapten conjugates adsorbed onto polystyrene surfaces were found to be efficient substrates for
proteases. Digestion of the solid-phase protein–hapten complexes resulted in proportional desorption of the attached conjugates
and decrease in the detectable hapten species. Gelatin–cholic acid conjugates, affinity-purified sheep anti-cholic acid antibody–HRP
and a chromogenic substrate were incorporated into a convenient and highly sensitive solid-phase immunochemical method. The
detectable signal is inversely proportional to enzyme activity. Bacterial proteases (alpha-chymotrypsin Type II, Type IX from
Bacillus polymyxa, Type XIV from Streptomyces griseus, Type XXIV from Bacillus licheniformens) were assayed. Dose–response curves for enzyme activities were measured within ranges of 0–550 µunits mL−1 for chymotrypsin, 0–12 µunits mL−1 for type IX, 0–35 µunits mL−1 for type XIV and 0–100 µunits mL−1 for type XXIV. The detection limits of the proteases studied were 89 µunits mL−1 for chymotrypsin, 0.26 µunits mL−1 for type IX, 5.8 µunits mL−1 for type XIV and 6.5 µunits mL−1 for type XXIV. It was demonstrated that the two-step immunochemical method combines the simplicity and sensitivity of solid-phase
enzyme immunoassays, the broad specificity of gelatin as a protease substrate and the flexibility of the solid-phase format.
Effect of increasing hapten density on the hydrolysis of gelatin–hapten conjugates by proteinase
Content Type Journal Article
Category Paper in Forefront
DOI 10.1007/s00216-010-3540-z
Authors
Ramadan A. Abuknesha, King’s College London, University of London Analytical Sciences Research Group, Pharmaceutical Science Research Division, School of Biomedical & Health Sciences 150 Stamford St. London SE1 9NH UK
Fiona Jeganathan, King’s College London, University of London Analytical Sciences Research Group, Pharmaceutical Science Research Division, School of Biomedical & Health Sciences 150 Stamford St. London SE1 9NH UK
Rens DeGroot, Imperial College London, South Kensington Campus Division of Investigative Science London SW7 2AZ UK
Dirk Wildeboer, King’s College London, University of London Analytical Sciences Research Group, Pharmaceutical Science Research Division, School of Biomedical & Health Sciences 150 Stamford St. London SE1 9NH UK
Robert G. Price, King’s College London, University of London Analytical Sciences Research Group, Pharmaceutical Science Research Division, School of Biomedical & Health Sciences 150 Stamford St. London SE1 9NH UK
A validated method based on liquid chromatography/positive ion electrospray–mass spectrometry (LC-ESI/MS) is described for
the quantification of perindopril and its active metabolite, perindoprilat, in human plasma. The assay was based on 500-μL
plasma samples, following solid-phase extraction using Oasis HLB cartridges. All analytes and the internal standard (trandolapril)
were separated by hydrophilic interaction liquid chromatography using a SeQuant Zic-HILIC analytical column (150.0 × 2.1 mm
i.d., particle size 3.5 μm, 200 Å) with isocratic elution. The mobile phase consisted of 10% 5.0 mM ammonium acetate water
solution in a binary mixture of acetonitrile/methanol (60:40, v/v) and pumped at a flow rate of 0.10 mL min−1. Quantitation of the analytes was performed with selected ion monitoring (SIM) in positive ionization mode using electrospray
ionization interface. The assay was found to be linear in the concentration range of 5.0–500.0 ng mL−1 for perindopril and perindoprilat. Intermediate precision were found less than 3.5% over the tested concentration ranges.
A run time of less than 6.0 min for each sample made it possible to analyze a large number of human plasma samples per day.
The method is the first reported application of HILIC in the analysis of angiotensin-converting enzyme inhibitors and can
be used to quantify perindopril and perindoprilat in human plasma covering a variety of pharmacokinetic or bioequivalence
studies.
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3551-9
Authors
Sofia Georgakakou, University of Athens School of Pharmacy, Division of Pharmaceutical Chemistry Panepistimiopolis, Zografou 157 71 Athens Greece
Michael Kazanis, University of Athens School of Pharmacy, Division of Pharmaceutical Chemistry Panepistimiopolis, Zografou 157 71 Athens Greece
Irene Panderi, University of Athens School of Pharmacy, Division of Pharmaceutical Chemistry Panepistimiopolis, Zografou 157 71 Athens Greece
The temporal dynamics of Fas-induced apoptosis is elucidated. Jurkat cells are captured on the affinity surface of a microdevice
coated with anti-CD95, an antibody known to induce apoptosis in cells via the extrinsic (caspase 8) pathway. The timing of
apoptosis induction is controlled by the binding of the cells to the surface. Once bound, the cells are continuously stained
with the caspase probe, l-bisaspartic acid rhodamine 110 (D2R), and the fluorescence of the cells was monitored for 6 h by light microscopy. This approach normalizes the temporal dynamics
for each cell, as the binding event is also the start of apoptosis. In addition to providing the number of apoptotic cells
over time, the fluorescence of individual cells can be monitored, providing information about the timing of caspase activity
in each cell. The rate of caspase cleavage of D2R in each cell is also measured and shows good agreement between the cells in a given population. The effects of the caspase
inhibitor, z-VAD-FMK, on the timing of caspase activity are also investigated and are shown to dramatically slow the apoptotic
process. In the future, other caspase probes could be used to provide additional information about the temporal dynamics of
caspase activation. Additional techniques, such as fluorescence correlation spectroscopy, can be coupled to these methods
to provide faster temporal response and help to elucidate the heterogeneity of the apoptosis process.
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3567-1
Authors
Randall D. Reif, Texas Tech University Department of Chemistry and Biochemistry Lubbock TX 79409 USA
Charmaine Aguas, Texas Tech University Department of Chemistry and Biochemistry Lubbock TX 79409 USA
Michelle M. Martinez, Texas Tech University Department of Chemistry and Biochemistry Lubbock TX 79409 USA
Dimitri Pappas, Texas Tech University Department of Chemistry and Biochemistry Lubbock TX 79409 USA
Proteins are undoubtedly some of the most essential molecules of life. While much is known about many proteins, some aspects
still remain mysterious. One particularly important aspect of understanding proteins is determining how structure helps dictate
function. Continued development and implementation of biophysical techniques that provide information about protein conformation
and dynamics is essential. In this review, we discuss hydrogen exchange mass spectrometry and how this method can be used
to learn about protein conformation and dynamics. The basic concepts of the method are described, the workflow illustrated,
and a few examples of its application are provided.
Figure Analysis of deuterium incorporation into protein with mass spectrometry
Content Type Journal Article
Category Trends
DOI 10.1007/s00216-010-3556-4
Authors
Sean R. Marcsisin, Northeastern University The Department of Chemistry & Chemical Biology and The Barnett Institute of Chemical & Biological Analysis Boston MA 02115 USA
John R. Engen, Northeastern University The Department of Chemistry & Chemical Biology and The Barnett Institute of Chemical & Biological Analysis Boston MA 02115 USA
Demian R. Ifa, Chunping Wu, Zheng Ouyang, R. Graham Cooks
(Critical Review from Analyst)
Demian R. Ifa, Analyst, 2010, DOI: 10.1039/b925257f
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Daniel J. Weston
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Analytical Chemistry, Volume 0, Issue 0, Articles ASAP (As Soon As Publishable).
Analytical Chemistry, Volume 0, Issue 0, Articles ASAP (As Soon As Publishable).
Analytical Chemistry, Volume 0, Issue 0, Articles ASAP (As Soon As Publishable).