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Aktuelle wissenschaftliche Fachartikel der
genannten Journale:
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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The content of this RSS Feed (c) The Royal Society of Chemistry
Franco Basile, Shaofeng Zhang, Yong-Seung Shin, Barbara Drolet
(Paper from Analyst)
Franco Basile, Analyst, 2010, DOI: 10.1039/c0an00071j
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The content of this RSS Feed (c) The Royal Society of Chemistry
(Editorial from Analyst)
Analyst, 2010, DOI: 10.1039/c003812c
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The content of this RSS Feed (c) The Royal Society of Chemistry
Martina Sattlecker, Conrad Bessant, Jennifer Smith, Nick Stone
(Paper from Analyst)
Martina Sattlecker, Analyst, 2010, DOI: 10.1039/b920229c
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The content of this RSS Feed (c) The Royal Society of Chemistry
Hong Lin Zhai, Ya Ting Chang, Chih Ching Wu, Jau Song Yu
(Communication from Analyst)
Hong Lin Zhai, Analyst, 2010, DOI: 10.1039/b927473a
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The content of this RSS Feed (c) The Royal Society of Chemistry
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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The content of this RSS Feed (c) The Royal Society of Chemistry
Yan Pan, Lars Konermann
(Critical Review from Analyst)
Yan Pan, Analyst, 2010, DOI: 10.1039/b924805f
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The content of this RSS Feed (c) The Royal Society of Chemistry
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 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
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
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
A hydrophilic interaction chromatography-based method, in combination with 1.7 µm ethylene bridged hybrid particle packed
column (100 mm × 2.1 mm I.D.) and ultraperformance liquid chromatography, has been developed to measure cytosine (C) and methylcytosine
(mC) in order to evaluate the extent of DNA methylation. Separation of cytosine and methylcytosine was achieved with good
resolution and in fairly short times (5.5 min) by using isocratic elution with a mixture of 97:3 (v/v) acetonitrile/10 mM ammonium acetate as a mobile phase. The determination coefficients of C and mC were high (R2 > 0.999) within the range tested. The %RSD for intraday and interday were respectively 2.2% and 2.5% for C and 3.5% and 3.8%
for mC. The limit of detection was 0.52 µM (0.52 fmol on-column) both for C and mC while the limit of quantification was 1.72 µM
(1.72 fmol on-column) both for C and mC. The smallest amount of purified DNA that yielded a measurable level of C and mC was
10 µg. On the whole, this method is simple, rapid, sensitive, and precise.
Content Type Journal Article
Category Short Communication
DOI 10.1007/s00216-010-3565-3
Authors
Salvatore Sotgia, University of Sassari Department of Biomedical Sciences and Centre of Excellence for Biotechnology Development and Biodiversity Research 07100 Sassari Italy
Angelo Zinellu, University of Sassari Department of Biomedical Sciences and Centre of Excellence for Biotechnology Development and Biodiversity Research 07100 Sassari Italy
Elisabetta Pisanu, University of Sassari Department of Biomedical Sciences and Centre of Excellence for Biotechnology Development and Biodiversity Research 07100 Sassari Italy
Luciano Murgia, University of Sassari Department of Biomedical Sciences and Centre of Excellence for Biotechnology Development and Biodiversity Research 07100 Sassari Italy
Gerard Aime Pinna, University of Sassari Department of Medicinal and Toxicological Chemistry 07100 Sassari Italy
Leonardo Gaspa, University of Sassari Department of Biomedical Sciences and Centre of Excellence for Biotechnology Development and Biodiversity Research 07100 Sassari Italy
Luca Deiana, University of Sassari Department of Biomedical Sciences and Centre of Excellence for Biotechnology Development and Biodiversity Research 07100 Sassari Italy
Ciriaco Carru, University of Sassari Department of Biomedical Sciences and Centre of Excellence for Biotechnology Development and Biodiversity Research 07100 Sassari Italy
A simple procedure has been developed and validated for the qualitative and quantitative analysis of several opiates (morphine,
6-acetylmorphine, codeine, 6-acetylcodeine) and tramadol in hair. The analytes were extracted from within the matrix via an
overnight incubation with methanol at 65 °C, and afterwards the samples were cleaned up by mixed-mode solid-phase extraction.
The extracts were derivatized with N-methyl-N-(trimethylsilyl) trifluoroacetamide with 5% trimethylchlorosilane and analyzed by gas chromatography–mass spectrometry in
the selected ion monitoring mode. The method was linear from 0.05 (lower limit of quantitation) to 50 ng/mg (40 ng/mg for
tramadol), with correlation coefficients higher than 0.99 for all compounds, accomplishing the cut-off values proposed by
the Society of Hair Testing for the detection of these substances in hair (0.2 ng/mg). Intra- and interday precision and trueness
were in conformity with the criteria normally accepted in bioanalytical method validation, and the sample cleanup step presented
a mean efficiency higher than 90% for all analytes. Furthermore, using these incubation conditions, 6-acetylmorphine did not
significantly hydrolyze to morphine. For these reasons, and because of its simplicity, the proposed method can be successfully
applied in the determination of these compounds in hair samples, and is suitable for application in routine analysis with
forensic purposes.
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3499-9
Authors
M. Barroso, Instituto Nacional de Medicina Legal—Delegação do Sul Rua Manuel Bento de Sousa, 3 1150-219 Lisboa Portugal
M. Dias, Instituto Nacional de Medicina Legal—Delegação do Sul Rua Manuel Bento de Sousa, 3 1150-219 Lisboa Portugal
D. N. Vieira, Instituto Nacional de Medicina Legal Largo da Sé Nova 3000-213 Coimbra Portugal
M. López-Rivadulla, Instituto Universitario de Medicina Legal San Francisco s/n 15782 Santiago de Compostela Spain
J. A. Queiroz, Universidade da Beira Interior—Centro de Investigação em Ciências da Saúde Av. Infante D. Henrique 6201-506 Covilhã Portugal
Daniel J. Weston
(Critical Review from Analyst)
Daniel J. Weston, Analyst, 2010, DOI: 10.1039/b925579f
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Demian R. Ifa, Chunping Wu, Zheng Ouyang, R. Graham Cooks
(Critical Review from Analyst)
Demian R. Ifa, Analyst, 2010, DOI: 10.1039/b925257f
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
Daniela Brondani, Iolanda Cruz Vieira, Clovis Piovezan, Jaqueline Maria Ramos da Silva, Ademir Neves, Jairton Dupont, Carla Weber Scheeren
(Paper from Analyst)
Daniela Brondani, Analyst, 2010, DOI: 10.1039/b925533h
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
A reverse-phase liquid chromatography method with diode array detection was developed to evaluate the quality of Ginkgo biloba extract through establishing chromatographic fingerprint and simultaneous determination of eight flavonoid compounds, namely
rutin, myricetin, quercitrin, quercetin, luteolin, kaempferol, apigenin, and isorhamnetin. The chromatographic separation
was performed on an Agilent SB-C18 column (250 × 4.6 mm, 5.0 µm) with a gradient elution program using a mixture of methanol
and 0.1% formic acid (v/v) as mobile phase within 55 min at 360-nm wavelength. The correlation coefficients of similarity for different batches of
G. biloba extract from the same manufacturer and G. biloba extract from different manufacturers were determined from the LC fingerprints, and they shared a close similarity. The eight
flavonoid compounds showed good regression (R2 > 0.9995) within test ranges, and the recovery of the method was in the range of 94.1–101.4%. In addition, the content of
those eight flavonoid compounds in G. biloba extract prepared by different manufacturers of China was determined to establish the effectiveness of the method. The results
indicated that the developed method by having a combination of chromatographic fingerprint and quantification analysis could
be readily utilized as a quality control method for G. biloba extract and its related traditional Chinese medicinal preparations.
Figure Fingerprint chromatograph of GBE from different manufactures.
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3536-8
Authors
Daoquan Tang, Xuzhou Medical College Department of Pharmaceutical Analysis Xuzhou Jiangsu 221004 China
Dongzhi Yang, Xuzhou Medical College Department of Pharmaceutical Analysis Xuzhou Jiangsu 221004 China
Anbang Tang, Xuzhou Medical College Student of school of pharmacy Xuzhou Jiangsu 221004 China
Yuanyuan Gao, Xuzhou Medical College Department of Pharmaceutical Analysis Xuzhou Jiangsu 221004 China
Xianglan Jiang, Xuzhou Medical College Department of Pharmaceutical Analysis Xuzhou Jiangsu 221004 China
Jie Mou, Xuzhou Medical College Department of Pharmaceutical Analysis Xuzhou Jiangsu 221004 China
Xiaoxing Yin, Xuzhou Medical College Department of Pharmaceutical Analysis Xuzhou Jiangsu 221004 China
In the present work, it is proposed, for the first time, an on-line automatic renewable molecularly imprinted solid-phase
extraction (MISPE) protocol for sample preparation prior to liquid chromatographic analysis. The automatic microscale procedure
was based on the bead injection (BI) concept under the lab-on-valve (LOV) format, using a multisyringe burette as propulsion
unit for handling solutions and suspensions. A high precision on handling the suspensions containing irregularly shaped molecularly
imprinted polymer (MIP) particles was attained, enabling the use of commercial MIP as renewable sorbent. The features of the
proposed BI-LOV manifold also allowed a strict control of the different steps within the extraction protocol, which are essential
for promoting selective interactions in the cavities of the MIP. By using this on-line method, it was possible to extract
and quantify riboflavin from different foodstuff samples in the range between 0.450 and 5.00 mg L−1 after processing 1,000 µL of sample (infant milk, pig liver extract, and energy drink) without any prior treatment. For milk
samples, LOD and LOQ values were 0.05 and 0.17 mg L−1, respectively. The method was successfully applied to the analysis of two certified reference materials (NIST 1846 and BCR
487) with high precision (RSD < 5.5%). Considering the downscale and simplification of the sample preparation protocol and
the simultaneous performance of extraction and chromatographic assays, a cost-effective and enhanced throughput (six determinations
per hour) methodology for determination of riboflavin in foodstuff samples is deployed here.
Figure Schematic representation of the manifold for determination of riboflavin in foodstuff. LOV lab-on-valve, MS multisyringe, HPLC high-performance liquid chromatography, Si syringe, Vi three-way commutation valve ( position off, solid line position on), A air, CS conditioning solvent (50% (v/v) MeOH/H2O), BS bead suspension in conditioning solvent, C carrier solution (H2O), D diluent (H2O), W waste, CC central channel, EL eluent (50% (v/v) MeOH/H2O+1% (v/v) CH3COOH), B channel for bead discarding, Sa sample/standard solution, HC holding coil, L1 connection tubing (8 cm), L2 connection tubing (44 cm), P chromatographic pump, IV injection valve, MC monolithic chromatographic column, λ diode array detector
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3522-1
Authors
Hugo M. Oliveira, Universidade do Porto REQUIMTE, Serviço de Química-Física, Faculdade de Farmácia Rua Aníbal Cunha, 164 4099-030 Porto Portugal
Marcela A. Segundo, Universidade do Porto REQUIMTE, Serviço de Química-Física, Faculdade de Farmácia Rua Aníbal Cunha, 164 4099-030 Porto Portugal
José L. F. C. Lima, Universidade do Porto REQUIMTE, Serviço de Química-Física, Faculdade de Farmácia Rua Aníbal Cunha, 164 4099-030 Porto Portugal
Manuel Miró, University of the Balearic Islands Department of Chemistry, Faculty of Sciences Carretera de Valldemossa km 7.5 07122 Palma Illes Balears Spain
Victor Cerdà, University of the Balearic Islands Department of Chemistry, Faculty of Sciences Carretera de Valldemossa km 7.5 07122 Palma Illes Balears Spain
A zirconia (ZrO2)-modified solid-phase extraction sorbent has been evaluated for selective extraction of phosphatidylcholines from biological
samples, followed by analysis of the isolated solutes by reversed-phase liquid chromatography–electrospray ionization–tandem
mass spectrometry. The clean-up process was optimized using seven standard phosphatidylcholines including two lyso derivatives.
Different acidic conditions were tested for the bonding and washing steps; for elution, various aqueous or methanolic bases
were studied. Experiments were conducted hydrodynamically using extraction cartridges, and statically in batch mode; the performance
of the sorbent was significantly better when used in the flow-through mode. The developed clean-up procedure was used to selectively
enrich phosphatidylcholines from whole milk, human plasma, and mouse plasma, to show the wide applicability of the method.
For the preceding extraction of total lipids from the matrix, different solvent mixtures (methanol–chloroform, methanol–methyl
tert-butyl ether, and ethanol–ethyl acetate) were compared. Accuracy and reproducibility of the proposed sample-preparation procedure
were evaluated. Matrix effects possibly affecting mass spectrometric analysis were studied before and after the solid-phase
extraction. They were found to be significant for several analytes, stressing the importance of a sample clean-up procedure.
Under identical experimental conditions, recovery of bound phosphatidylcholines by zirconia was superior to that by other
metal oxides, for example titania (TiO2) and stannia (SnO2).
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3527-9
Authors
Ana Gonzálvez, University of Vienna Department of Analytical Chemistry Waehringerstrasse 38 1090 Vienna Austria
Beatrix Preinerstorfer, University of Vienna Department of Analytical Chemistry Waehringerstrasse 38 1090 Vienna Austria
Wolfgang Lindner, University of Vienna Department of Analytical Chemistry Waehringerstrasse 38 1090 Vienna Austria
A partial least squares (PLS) regression model based on attenuated total reflectance–Fourier transform infrared spectra of
heated olive oil samples has been developed for the determination of polymerized triacylglycerides (PTGs) generated during
thermal treatment of oil. Three different approaches for selection of the spectral regions used to build the PLS model were
tested and compared: (1) variable selection based on expert knowledge, (2) uninformative variable elimination PLS, and (3)
interval PLS. Each of the three variable selection methods provided PLS models from heated olive oil samples with excellent
performance for the prediction of PTGs in fried olive oils with comparable model statistics. However, besides a high coefficient
of determination (R2 of 0.991) and low calibration, validation, and prediction errors of 1.14%, 1.21%, and 1.40% w/w, respectively, variable selection based on expert knowledge gave additionally almost identical low calibration (−0.0017%
w/w) and prediction (−0.0023% w/w) bias. Furthermore, it was verified that the determination of PTGs was not influenced by the type of foodstuff fried in the
olive oil.
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3546-6
Authors
Julia Kuligowski, Universidad de Valencia Department of Analytical Chemistry Edificio Jerónimo Muñoz, 50th Dr. Moliner 46100 Burjassot Spain
Guillermo Quintás, Universidad de Valencia Department of Analytical Chemistry Edificio Jerónimo Muñoz, 50th Dr. Moliner 46100 Burjassot Spain
Salvador Garrigues, Universidad de Valencia Department of Analytical Chemistry Edificio Jerónimo Muñoz, 50th Dr. Moliner 46100 Burjassot Spain
Miguel de la Guardia, Universidad de Valencia Department of Analytical Chemistry Edificio Jerónimo Muñoz, 50th Dr. Moliner 46100 Burjassot Spain
Penicillins are used universally in both human and veterinary medicine. The European Union (EU) has established maximum residue
levels (MRLs) for most ß-lactam antibiotics in milk and animal tissues and included them in the National Residue Monitoring
Programs. In this study, a novel method is described for the determination and confirmation of eight penicillins in porcine
tissues, milk and animal feed by liquid chromatography–tandem mass spectrometry (LC–MS/MS). To prevent degradation of penicillin
residues during workup, a derivatisation procedure was developed, by which penicillins were converted to stable piperidine
derivatives. Deuterated piperidine derivatives were synthesised for all relevant penicillins, enabling the use of isotope
dilution for accurate quantification. Penicillin residues were derivatised in the crude extract with piperidine and isolated
using solid-phase extraction. The penicillin piperidine derivatives were determined by LC–MS/MS. The method was validated
at the current MRLs, which range from 25–300 µg kg−1 in muscle and kidney to 4–30 µg kg−1 in milk as well as at the target value of 100 µg kg−1 chosen for animal feed, according to the EU requirements for a quantitative confirmatory method. Accuracy ranged from 94–113%
(muscle), 83–111% (kidney) and 87–103% (milk) to 88–116% (animal feed). Intra-day precision (relative standard deviation (RSD)r) ranged from 5–13% (muscle, n = 18), 4–17% (kidney, n = 7) and 5–18% (milk, n = 7) to 11–32% (animal feed, n = 18). Inter-day precision (RSDRL, n = 18) ranged from 6–23% (muscle) to 11–36% (animal feed). From the results, it was concluded that the method was fit for
purpose at the target MRLs in animal tissue and target levels for animal feed.
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3523-0
Authors
Frédérique van Holthoon, Wageningen UR RIKILT - Institute of Food Safety Akkermaalsbos 2 P.O. Box 230 6700 AE Wageningen The Netherlands
Patrick P. J. Mulder, Wageningen UR RIKILT - Institute of Food Safety Akkermaalsbos 2 P.O. Box 230 6700 AE Wageningen The Netherlands
Eric O. van Bennekom, Wageningen UR RIKILT - Institute of Food Safety Akkermaalsbos 2 P.O. Box 230 6700 AE Wageningen The Netherlands
Henri Heskamp, Wageningen UR RIKILT - Institute of Food Safety Akkermaalsbos 2 P.O. Box 230 6700 AE Wageningen The Netherlands
Tina Zuidema, Wageningen UR RIKILT - Institute of Food Safety Akkermaalsbos 2 P.O. Box 230 6700 AE Wageningen The Netherlands
Hans (J.) A. van Rhijn, Food and Consumer Product Safety Authority (VWA)—Lab Region East P.O. Box 19506 2500 CM Den Haag The Netherlands
Imma Ferrer, E. Michael Thurman (Eds.): Liquid chromatography time-of-flight mass spectrometry. Principles, tools, and applications for accurate mass analysis
Content Type Journal Article
Category Books and software in Review
DOI 10.1007/s00216-010-3525-y
Authors
Christian Neusüβ, Aalen University Chemistry Faculty Beethovenstr. 1 73430 Aalen Germany
Haiwei Gu, Shuiping Yang, Jianqiang Li, Bin Hu, Huanwen Chen, Lili Zhang, Qiang Fei
(Paper from Analyst)
Haiwei Gu, Analyst, 2010, DOI: 10.1039/b921579d
To cite this article before page numbers are assigned, use the DOI form of citation above.
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Xiao-tong Chen, Yu Xiang, Na Li, Pan-Shu Song, Ai-jun Tong
(Paper from Analyst)
Xiao-tong Chen, Analyst, 2010, DOI: 10.1039/b925508g
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Stephen L.R. Ellison, Vicki J. Barwick, Trevor J. Duguid Farrant: Practical statistics for the analytical scientist. A bench guide, 2nd ed.
Content Type Journal Article
Category Books and Software in Review
DOI 10.1007/s00216-010-3519-9
Authors
Jürgen W. Einax, Friedrich-Schiller-Universität Jena Institut für Anorganische und Analytische Chemie, Lehrbereich Umweltanalytik Lessingstr. 8 07743 Jena Germany
Illegal steroid administration to enhance growth performance in veal calves has long been, and still is, a serious issue facing
regulatory agencies. Over the last years, stating undisputable markers of illegal treatment has become complex because of
the endogenous origin of several anabolic steroids. Knowledge on the origin of an analyte is therefore of paramount importance.
The present study shows the presence of steroid analytes in wooden crates used for housing veal calves. For this purpose,
an analytical procedure using accelerated solvent extraction (ASE®), solid-phase extraction (SPE) and ultra-high performance
liquid chromatography coupled to triple quadrupole mass spectrometry (U-HPLC-MS-MS) is developed for the characterisation
of androstadienedione (ADD), boldenone (bBol), androstenedione (AED), β-testosterone (bT), α-testosterone (aT), progesterone
(P) and 17α-hydroxy-progesterone (OH-P) in wood samples. In samples of wooden crates used for housing veal calves, ADD, AED,
aT and P could be identified. Using the standard addition approach concentrations of these analytes were determined ranging
from 20 ± 4 ppb to 32 ± 4 ppb for ADD, from 19 ± 5 ppb to 44 ± 17 ppb for AED, from 11 ± 6 ppb to 30 ± 2 ppb for aT and from
14 ± 1 ppb to 42 ± 27 ppb for P, depending on the sample type. As exposure of veal calves to steroid hormones in their housing
facilities might complicate decision-making on illegal hormone administration, inequitable slaughter of animals remains possible.
Therefore, complete prohibition of wooden calf accommodation should be considered.
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3462-9
Authors
K. Verheyden, Ghent University Faculty of Veterinary Medicine, Research Group of Veterinary Public Health and Zoonoses, Laboratory of Chemical Analysis Salisburylaan 133 9820 Merelbeke Belgium
H. Noppe, Ghent University Faculty of Veterinary Medicine, Research Group of Veterinary Public Health and Zoonoses, Laboratory of Chemical Analysis Salisburylaan 133 9820 Merelbeke Belgium
J. Vanden Bussche, Ghent University Faculty of Veterinary Medicine, Research Group of Veterinary Public Health and Zoonoses, Laboratory of Chemical Analysis Salisburylaan 133 9820 Merelbeke Belgium
K. Wille, Ghent University Faculty of Veterinary Medicine, Research Group of Veterinary Public Health and Zoonoses, Laboratory of Chemical Analysis Salisburylaan 133 9820 Merelbeke Belgium
K. Bekaert, Ghent University Faculty of Veterinary Medicine, Research Group of Veterinary Public Health and Zoonoses, Laboratory of Chemical Analysis Salisburylaan 133 9820 Merelbeke Belgium
L. De Boever, Ghent University Faculty of Bioscience Engineering, Department of Forest and Water Management, Laboratory of Wood Technology Coupure Links 653 9000 Ghent Belgium
J. Van Acker, Ghent University Faculty of Bioscience Engineering, Department of Forest and Water Management, Laboratory of Wood Technology Coupure Links 653 9000 Ghent Belgium
C. R. Janssen, Ghent University Faculty of Bioscience Engineering, Department of Applied Ecology and Environmental Biology, Laboratory of Environmental Toxicology and Aquatic Ecology Jozef Plateaustraat 22 9000 Ghent Belgium
H. F. De Brabander, Ghent University Faculty of Veterinary Medicine, Research Group of Veterinary Public Health and Zoonoses, Laboratory of Chemical Analysis Salisburylaan 133 9820 Merelbeke Belgium
L. Vanhaecke, Ghent University Faculty of Veterinary Medicine, Research Group of Veterinary Public Health and Zoonoses, Laboratory of Chemical Analysis Salisburylaan 133 9820 Merelbeke Belgium
An electrochemical DNA biosensor based on the screen printed carbon paste electrode (SPCPE) with an immobilized layer of calf
thymus double-stranded DNA has been used for in vitro investigation of the interaction between genotoxic nitro derivatives
of fluorene (namely 2-nitrofluorene and 2,7-dinitrofluorene) and DNA. Two types of DNA damage have been detected at the DNA/SPCPE
biosensor: first, that caused by direct association of the nitrofluorenes, for which an intercalation association has been
found using the known DNA intercalators [Cu(phen)2]2+ and [Co(phen)3]3+ as competing agents, and, second, that caused by short-lived radicals generated by electrochemical reduction of the nitro
group (observable under specific conditions only).
Figure Anodic DPV response of DNA bases at the DNA/SPCPE (after baseline correction) recorded in AcB -methanol (99:1) medium; Eamp
50 mV, pulse width 100 ms, scan rate 20 mV s−1, Estep 5 mV, 36°C. DP voltammograms recorded at the DNA/SPCPE before (green
curve) and after successive CV cathodic/anodic cycling between 0 and −1000 mV (15 scans; scan rate 50 mV s−1) in solution
of 2-NF (c=1×10−5 mol L−1) in AcB -methanol (99:1) (red curve). Two different DNA/SPCPEs were used to record green and red
curve
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3517-y
Authors
Vlastimil Vyskočil, UNESCO Laboratory of Environmental Electrochemistry Charles University in Prague, Faculty of Science, Department of Analytical Chemistry Hlavova 2030/8 12843 Prague 2 Czech Republic
Ján Labuda, Slovak University of Technology in Bratislava, Faculty of Chemical and Food Technology, Institute of Analytical Chemistry Radlinského 9 81237 Bratislava Slovakia
Jiří Barek, UNESCO Laboratory of Environmental Electrochemistry Charles University in Prague, Faculty of Science, Department of Analytical Chemistry Hlavova 2030/8 12843 Prague 2 Czech Republic
Two independent liquid chromatography inductively coupled plasma-mass spectrometry (LC/ICP-MS) methods for the separation
of arsenic species in urine have been developed with quantification by standard additions. Seven arsenic species have been
quantified in a new NIST frozen human urine Standard Reference Material (SRM) 2669 Arsenic Species in Frozen Human Urine,
Levels 1 and 2. The species measured were: arsenite (As(III)), arsenate (As(V)), monomethylarsonate (MMA), dimethylarsinate
(DMA), arsenobetaine (AB), arsenocholine (AC), and trimethylarsine oxide (TMAO). The purity of each arsenic standard used
for quantification was measured as well as the arsenic species impurities determined in each standard. Analytical method limits
of detection (LD) for the various species in both methods ranged from 0.2 to 0.8 μg L−1 as arsenic. The results demonstrate that LC/ICP-MS is a sensitive, reproducible, and accurate technique for the determination
of low-level arsenic species in urine. Measurements of the arsenic species 3 years after initial production of the SRM demonstrate
the stability of the arsenic species in the urine reference material.
Figure SRM 2669 Arsenic Species in Frozen Human Urine
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3541-y
Authors
W. Clay Davis, Hollings Marine Laboratory National Institute of Standards and Technology (NIST), Analytical Chemistry Division 331 Fort Johnson Road Charleston SC 29412 USA
Rolf Zeisler, National Institute of Standards and Technology (NIST), Analytical Chemistry Division 100 Bureau Drive, Stop 8391 Gaithersburg MD 20899 USA
John R. Sieber, National Institute of Standards and Technology (NIST), Analytical Chemistry Division 100 Bureau Drive, Stop 8391 Gaithersburg MD 20899 USA
Lee L. Yu, National Institute of Standards and Technology (NIST), Analytical Chemistry Division 100 Bureau Drive, Stop 8391 Gaithersburg MD 20899 USA
A simple and easily automable method based on solid-phase microextraction followed by gas chromatographic–mass spectrometric
analysis was developed for the determination of two potential angiogenesis modulators 17β-estradiol (17-BE) and 2-methoxyestradiol
(2-MEOE) in culture media. Trifluoroacetic anhydride was used as the derivatising agent. A homemade octadecyl silica coating,
characterised by a coating thickness of 72 ± 10 μm and a good thermal stability until 250 °C, was prepared. Experimental design
was used to optimise the extraction conditions in terms of derivatisation time, derivatisation temperature and time of extraction.
As for method validation, lower limits of quantification of 0.17 and 0.015 µg/l for 17β-estradiol and 2-methoxyestradiol,
respectively, were obtained. Finally, the capabilities of the developed fibres were evaluated for the analysis of the investigated
analytes developed by granulosa cells in culture media maintained under normoxic, hypoxic and anoxic conditions, in order
to better elucidate their possible role in the angiogenic process. An increase of the production of both 17-BE and 2-MEOE
in hypoxic and anoxic conditions seems to be related to the effect of oxygen deprivation.
Figure 17-βestradiol and 2-methoxyestradiol as potential angiogenesis modulators
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3508-z
Authors
Federica Bianchi, Università degli Studi di Parma Dipartimento di Chimica Generale ed Inorganica, Chimica Analitica, Chimica Fisica Viale Usberti 17/A 43100 Parma Italy
Monica Mattarozzi, Università degli Studi di Parma Dipartimento di Chimica Generale ed Inorganica, Chimica Analitica, Chimica Fisica Viale Usberti 17/A 43100 Parma Italy
Maria Careri, Università degli Studi di Parma Dipartimento di Chimica Generale ed Inorganica, Chimica Analitica, Chimica Fisica Viale Usberti 17/A 43100 Parma Italy
Alessandro Mangia, Università degli Studi di Parma Dipartimento di Chimica Generale ed Inorganica, Chimica Analitica, Chimica Fisica Viale Usberti 17/A 43100 Parma Italy
Marilena Musci, Università degli Studi di Parma Dipartimento di Chimica Generale ed Inorganica, Chimica Analitica, Chimica Fisica Viale Usberti 17/A 43100 Parma Italy
Francesca Grasselli, Università degli Studi di Parma Dipartimento di Produzioni Animali, Biotecnologie Veterinarie, Qualità e Sicurezza degli Alimenti, Sezione di Fisiologia Veterinaria Via del Taglio 8 43100 Parma Italy
Simona Bussolati, Università degli Studi di Parma Dipartimento di Produzioni Animali, Biotecnologie Veterinarie, Qualità e Sicurezza degli Alimenti, Sezione di Fisiologia Veterinaria Via del Taglio 8 43100 Parma Italy
Giuseppina Basini, Università degli Studi di Parma Dipartimento di Produzioni Animali, Biotecnologie Veterinarie, Qualità e Sicurezza degli Alimenti, Sezione di Fisiologia Veterinaria Via del Taglio 8 43100 Parma Italy
Different compounds have been reported as biomarkers of a smoking habit, but, to date, there is no appropriate biomarker for
tobacco-related exposure because the proposed chemicals seem to be nonspecific or they are only appropriate for short-term
exposure. Moreover, conventional sampling methodologies require an invasive method because blood or urine samples are required.
The use of a microtrap system coupled to gas chromatography–mass spectrometry analysis has been found to be very effective
for the noninvasive analysis of volatile organic compounds in breath samples. The levels of benzene, 2,5-dimethylfuran, toluene,
o-xylene, and m- p-xylene have been analyzed in breath samples obtained from 204 volunteers (100 smokers, 104 nonsmokers; 147 females, 57 males;
ages 16 to 53 years). 2,5-Dimethylfuran was always below the limit of detection (0.005 ppbv) in the nonsmoker population and
always detected in smokers independently of the smoking habits. Benzene was only an effective biomarker for medium and heavy
smokers, and its level was affected by smoking habits. Regarding the levels of xylenes and toluene, they were only different
in heavy smokers and after short-term exposure. The results obtained suggest that 2,5-dimethylfuran is a specific breath biomarker
of smoking status independently of the smoking habits (e.g., short- and long-term exposure, light and heavy consumption),
and so this compound might be useful as a biomarker of smoking exposure.
Figure Extracted GC-MS chromatograms (m/z=78, 91, and 96) from a smoker and a healthy nonsmoker person.
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3524-z
Authors
Monica Alonso, University of Girona Department of Chemistry 17071 Gerona Spain
Mar Castellanos, Dr. Josep Trueta University Hospital Department of Neurology 17007 Gerona Spain
Juan M. Sanchez, University of Girona Department of Chemistry 17071 Gerona Spain
Abdelilah Beljebbar, Sylvain Dukic, Nadia Amharref, Michel Manfait
(Paper from Analyst)
Abdelilah Beljebbar, Analyst, 2010, DOI: 10.1039/b922184k
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Volatile organic compounds emitted from historical books made from cotton/linen rag and wood pulp paper have been studied.
Different profiles were obtained using different solid-phase microextraction (SPME) fibres to access the compounds involved
in the decomposition reactions occurring in cotton/linen rag and wood pulp paper upon natural ageing and precocious/accelerated
degradation. Contact headspace solid-phase extraction coupled with gas chromatography/time-of-flight mass spectrometry (GC-TOF-MS)
was improved as a non-destructive methodology for the analysis of historical books. Potential markers of cellulose degradation—linear
hydrocarbons, linear aldehydes, and 2-furfural—together with potential markers of cotton/linen rag paper (isopropylic esters)
were identified. Chiral analysis (SPME-c-GC-TOF-MS) showed that only the enantiomer (S)-2-ethyl-1-hexanol is present as an emanation compound in both types of paper. Validation studies for a larger number of
books are being done.
Figures 1–3 Portuguese old books made from cotton/linen rag paper.
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3520-3
Authors
Elvira M. Gaspar, Universidade Nova de Lisboa CQFB-Requimte, Departamento de Química, Faculdade de Ciências e Tecnologia, FCT 2829-516 Caparica Portugal
José C. Santana, Universidade Nova de Lisboa CQFB-Requimte, Departamento de Química, Faculdade de Ciências e Tecnologia, FCT 2829-516 Caparica Portugal
João F. Lopes, Universidade Nova de Lisboa CQFB-Requimte, Departamento de Química, Faculdade de Ciências e Tecnologia, FCT 2829-516 Caparica Portugal
Marcos B. Diniz, Universidade Nova de Lisboa CQFB-Requimte, Departamento de Química, Faculdade de Ciências e Tecnologia, FCT 2829-516 Caparica Portugal
Lithium salts are still one of the most popular therapeutic approaches to the treatment of bipolar disorders, notwithstanding
the introduction of more modern, less toxic drugs. Because of a narrow therapeutic range, lithium serum concentrations must
be strictly monitored during the treatment to avoid life-threatening neurotoxicity. For this purpose, methods based on flame
photometry or ion-selective electrodes are usually applied. The aim of the present work was to develop and validate a simple
method for the determination of lithium in serum based on capillary zone electrophoresis with indirect detection. A validation
of the method was carried out, including a comparison with an automated routine method based on ion-selective electrodes.
Content Type Journal Article
Category Technical Note
DOI 10.1007/s00216-010-3537-7
Authors
Jennifer P. Pascali, University of Verona Department of Medicine and Public Health, Unit of Forensic Medicine P.le L.A. Scuro 10 37134 Verona Italy
Daniela Sorio, University of Verona Department of Medicine and Public Health, Unit of Forensic Medicine P.le L.A. Scuro 10 37134 Verona Italy
Federica Bortolotti, University of Verona Department of Medicine and Public Health, Unit of Forensic Medicine P.le L.A. Scuro 10 37134 Verona Italy
Franco Tagliaro, University of Verona Department of Medicine and Public Health, Unit of Forensic Medicine P.le L.A. Scuro 10 37134 Verona Italy
Hua Wang, Wenjian Sun, Junsheng Zhang, Xiaohui Yang, Tao Lin, Li Ding
(Paper from Analyst)
Hua Wang, Analyst, 2010, DOI: 10.1039/b922616h
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Commercial poly(vinyl acetate) (PVAc) paint formulations for artists include a number of compounds in addition to the PVAc
polymer and pigments to improve the physical and chemical properties of the resulting product. Among the most common additives
are surfactants, coalescing agents, defoamers, freeze–thaw agents and thickeners. These products significantly influence the
behaviour of the dried film. Nevertheless, they are usually difficult to detect with conventional analytical methods given
their low concentration. In order to identify these additives, present in the dried film as minor components, an analytical
method based on in situ thermally assisted pyrolysis–silylation gas chromatography–mass spectrometry (GC-MS) using hexamethyldisilazane
as a derivatisation reagent is proposed. This method improves the conventional GC-MS analysis performed by direct pyrolysis
and enables the simultaneous identification of the PVAc binding medium and the additives included by the manufacturer in the
commercial paint. Five different commercial PVAc paints have been analysed, namely, armour green, burnt umber, oriental red,
raw umber and white from Flashe®. Internal plasticiser VeoVa consisting of C10 fatty acids with highly branched chains has been recognised from the MS spectra. On the other hand, the differences found
in the additive content of the studied paints, in particular the poly(ethylene glycol)-type surfactant, are in good agreement
with their mechanical properties.
Figure Picture of armour green Flashe® paint sample breaking in the mechanical tester’s gauge. The photo evidences the type of break
these samples experience. Rather than a clean break, the sample experiences several simultaneous fractures with a saw-tooth-like
pattern
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3505-2
Authors
Miguel F. Silva, Universidad Politécnica de Valencia Instituto de Restauración del Patrimonio Camino de Vera s/n 46022 Valencia Spain
Maria Teresa Doménech-Carbó, Universidad Politécnica de Valencia Instituto de Restauración del Patrimonio Camino de Vera s/n 46022 Valencia Spain
Laura Fuster-López, Universidad Politécnica de Valencia Instituto de Restauración del Patrimonio Camino de Vera s/n 46022 Valencia Spain
Marion F. Mecklenburg, Smithsonian Institution Museum Conservation Institute 4210 Silver Hill Road Suitland MD 20746-2863 USA
Susana Martin-Rey, Universidad Politécnica de Valencia Instituto de Restauración del Patrimonio Camino de Vera s/n 46022 Valencia Spain
A simple, low-cost process to integrate complementary metal oxide semiconductor array detectors (CMOSAD) for chemiluminescence
is presented, evaluated, and applied to the determination of nitrite in ground water samples. CMOS arrays of different brands
(obtained from commercial image sensors) were adapted as chemiluminescence detectors on microfluidic devices. The performance
of the CMOSADs was evaluated in the visible zone of the spectrum using a tungsten halogen lamp as light source. Intrinsic
parameters assessed included signal stability, spectral response, dark current, and signal-to-noise ratio. Thereafter, the
CMOSADs were integrated on microfluidic devices and their performances in quantitative analysis were assessed with the chemiluminometric
reaction of hydrogen peroxide with luminol, catalyzed with hexacyanoferrate (III). The parameters assessed were sensitivity,
linear range, detection limit, reproducibility, correlation coefficient of the calibration curves, and baseline drift during
measurements. The CMOSAD with the best performance was selected to assess the applicability of the developed microfluidic
devices with the integrated detector. The microfluidic system permitted the determination of nitrite with both good precision
and good recovery values in the analysis of ground water samples. Integration was easily achieved and enabled the development
of a simple, low-cost, and feasible alternative to conventional detectors.
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3518-x
Authors
Eunice R. G. O. Rodrigues, REQUIMTE, Serviço de Química-Física, Faculdade de Farmácia da Universidade do Porto Rua Aníbal Cunha 164 4099-030 Porto Portugal
Rui A. S. Lapa, REQUIMTE, Serviço de Química-Física, Faculdade de Farmácia da Universidade do Porto Rua Aníbal Cunha 164 4099-030 Porto Portugal
Five adrenolytic drugs have been analyzed by liquid chromatography–mass spectrometry (LC–MS). Samples were prepared by solid-phase
microextraction (SPME) using polypyrrole fibers coated on stainless steel support as an adsorbent for the drugs. Adsorption
efficiencies were 95% and were close for all the drugs investigated. Relative standard deviations (RSD), calculated for samples
prepared in standard solutions, were in the range 2.5–13%, however RSD values for the drugs in human plasma were 2.5–4.5%.
Using LC–MS the limit of detection (LOD) and the limit of quantification (LOQ) were in the ranges 0.11–0.18 and 0.39–0.54 ng mL−1, respectively, for the five drugs.
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3483-4
Authors
Boguslaw Buszewski, Nicolaus Copernicus University Department of Environmental Chemistry and Bioanalytics, Faculty of Chemistry Gagarin 7 87-100 Torun Poland
Pawel Olszowy, Nicolaus Copernicus University Department of Environmental Chemistry and Bioanalytics, Faculty of Chemistry Gagarin 7 87-100 Torun Poland
Tomasz Ligor, Nicolaus Copernicus University Department of Environmental Chemistry and Bioanalytics, Faculty of Chemistry Gagarin 7 87-100 Torun Poland
Malgorzata Szultka, Nicolaus Copernicus University Department of Environmental Chemistry and Bioanalytics, Faculty of Chemistry Gagarin 7 87-100 Torun Poland
Jacek Nowaczyk, Nicolaus Copernicus University Department of Physical Chemistry and Physicochemistry of Polymers, Faculty of Chemistry Gagarin 7 87-100 Torun Poland
Maciej Jaworski, Nicolaus Copernicus University Department of Surgery, Collegium Medicum St. Joseph Street 53-59 85-067 Bydgoszcz Poland
Marek Jackowski, Nicolaus Copernicus University Department of Surgery, Collegium Medicum St. Joseph Street 53-59 85-067 Bydgoszcz Poland
Juan Hu, Peng-Cheng Zheng, Jian-Hui Jiang, Guo-Li Shen, Ru-Qin Yu, Guo-Kun Liu
(Paper from Analyst)
Juan Hu, Analyst, 2010, DOI: 10.1039/b920358c
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Flow field-flow fractionation (FlFFF) was used for size characterization of gold nanoparticles. The measured particle sizes
obtained from FlFFF for the commercial 10 nm gold nanoparticle standard and the gold nanoparticles synthesized in the laboratory
were in good agreement with those measured by transmission electron microscopy (TEM). Further, the capability of α-tocopherol
to induce enlargement of gold nanoparticles by catalysis of the reduction of AuCl4− by citrate was observed by monitoring the changes in particle size of gold nanoparticles using FlFFF. The effects of α-tocopherol
and incubation time on enlargement of the gold nanoparticles were examined. Higher concentrations of α-tocopherol resulted
in larger nanoparticles. At fixed α-tocopherol concentration, larger nanoparticles were formed at longer incubation times.
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3511-4
Authors
Wimut Sermsri, Mahidol University Department of Chemistry and Center for Innovation in Chemistry, Faculty of Science Rama VI Road Bangkok 10400 Thailand
Purim Jarujamrus, Mahidol University Department of Chemistry and Center for Innovation in Chemistry, Faculty of Science Rama VI Road Bangkok 10400 Thailand
Juwadee Shiowatana, Mahidol University Department of Chemistry and Center for Innovation in Chemistry, Faculty of Science Rama VI Road Bangkok 10400 Thailand
Atitaya Siripinyanond, Mahidol University Department of Chemistry and Center for Innovation in Chemistry, Faculty of Science Rama VI Road Bangkok 10400 Thailand
A procedure for the determination of traces of mercury by liquid-phase microextraction based on solidification of a floating
organic droplet for separation and electrothermal atomic absorption spectrometry for final measurement has been developed.
For this purpose, 50 µL of pre-heated (50 °C) undecanoic acid (UA), are added to 25 mL of aqueous sample solution at pH 5.
The mixture, maintained at 50 °C, is stirred for 10 min using a high stirring rate in order to fragment the UA drop into droplets,
thus favoring the extraction process. Next, the vial is immersed in an ice bath, which results in the solidification of the
UA drop that is easily separated. Injection into the atomizer is carried out after gentle heating. The pyrolytic atomizers
are coated with electrolytically reduced palladium that acts as an effective chemical modifier for more than 500 firings.
Under the optimized conditions, the detection limit was 70 ng L−1 mercury with an enrichment factor of 430. The relative standard deviation of the measurements was in the 2.1–3.5% range.
Recovery studies applied to the determination of mercuric ions in bottled and tap water samples were in the 92–104% range.
Figure LPME-SFO allows liquid phase and the solidified organic reagent to be easily separated
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3500-7
Authors
I. López-García, Faculty of Chemistry, University of Murcia Department of Analytical Chemistry 30071 Murcia Spain
R. E. Rivas, Faculty of Chemistry, University of Murcia Department of Analytical Chemistry 30071 Murcia Spain
M. Hernández-Córdoba, Faculty of Chemistry, University of Murcia Department of Analytical Chemistry 30071 Murcia Spain
Ivory X. Peng, Rachel R. Ogorzalek Loo, Eli Margalith, Mark W. Little, Joseph A. Loo
(Paper from Analyst)
Ivory X. Peng, Analyst, 2010, DOI: 10.1039/b923303b
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
A rapid and simple method for separation and detection of six heterocyclic aromatic amines (2-amino-1-methyl-6-phenylimidazo
[4,5-b]-pyridine, 2-amino-1-methyl-imidazo [4,5-f]-quinoline, 2-amino-3,8-dimethyl-imidazo [4,5-f]-quinoxaline, 2-amino-3,7,8-trimethyl-imidazo [4,5-f]-quinoxaline, 2-amino-3,4,8-trimethyl-imidazo [4,5-f]-quinoxaline, and 2-amino-3,4-dimethyl-imidazo [4,5-f]-quinoline) in human urine samples is proposed to reflect daily intake and recent HAAs exposure. This method comprises previous
clean-up and preconcentration of the analytes on Strata-X reversed phase extraction cartridges followed by capillary liquid
chromatography (CLC) and evaporative light-scattering detection (ELSD). A mobile phase of acetonitrile and ammonium acetate
35 mM at pH 5.15 through a gradient of composition and a flow rate of 15 μL min−1 resulted in good separations of the analytes. Temperature and gas pressure were optimized for detection. The CLC-ELSD allows
the separation and quantification of HAAs with good resolution, precision, and sensitivity. The usefulness of the proposed
method was demonstrated by the analysis of synthetic and natural human urine samples spiked with different concentration levels
of heterocyclic amines.
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-009-3370-z
Authors
Fernando De Andrés, University of Castilla-La Mancha Department of Analytical Chemistry and Food Technology, Faculty of Chemistry Av. Camilo José Cela, 10 13004 Ciudad Real Spain
Mohammed Zougagh, University of Castilla-La Mancha Department of Analytical Chemistry and Food Technology, Faculty of Chemistry Av. Camilo José Cela, 10 13004 Ciudad Real Spain
Gregorio Castañeda, University of Castilla-La Mancha Department of Analytical Chemistry and Food Technology, Faculty of Chemistry Av. Camilo José Cela, 10 13004 Ciudad Real Spain
Angel Ríos, University of Castilla-La Mancha Department of Analytical Chemistry and Food Technology, Faculty of Chemistry Av. Camilo José Cela, 10 13004 Ciudad Real Spain
A survey of gilts applied to stucco surfaces that specifically focuses on the compositions of their colored grounds is reported.
Gilt samples of a common geographical (Lombardy in Italy) and temporal provenance (17th–18th century) were studied in the
form of polished cross-sections by optical and electron microscopy (SEM-EDS), micro-Raman (μRaman) spectroscopy and Fourier-transform
infrared microspectroscopy (μFTIR). Comparing samples with superimposed grounds and gilts enabled light to be shed on the
choice of specific materials, their stratigraphic functions, decorative effects, and technological performances. Iron oxide
pigments were found in the older grounds, sometimes in the presence of lead white (2PbCO3·Pb(OH)2) or minium (Pb3O4). In more recent grounds, chrome yellow (PbCrO4), chrome orange (PbCrO4·PbO), cinnabar (α-HgS) and barium white (BaSO4), invariably mixed with lead white, were encountered. Evidence for the use of organic mordants (colophony and wax, or siccative
oil) was obtained by μFTIR. This combined μFTIR and μRaman spectroscopic and elemental (SEM-EDS) analytical approach enhances
knowledge of the composition of gold grounds, their variability and their chronological evolution.
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3491-4
Authors
A. Sansonetti, Istituto per la Conservazione e Valorizzazione dei Beni Culturali CNR via Cozzi 53 20125 Milan Italy
J. Striova, Istituto per la Conservazione e Valorizzazione dei Beni Culturali CNR via Cozzi 53 20125 Milan Italy
D. Biondelli, Istituto per la Conservazione e Valorizzazione dei Beni Culturali CNR via Cozzi 53 20125 Milan Italy
E. M. Castellucci, University of Florence LENS and Chemistry Department via Lastruccia 3 50019 Sesto Fiorentino Italy
Secondary ion mass spectrometry (SIMS) depth profiling has been applied to the study of the thermal annealing of ohmic contacts
for high electron mobility transistors. The metallic stacks (Ti/Al/Ni/Au) were deposited over the Al0.28Ga0.72N/GaN/sapphire heterostructures and subjected to a rapid thermal annealing (850 °C for 30 s under N2 atmosphere) to improve the contact performance. The surface morphology and the in-depth chemical distribution of the layered
contacts were severely modified due to the treatment. These modifications have been analyzed by SIMS depth profiling and scanning
electron microscopy–energy-dispersive X-ray microanalysis. The SIMS analysis conditions have been optimized to achieve simultaneously
good sensitivity and to avoid ion-induced mixing effects produced by the primary beam sputtering.
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3482-5
Authors
H. Téllez, University of Málaga Department of Analytical Chemistry 29071 Málaga Spain
J. M. Vadillo, University of Málaga Department of Analytical Chemistry 29071 Málaga Spain
J. J. Laserna, University of Málaga Department of Analytical Chemistry 29071 Málaga Spain
Quantum dots (QDs), also named semiconductor nanocrystals, have initiated a new realm of bioscience by combining nanomaterials
with biology, which will profoundly influence future biological and biomedical research. In this review, we describe the extraordinary
optical properties of QDs and developments in methods for their synthesis. We focus on fluorescent imaging with QDs both in
vitro and in vivo, and the cytotoxicity of QDs and potential barriers to their use in practical biomedical applications. Finally,
we provide insights into improvements aimed at decreasing the cytotoxicity of QDs and the future outlook of QD applications
in biomedical fields.
Figure The unique tunable optical and chemical properties of QDs have been exploited in a growing array of biomedical applications
including clinical diagnostics and molecular, cellular, and tumor imaging
Content Type Journal Article
Category Review
DOI 10.1007/s00216-010-3481-6
Authors
Chao Wang, Jilin University Department of Analytical Chemistry, College of Chemistry Changchun 130012 China
Xue Gao, Jilin University Department of Analytical Chemistry, College of Chemistry Changchun 130012 China
Xingguang Su, Jilin University Department of Analytical Chemistry, College of Chemistry Changchun 130012 China
The absorbance at 260 nm (A260) is ubiquitously used for nucleic acid quantification. We show that following oxygenation, DNA solutions experience alterations
in both spectral properties (hyperchromism in the UV region, λmax 260 nm) and DNA conformation. The spectral changes caused by oxygen–DNA complexation are stable for at least several weeks
at room temperature or several hours at 37 °C, but are also reversible by purging with nitrogen. Our data indicate that DNA
in working solutions might already exist in the oxygen-complexed state, potentially confounding spectrophotometric analyses.
Further, the presence of these complexes does not appear to impart cell toxicity in vitro or affect the biophysical functional
behaviour (e.g. hybridisation) of DNA. Interestingly, our work also suggests that hybridisation could determine a release
of bound oxygen, a phenomenon that could open the way to the use of such systems as oxygen carriers.
Figure Oxygenation causes a marked hyperchromism in the main absorption bands of DNA (260 nm). The effect of this phenomenon on the
ubiquitous A260 readings can seriously affect the determination of DNA concentration
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3461-x
Authors
Rupak Doshi, The University of Manchester School of Translational Medicine, Manchester Interdisciplinary Biocentre Manchester M1 7ND UK
Philip J. R. Day, The University of Manchester School of Translational Medicine, Manchester Interdisciplinary Biocentre Manchester M1 7ND UK
Paolo Carampin, The University of Manchester Laboratory of Polymer and Biomaterials, School of Pharmacy & Pharmaceutical Sciences Manchester M13 9PL UK
Ewan Blanch, The University of Manchester Faculty of Life Sciences, Manchester Interdisciplinary Biocentre Manchester M1 7ND UK
Ian J. Stratford, The University of Manchester Experimental Oncology, School of Pharmacy & Pharmaceutical Sciences Manchester M13 9PL UK
Nicola Tirelli, The University of Manchester Laboratory of Polymer and Biomaterials, School of Pharmacy & Pharmaceutical Sciences Manchester M13 9PL UK
The cellular behavior of ginsenosides on cancer cells has not been measured directly despite their potent anticancer activities
and biological actions. A liquid chromatography–mass spectrometry (LC-MS) method was developed to measure the selective cellular
uptake of ginsenosides in both cell lysates and culture media. Fifteen ginsenosides were separated within 17 min with good
peak shapes using a 2-μm sub-particle size C18 column. Quantification was performed by triple-quadrupole MS with electrospray
ionization in negative ion mode. The sample preparation containing the solid-phase extraction was linear (correlation coefficient,
r2 > 0.992) for all analytes, while the limit of quantification ranged from 0.5 to 2.0 ng/mL in both matrices. The assay precision
(%CV) and accuracy (%bias) at three different concentrations (5, 20, and 100 ng/mL) were 1.4% to 11.6% and 94.9% to 106.4%,
respectively. When this method was used to examine the selective cellular uptake of ginsenosides, the relative non-polar and
protopanaxadiol class ginsenosides, such as Rg3, Rk1, Rg5, Rh2, compound-K, and protopanaxadiol (PPD), showed cellular uptake
in the MCF-7 cells, but the relative polar and protopanaxatriol class of ginsenosides did not accumulate in the cells. The
most non-polar ginsenoside PPD, which is an aglycone of the protopanaxadiol type, resulted in the highest uptake rate. These
results show that the different anticancer activities are due to the selective uptake of ginsenosides based on their chemical
structures. This LC-MS-based method can be used to estimate the biological activity of ginsenosides on cells from their structural
diversity.
Figure The structure and the ratios of cellular uptake of ginsenosides evaluated by liquid chromatography–mass spectrometry
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3515-0
Authors
Young Wan Ha, Korea Institute of Science and Technology Life/Health Division 39-1 Hawolkok-dong Seoul 136-791 Korea
Kwang Seok Ahn, Kyung Hee University College of Oriental Medicine Seoul 130-701 Korea
Jang-Choon Lee, Kyung Hee University College of Oriental Medicine Seoul 130-701 Korea
Sung-Hoon Kim, Kyung Hee University College of Oriental Medicine Seoul 130-701 Korea
Bong Chul Chung, Korea Institute of Science and Technology Life/Health Division 39-1 Hawolkok-dong Seoul 136-791 Korea
Man Ho Choi, Korea Institute of Science and Technology Life/Health Division 39-1 Hawolkok-dong Seoul 136-791 Korea
We introduce a novel combination of magnetic particles with hydrazine chemistry, dubbed as hydrazine-functionalized magnetic
particles (HFMP) for isolation of glycopeptides. Four methods have been developed and compared for the production of HFMP
by hydrazine modification of the surface of the carboxyl and epoxy-silanized magnetic particles, respectively. The evaluation
of the capability and specificity of HFMP as well as the optimization of the coupling condition for capturing of glycoproteins
were systematically investigated. The results showed that HFMP prepared by adipic dihydrazide functionalization from carboxyl-silanized
magnetic particles (HFCA) displayed the maximum capture capacity and isolated efficiency for glycoprotein. When measured with
glycoproteins, the capacity of the HFCA (1 g) for coupling bovine fetuin was 130 ± 5.3 mg. The capability of this method was
also confirmed by successful isolation of all formerly glycosylated peptides from standard glycoproteins and identification
of their glycosylation sites, which demonstrated the feasibility of the HFCA as an alternative solid support for isolation
of glycoproteins/glycopeptides.
Figure Schematic diagram for the preparation of hydrazine-functionalized magnetic particles (HFMP) and isolation of N-linked glycopeptides
by HFMP from protein sample.
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3513-2
Authors
Shisheng Sun, Northwest University College of Life Sciences Xi’an Shaanxi 710069 China
Ganglong Yang, Northwest University College of Life Sciences Xi’an Shaanxi 710069 China
Ting Wang, Northwest University College of Life Sciences Xi’an Shaanxi 710069 China
Qinzhe Wang, Northwest University College of Life Sciences Xi’an Shaanxi 710069 China
Chao Chen, National Engineering Research Center for Miniaturized Detection System Xi’an Shaanxi 710069 China
Zheng Li, Northwest University College of Life Sciences Xi’an Shaanxi 710069 China
A novel derivatizing agent, 5-chloro-2,2,3,3,4,4,5,5-octafluoropentyl chloroformate (ClOFPCF), was synthesized and tested
as a reagent for direct water derivatization of highly polar and hydrophilic analytes. Its analytical performance satisfactorily
compared to a perfluorinated chloroformate previously described, namely 2,2,3,3,4,4,5,5-octafluoropentyl chloroformate (OFPCF).
The chemical properties (reactivity, selectivity, derivatization products, and their chromatographic and spectral features)
for ClOFPCF were investigated using a set of 39 highly polar standard analytes, including, among others, hydroxylamine, malic
and succinic acids, resorcinol, hydroxybenzaldehyde, and dihydroxybenzoic acid. Upon derivatization, the analytes were extracted
from the aqueous solvent and analyzed by gas chromatography (GC)-mass spectrometry (MS) in the electron-capture negative ionization
(ECNI) mode. Positive chemical ionization (PCI)-MS was used for confirming the molecular ions, which were virtually absent
in the ECNI mass spectra. ClOFPCF showed good reaction efficiency, good chromatographic and spectroscopic properties (better
than with OFPCF), good linearity in calibration curves, and low detection limits (0.3–1 µg/L). A unique feature of the derivatizations
with ClOFPCF, and, in general, highly fluorinated chloroformates, is their effectiveness in reacting with carboxylic, hydroxylic,
and aminic groups at once, forming multiply-substituted non-polar derivatives that can be easily extracted from the aqueous
phase and determined by GC-ECNI-MS. The entire procedure from raw aqueous sample to ready-to-inject hexane solution of the
derivatives requires less than 10 min. Another benefit of this procedure is that it produced stable derivatives, with optimal
volatility for GC separation, and high electron affinity, which allows their detection as negative ions at trace level. In
addition, their mass spectra exhibits chlorine isotopic patterns that clearly indicate how many polar hydrogens of the analyte
undergo derivatization. Finally, derivatization with ClOFPCF was used successfully to identify 13 unknown highly polar disinfection
byproducts (DBPs) in ozonated fulvic and humic acid aqueous solutions and in real ozonated drinking water.
Figure The derivatization of hydroxylamine with 5-chloro-2,2,3,3,4,4,5,5-octafluoropentyl chloroformate yields optimal gas chromatographic
separation despite a 27-fold molecular weight increment.
Content Type Journal Article
Category Paper in Forefront
DOI 10.1007/s00216-010-3477-2
Authors
Marco Vincenti, Università degli Studi di Torino Dipartimento di Chimica Analitica Via Pietro Giuria 5 10125 Torino Italy
Francesca Fasano, Università degli Studi di Torino Dipartimento di Chimica Analitica Via Pietro Giuria 5 10125 Torino Italy
Maria Carmen Valsania, Università degli Studi di Torino Dipartimento di Traumatologia, Ortopedia e Medicina del Lavoro Via Zuretti 29 10126 Torino Italy
Rongrong Liu, Weiling Teo, Siyu Tan, Huajun Feng, Parasuraman Padmanabhan, Bengang Xing
(Paper from Analyst)
Rongrong Liu, Analyst, 2010, DOI: 10.1039/b926909f
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The content of this RSS Feed (c) The Royal Society of Chemistry
Georgianna L. Martin, Carolin Lau, Shelley D. Minteer, Michael J. Cooney
(Paper from Analyst)
Georgianna L. Martin, Analyst, 2010, DOI: 10.1039/b921409g
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The content of this RSS Feed (c) The Royal Society of Chemistry
Zhi-Min Zhang, Shan Chen, Yi-Zeng Liang
(Paper from Analyst)
Zhi-Min Zhang, Analyst, 2010, DOI: 10.1039/b922045c
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The content of this RSS Feed (c) The Royal Society of Chemistry
Jacob T. Shelley, Gary M. Hieftje
(Paper from Analyst)
Jacob T. Shelley, Analyst, 2010, DOI: 10.1039/b927389a
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The content of this RSS Feed (c) The Royal Society of Chemistry
A novel method for rapid HPLC-ICP-MS analysis of oxaliplatin in human urine was developed implementing a stationary HPLC phase
with a particle size of 1.8 µm. The method allowed a cycle time of <1 min at a HPLC flow rate of 0.9 mL min−1. Procedural limits of detection of 0.05 µg L−1 oxaliplatin (150 fg on column) were obtained. Analysis of oxaliplatin in patient urine showed that accurate quantification
of the intact drug demanded for storage at −80 °C and rapid measurement after thawing.
Content Type Journal Article
Category Technical Note
DOI 10.1007/s00216-010-3504-3
Authors
Gunda Koellensperger, University of Natural Resources and Applied Life Sciences, BOKU, Vienna Department of Chemistry, Division of Analytical Chemistry Muthgasse 18 1190 Vienna Austria
Stephan Hann, University of Natural Resources and Applied Life Sciences, BOKU, Vienna Department of Chemistry, Division of Analytical Chemistry Muthgasse 18 1190 Vienna Austria
Maria Gabrielle Eleonore Gerarda Bremer, Nathalie Gabrielle Esther Smits, Willem Haasnoot, Michel Wilhelmus Franciscus Nielen
(Paper from Analyst)
Maria Gabrielle Eleonore Gerarda Bremer, Analyst, 2010, DOI: 10.1039/b925372f
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The content of this RSS Feed (c) The Royal Society of Chemistry
This paper describes the application of TiO2 nano-particles (anatase form) for the solid-phase extraction of iron from coastal seawater samples. We investigated the adsorption
processes by infra-red spectroscopy. We compared in batch and on-(mini)column extraction approaches (0.1 and 0.05 g TiO2 per sample, respectively), combined to external calibration and detection by inductively coupled plasma mass spectrometry
at medium mass resolution. Globally, this titania phase was slightly more efficient with seawater than with ultra-pure water,
although between pH 2 and pH 7, the Fe retention efficiency progressed more in ultra-pure water than in seawater (6.9 versus
4.8 times improvement). Different reaction schemes are proposed between Fe(III) species and the two main categories of titania
sites at pH 2 (adsorption of [FeLx](3 − x)+ via possibly the mediation of chlorides) and at pH 7 (adsorption of [Fe(OH)2]+ and precipitation of [Fe(OH)3]0). Under optimised conditions, the inlet system was pre-cleaned by pumping 6% HCl for ∼2 h, and the column was conditioned
by aspirating ultra-pure water (1.7 g min−1) and 0.05% ammonia (0.6 g min−1) for 1 min. Then 3 g seawater sample was loaded at the same flow rate while being mixed on-line with 0.05% ammonia at 0.6 g
min−1 to adjust the pH to 7. The iron retained on the oxide powder was then eluted with 3 g 6% HCl (<0.002% residual salinity in
the separated samples). The overall procedural blank was 220 ± 46 (2 s, n = 16) ng Fe kg−1 (the titania was renewed in the column every 20 samples, with 2-min rinsing in between samples with 6% HCl at 1.5 g min−1). The recovery estimated from the Canadian certified reference material CASS-2 was 69.5 ± 7.6% (2 s, n = 4). Typically, the relative combined uncertainty (k = 2) estimated for the measurement of ∼1 µg Fe kg−1 (0.45 µm filtered and acidified to pH 1.5) of seawater was ∼12%. We applied our method to a similar sample, from the coastal
region of the North Sea. The agreement well within stated uncertainties of our result with the value obtained independently
by isotope dilution mass spectrometry further validated our method.
Content Type Journal Article
Category Technical Note
DOI 10.1007/s00216-009-3436-y
Authors
Christophe R. Quétel, Joint Research Centre—European Commission Institute for Reference Materials and Measurements 111 Retieseweg 2440 Geel Belgium
Emilia Vassileva, Joint Research Centre—European Commission Institute for Reference Materials and Measurements 111 Retieseweg 2440 Geel Belgium
Ivan Petrov, Joint Research Centre—European Commission Institute for Reference Materials and Measurements 111 Retieseweg 2440 Geel Belgium
Kristina Chakarova, Bulgarian Academy of Sciences Institute of General and Inorganic Chemistry 1113 Sofia Bulgaria
Konstantin I. Hadjiivanov, Bulgarian Academy of Sciences Institute of General and Inorganic Chemistry 1113 Sofia Bulgaria
Four compounds are docked to a pentameric bundle representing the transmembrane part of the Vpu protein from HIV-1. Employing
the docking algorithm FlexX, their free energy of binding is estimated leading to the conclusion that potential drug candidates
need to form H-bonds either with neighbouring or with n + 2 helices at the site of the serines within the bundle.
Content Type Journal Article
Category Short Communication
DOI 10.1007/s00216-010-3498-x
Authors
George Patargias, Oxford University Biomembrane Structure Unit, Department of Biochemistry South Parks Road Oxford OX1 3QU UK
Gary Ewart, Biotron Limited Suite 1.9, 56 Delhi Rd North Ryde NSW 2113 Australia
Carolyn Luscombe, Biotron Limited Suite 1.9, 56 Delhi Rd North Ryde NSW 2113 Australia
Wolfgang B. Fischer, Oxford University Biomembrane Structure Unit, Department of Biochemistry South Parks Road Oxford OX1 3QU UK
Junfang Wu, Yanpeng An, Jianwu Yao, Yulan Wang, Huiru Tang
(Paper from Analyst)
Junfang Wu, Analyst, 2010, DOI: 10.1039/b927543f
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The content of this RSS Feed (c) The Royal Society of Chemistry
Helena L. Woodvine, Jonathan G. Terry, Anthony J. Walton, Andrew R. Mount
(Paper from Analyst)
Helena L. Woodvine, Analyst, 2010, DOI: 10.1039/b924342a
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The content of this RSS Feed (c) The Royal Society of Chemistry
Qi-Zhen Chen, Yi-Min Fang, Hang Wei, Zong-Xiong Huang, Guo-Nan Chen, Jian-Jun Sun
(Paper from Analyst)
Qi-Zhen Chen, Analyst, 2010, DOI: 10.1039/b927327a
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The content of this RSS Feed (c) The Royal Society of Chemistry
Ying Zhang, Zachary S. Breitbach, Chunlei Wang, Daniel W. Armstrong
(Paper from Analyst)
Ying Zhang, Analyst, 2010, DOI: 10.1039/b925945g
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The content of this RSS Feed (c) The Royal Society of Chemistry
Abstract Recent developments in nanotechnology have led to the production of new materials with a wide array of applications, particularly
in catalysis. Because of their small size, nanoparticles have a maximized surface-to-volume ratio, thus making them attractive
targets for use as catalytic structures; however, the number of analytical techniques available to fully characterize materials
on such a size scale is quite limited. As a result, a complete understanding of the entire nanoparticle structure remains
unclear, especially when considering the active structural motif from which the specific activity arises. Metallic Pd materials
have been widely studied due to their immense potential as catalysts for reactions such as olefin hydrogenation and C–C bond
synthesis. These materials require surface passivants to act as ligands and stabilize the nanoparticles against aggregation
and bulk formation. These ligands have the added value to function as gates that selectively allow reagents to reach the active
surface of the Pd nanoparticles for chemical turnover. This accounts for the observed selectivities of the catalysts with
the corresponding changes in the turnover frequency values. Here we present a broad overview of recent advances in the use
of Pd nanoparticles for the industrially important hydrogenation reaction with a focus on characterizing and understanding
the base structural effects that give rise to the catalytic activity.
Figure The figure presents a reaction system to monitor the hydrogenation of olefin containing compounds. The flask on the right
is where the reaction is processed, while the volume of H2 used during the synthesis is measured from the burette in the middle
of the apparatus. The hydrogenation reaction equation is shown in blue.
Content Type Journal Article
Category Review
DOI 10.1007/s00216-010-3516-z
Authors
Marc R. Knecht, University of Kentucky Department of Chemistry 101 Chemistry-Physics Building Lexington KY 40506-0055 USA
Dennis B. Pacardo, University of Kentucky Department of Chemistry 101 Chemistry-Physics Building Lexington KY 40506-0055 USA
Abstract Developments of optical protein sensors with nanostructure based on the noble metals have currently received great attention
for their high efficiency and simultaneous analysis of various important biomolecules from proteomics to genetics. In this
study, we exploited the absorbance spectra of gold-capped nanoparticles substrate for label-free detections of antigen–antibody
reactions using a specific thiolated RNA aptamer. These synthesized RNA aptamers have been optimized to bind to the Fc portion
of the human IgG1 subclass, due to their ability to orient antibodies direction on the gold surface. After attaching the anti-fibrinogen
antibodies on the surface via these linkers, our thiolated RNA aptamer-based nanostructured sensors were easily applicable
to specific detections of fibrinogen with a limit of detection of 0.1 ng/mL. These nanostructured sensor-based models will
open a way to display numerous immunosensors as well as to develop other functionally similar sensors which could then be
expanded into multi-arrays assay systems.
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3488-z
Authors
Ha Minh Hiep, Osaka University Department of Applied Physics, Graduate School of Engineering Suita Osaka 565-0871 Japan
Masato Saito, Osaka University Department of Applied Physics, Graduate School of Engineering Suita Osaka 565-0871 Japan
Yoshikazu Nakamura, University of Tokyo Department of Basic Medical Sciences, Institute of Medical Science Minato-ku Tokyo 108-8639 Japan
Eiichi Tamiya, Osaka University Department of Applied Physics, Graduate School of Engineering Suita Osaka 565-0871 Japan
Abstract A new immunoassay has been developed based on a commercially available anti-caffeine monoclonal antibody and a de novo synthesized
tracer, using horseradish peroxidase and UV–visible detection. Caffeine, which is frequently found in surface waters, can
be quantified with a relative error lower than 20% for concentrations above 0.025 μg L−1 (limit of quantitation, direct analysis). The limit of detection is 0.001 μg L−1 and can be reduced by solid-phase extraction (SPE). Moreover, with minor adaptations, the assay can be used to quantify caffeine
in several beverages, shampoo, and caffeine tablets. The results obtained by ELISA correlate well with those from liquid chromatography–tandem
mass spectrometry (LC–MS–MS) for the tested matrices. Several surface waters from Berlin were analysed and all tested positive
for caffeine, with concentrations higher than 0.030 μg L−1. In one run 66 samples can be analysed within 2 h.
Figure A caffeine ELISA is described that allows sensitive and selective analysis of surface water concentrations as well as determination
of caffeine in beverages.
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3506-1
Authors
José João Carvalho, BAM Federal Institute for Materials Research and Testing Richard-Willstätter-Str. 11 12489 Berlin Germany
Michael G. Weller, BAM Federal Institute for Materials Research and Testing Richard-Willstätter-Str. 11 12489 Berlin Germany
Ulrich Panne, BAM Federal Institute for Materials Research and Testing Richard-Willstätter-Str. 11 12489 Berlin Germany
Rudolf J. Schneider, BAM Federal Institute for Materials Research and Testing Richard-Willstätter-Str. 11 12489 Berlin Germany
Abstract A unification of doping-control screening procedures of prohibited small molecule substances—including stimulants, narcotics,
steroids, β2-agonists and diuretics—is highly urgent in order to free resources for new classes such as banned proteins. Conceptually
this may be achieved by the use of a combination of one gas chromatography–time-of-flight mass spectrometry method and one
liquid chromatography–time-of-flight mass spectrometry method. In this work a quantitative screening method using high-resolution
liquid chromatography in combination with accurate-mass time-of-flight mass spectrometry was developed and validated for determination
of glucocorticosteroids, β2-agonists, thiazide diuretics, and narcotics and stimulants in urine. To enable the simultaneous
isolation of all the compounds of interest and the necessary purification of the resulting extracts, a generic extraction
and hydrolysis procedure was combined with a solid-phase extraction modified for these groups of compounds. All 56 compounds
are determined using positive electrospray ionisation with the exception of the thiazide diuretics for which the best sensitivity
was obtained by using negative electrospray ionisation. The results show that, with the exception of clenhexyl, procaterol,
and reproterol, all compounds can be detected below the respective minimum required performance level and the results for
linearity, repeatability, within-lab reproducibility, and accuracy show that the method can be used for quantitative screening.
If qualitative screening is sufficient the instrumental analysis may be limited to positive ionisation, because all analytes
including the thiazides can be detected at the respective minimum required levels in the positive mode. The results show that
the application of accurate-mass time-of-flight mass spectrometry in combination with generic extraction and purification
procedures is suitable for unification and expansion of the window of screening methods of doping laboratories. Moreover,
the full-scan accurate-mass data sets obtained still allow retrospective examination for emerging doping agents, without re-analyzing
the samples.
Content Type Journal Article
Category Original Paper
DOI 10.1007/s00216-010-3484-3
Authors
R. J. B. Peters, Wageningen UR RIKILT- Institute of Food Safety Akkermaalsbos 2 P.O. Box 230 6700 AE Wageningen The Netherlands
J. E. Oosterink, Wageningen UR RIKILT- Institute of Food Safety Akkermaalsbos 2 P.O. Box 230 6700 AE Wageningen The Netherlands
A. A. M. Stolker, Wageningen UR RIKILT- Institute of Food Safety Akkermaalsbos 2 P.O. Box 230 6700 AE Wageningen The Netherlands
C. Georgakopoulos, Olympic Athletic Center of Athens Doping Control Laboratory of Athens Kifissias 37 15123 Maroussi, Athens Greece
M. W. F. Nielen, Wageningen UR RIKILT- Institute of Food Safety Akkermaalsbos 2 P.O. Box 230 6700 AE Wageningen The Netherlands
Chaogui Chen, Jichao Zhang, Yan Du, Xiurong Yang, Erkang Wang
(Paper from Analyst)
Chaogui Chen, Analyst, 2010, DOI: 10.1039/b924545f
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Suncerae I. Smith, Jennifer S. Brodbelt
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Suncerae I. Smith, Analyst, 2010, DOI: 10.1039/b924023c
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Hong Chi, Bianhua Liu, Guijian Guan, Zhongping Zhang, Ming-Yong Han
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Hong Chi, Analyst, 2010, DOI: 10.1039/c000285b
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Wai Siang Law, Huan Wen Chen, Roman Balabin, Christian Berchtold, Lukas Meier, Renato Zenobi
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Wai Siang Law, Analyst, 2010, DOI: 10.1039/b924156f
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Cuisong Zhou, Zhen Liu, Jianyuan Dai, Dan Xiao
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Cuisong Zhou, Analyst, 2010, DOI: 10.1039/b923031a
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Gergely Lautner, Zsofia Balogh, Viola Bardoczy, Tamas Meszaros, Robert E. Gyurcsanyi
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Gergely Lautner, Analyst, 2010, DOI: 10.1039/b922829b
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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 82, Issue 5, Page 1571-1579, March 1, 2010.
Analytical Chemistry, Volume 0, Issue 0, Articles ASAP (As Soon As Publishable).
Analytical Chemistry, Volume 82, Issue 5, Page 1570, March 1, 2010.