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Analytical and Bioanalytical Chemistry (v.381, #1)

Master of your own career by John Fetzer (pp. 9-10).

Informatics and Mass Spectrometry Challenge by Juris Meija (pp. 11-12).
For the first time this year, we would like to invite you to participate in the Analytical Challenge, which is a series of puzzles to entertain and challenge our readers. We hope that you not only find this feature stimulating but that it provides you with points of further interest for your work and study. And please note: there is a prize to be won (a Springer book from our catalogue up to a value of € 75).These Analytical Challenges are published every two months. Two years ago, we first began with a series of spectroscopy challenges by Ernö Pretsch and Renato Zenobi, which may still be viewed on the ‘Springer’ chemistry website www.springeronline.com. Mass spectrometry is the topic in the present challenge. Please read on...
Asianalysis VII in Hong Kong by Wang Chan (pp. 14-15).
H. Lohninger: Teach/Me—Data Analysis by Stefan Busche (pp. 22-23).
ERM — A new landmark for reference materials by Hendrik Emons; John Marriott; Ralf Matschat (pp. 28-29).
Analytical chemistry in the European higher education area by Reiner Salzer; Terence Mitchell; Pascal Mimero; Miltiadis Karayannis; Constatinos Efstathiou; Anthony Smith; Miguel Valcárcel (pp. 33-40).
Optical microarray biosensors by Michael G. Weller (pp. 41-43).
Electrogenerated chemiluminescence on microfluidic chips by Jilin Yan; Xiurong Yang; Erkang Wang (pp. 48-50).
Sampling of material using femtosecond pulses by Ota Samek; Vanja Margetic; Roland Hergenröder (pp. 54-56).
Fully automated biosensors for water analysis by Guenther Proll; Jens Tschmelak; Guenter Gauglitz (pp. 61-63).
Quantitative proteomics by Michael W. Linscheid (pp. 64-66).
Reliable GMO analysis by Stefanie Trapmann; Hendrik Emons (pp. 72-74).
Sample preparation for pharmaceutical analysis by Xiaofang Fu; Yiping Liao; Huwei Liu (pp. 75-77).
Current and future screening systems by M. Valcárcel; S. Cárdenas (pp. 81-83).
The development of microarray standards by Morten T. Andersen; Carole A. Foy (pp. 87-89).
Micro-scale analytical plasmas for liquid chromatography detection by Jacob L. Venzie; R. Kenneth Marcus (pp. 96-98).
Reference materials: are they fit-for-purpose for food analysis? by Franz Ulberth; Hendrik Emons (pp. 99-101).
Challenges and needs in food measurements by Elke Anklam; Christoph von Holst (pp. 102-105).

Advances in analytical toxicology: the current role of liquid chromatography–mass spectrometry in drug quantification in blood and oral fluid by Hans H. Maurer (pp. 110-118).
This paper reviews procedures for quantification of drugs in the biosamples blood, plasma, serum, or oral fluid (saliva, etc.) using liquid chromatography coupled with single-stage or tandem mass spectrometry (LC–MS, LC–MS–MS). Such procedures are important prerequisites for competent toxicological judgment and consultation in clinical and forensic toxicology. They cover blood (plasma, serum) analysis of amphetamines and related designer drugs, anesthetics, anticonvulsants, benzodiazepines, opioids, serotonergic drugs, tricyclic antidepressants, neuroleptics, antihistamines, beta-blockers, muscle relaxants, and sulfonylurea-type antidiabetics, and oral fluid analysis of amphetamines and related designer drugs, cocaine, benzoylecgonine, codeine, morphine, enantiomers of methadone and its main metabolite 2-ethylidene-1,5-dimethyl-3,3-diphenylpyrrolidine (EDDP), the nicotine metabolites cotinine and hydroxycotinine, and finally risperidone and its metabolite 9-hydroxyrisperidone. Basic information on the procedures is given in two tables and an example of quantification is illustrated in two figures. The pros and cons of such LC–MS procedures including sample work-up and ion suppression effects are critically discussed.

Keywords: Drug; Blood; Oral fluid; Liquid chromatography–mass spectrometry


Miniaturization in sample treatment for environmental analysis by L. Ramos; J. J. Ramos; U. A. Th. Brinkman (pp. 119-140).
The increasing demand for faster, more cost-effective and environmentally friendly analytical methods is a major incentive to improve the classical procedures used for sample treatment in environmental analysis. In most classical procedures, the use of rapid and powerful instrumental techniques for the final separation and detection of the analytes contrasts with the time-consuming and usually manual methods used for sample preparation, which slows down the total analytical process. The efforts made in this field in the past ten years have led to the adaptation of existing methods and the development of new techniques to save time and chemicals, and improve overall performance. One route has been to develop at-line or on-line and, frequently, automated systems. In these approaches, miniaturization has been a key factor in designing integrated analytical systems to provide higher sample throughput and/or unattended operation. Selected examples of novel developments in the field of miniaturized sample preparation for environmental analysis are used to evaluate the merits of the various techniques on the basis of published data on real-life analyses of trace-level organic pollutants. Perspectives and trends are briefly discussed.

Keywords: Sample preparation; Miniaturization; Environmental analysis; Trace analysis; Micro-contaminants


Direct optical sensors: principles and selected applications by Guenter Gauglitz (pp. 141-155).
In the field of bio and chemosensors a large number of detection principles has been published within the last decade. These detection principles are based either on the observation of fluorescence-labelled systems or on direct optical detection in the heterogeneous phase. Direct optical detection can be measured by remission (absorption of reflected radiation, opt(r)odes), by measuring micro-refractivity, or measuring interference. In the last case either Mach–Zehnder interferometers or measurement of changes in the physical thickness of the layer (measuring micro-reflectivity) caused, e.g., by swelling effects in polymers (due to interaction with analytes) or in bioassays (due to affinity reactions) also play an important role. Here, an overview of methods of microrefractometric and microreflectometric principles is given and benefits and drawbacks of the various approaches are demonstrated using samples from the chemo and biosensor field. The quality of sensors does not just depend on transduction principles but on the total sensor system defined by this transduction, the sensitive layer, data acquisition electronics, and evaluation software. The intention of this article is, therefore, to demonstrate the essentials of the interaction of these parts within the system, and the focus is on optical sensing using planar transducers, because fibre optical sensors have been reviewed in this journal only recently. Lack of selectivity of chemosensors can be compensated either by the use of sensor arrays or by evaluating time-resolved measurements of analyte/sensitive layer interaction. In both cases chemometrics enables the quantification of analyte mixtures. These data-processing methods have also been successfully applied to antibody/antigen interactions even using cross-reactive antibodies. Because miniaturisation and parallelisation are essential approaches in recent years, some aspects and current trends, especially for bio-applications, will be discussed. Miniaturisation is especially well covered in the literature.

Keywords: Optical; Chemosensing; Biosensing; Transducer; Application


Detection of influenza virus: traditional approaches and development of biosensors by Yoshihisa Amano; Quan Cheng (pp. 156-164).
Influenza is an acute respiratory disease caused by the influenza virus. The disease occurs annually, causing fatality in the elderly and children and billions of dollars loss in business and productivity. Traditional viral detection methods include MDCK cell culture, complement fixation, hemagglutinin-inhibition, and recently RT-PCR. Although effective, these methods generally involve labor-intensive laboratory procedures and often require trained personnel to carry them out. The development of biosensor technologies will enable rapid and specific disease diagnosis on-site so that a clinician can quickly determine whether treatment is needed. This paper reviews traditional viral assays and progress in the biosensor development for influenza virus. Recent advances in single-step direct detection using non-labeling techniques such as surface plasmon resonance, quartz-crystal microbalance, and colorimetric functional polymers are discussed.

Keywords: Biosensor; Influenza virus; Surface plasmon resonance; Quartz-crystal microbalance; Colorimetric sensor


New dimension in nano-imaging: breaking through the diffraction limit with scanning near-field optical microscopy by Akiko Rasmussen; Volker Deckert (pp. 165-172).
In recent years scanning near-field optical microscopy (SNOM) has developed into a powerful surface analytical technique for observing specimens with lateral resolution equal to or even better than 100 nm. A large number of applications, from material science to biology, have been reported. In this paper, two different kinds of near-field optical microscopy, aperture and scattering-type SNOM, are reviewed together with recent studies in surface analysis and biology. Here, near-field optical techniques are discussed in comparison with related methods, such as scanning probe and standard optical microscopy, with respect to their specific advantages and fields of application.

Keywords: Scanning near-field optical microscopy (SNOM); Fluorescence; Raman; Atomic-force microscopy (AFM); Confocal imaging


Glow discharge mass spectrometry by Volker Hoffmann; Martin Kasik; Peter K. Robinson; Cornel Venzago (pp. 173-188).
Over the past twenty years or so, glow discharge mass spectrometry (GDMS) has become the industry standard for the analysis of trace elements in metals and semiconductors. A review of its history is followed by a picture of the present situation and a look to where the future may lie. Applications are summarised, including the ability of GDMS to offer depth-resolved data and non-conductor analysis, and the well-documented quantitative nature of the results is reviewed. The effects resulting from the physical properties of the analyte material are discussed at length. Finally, recent work such as “fast flow” sources and pulsed glow discharges is reviewed.

Keywords: Glow discharge mass spectrometry; Depth profile; Temperature; Fast flow; Pulse


Solid-phase extraction of room-temperature imidazolium ionic liquids from aqueous environmental samples by Piotr Stepnowski (pp. 189-193).
Owing to their favorable properties, ionic liquids have recently gained recognition as possibly environmentally benign solvents. Now among the most promising industrial chemicals, they have already been labeled “green”, but this appellation seems due entirely to their very low vapor pressure. This growing interest in the various applications of ionic liquids will soon result in their presence in the environment. Therefore, reliable analytical tools for the environmental analysis of ionic liquids need to be developed urgently. This paper presents a newly developed analytical procedure for the enrichment of 1-alkyl- and 1-aryl-3-methylimidazolium ionic liquids from water samples. The method is based on cation exchange solid-phase extraction followed by selective elution. Pre-concentrated samples are subjected to high-performance liquid chromatography (HPLC) with an advanced methodology for qualitative and quantitative analysis. The overall procedure was verified by using standard spiked samples of tap water, seawater, and freshwater.

Keywords: Ionic liquids; Analysis; SPE; Cation exchange; Environmental samples


Development and characterisation of a new interface for coupling capillary LC with collision-cell ICP–MS and its application for phosphorylation profiling of tryptic protein digests by Daniel Pröfrock; Peter Leonhard; Wolfgang Ruck; Andreas Prange (pp. 194-204).
A comparison of different nebulisers for direct hyphenation of capillary and nano liquid chromatography (Cap-LC, Nano-LC) and quadrupole-based collision cell inductively coupled plasma mass spectrometry (CC-ICP–MS) for phosphorylation profiling of tryptic protein digests is described. Helium was used as cell gas and specially tuned instrumental conditions were used to achieve background minimisation at the mass of phosphorus, because of kinetic energy discrimination of the interfering polyatomic ions. The proposed set-up is based on a modified capillary electrophoresis interface and a home-made 4 mL spray chamber. It enables the use of gradient conditions with a highly concentrated organic mobile phase as often used in protein phosphorylation analysis, without the need to apply membrane desolvation for removal of the organic phase or further background minimisation. No significant signal suppression or other negative effects caused by the organic mobile phase occur, because of the low flow rates used in Cap-LC and the robust plasma conditions of the CC-ICP–MS instrument. A tryptic digest of beta-casein was investigated as model compound to demonstrate the applicability of the proposed set-up for phosphorylation profiling in protein analysis using quadrupole based collision-cell ICP–MS as phosphorus-specific detector. Detection limits for phosphorylated peptides down to the sub picomole level were obtained. As a complementary technique, electrospray ionisation tandem mass spectrometry (ESI–MS–MS) with data base searching was used for further characterisation of the phosphorylated peptides detected.

Keywords: Capillary-LC; Protein; Phosphorylation; Post-translational modification; ICP–MS; Hyphenation; Collision cell; Reaction cell


Styrene oxide DNA adducts: quantitative determination using 31P monitoring by Michael Edler; Norbert Jakubowski; Michael Linscheid (pp. 205-211).
The reaction of styrene oxide, a potential carcinogen in humans, with DNA constituents has been used to develop an improved method for quantification of DNA adducts. To enable monitoring of DNA adducts caused by xenobiotics at physiological relevant levels, a robust, reliable and powerful method based on monitoring of phosphorus in nucleotides is described. An efficient enzymatic digestion step and a sample-preconcentration procedure are essential, and enable separation of alkylated nucleotides from the large excess of native nucleotides. The adducts are detected by means of the phosphorus signal measured at mass m/z=31 with an inductively-coupled-plasma mass spectrometer. Bis(4-nitrophenyl)phosphate (BNPP) serves as internal standard for quantification of the adducts. The absolute limit of detection, 45 fmol, corresponds to detection of three modified nucleotides among 107 native nucleotides (the calculation is based on use of 50 μg calf thymus DNA). An adduct formation ratio at the DNA of 3.6 adducts per 1000 nucleotides was measured, which is 75% lower than for reaction with monomeric 2′-deoxy-nucleotides. In addition, a substantial amount of phosphate adducts were detected, but in DNA the rate of phosphate formation was lower than with monomeric nucleotides. Most probably these adducts escaped unnoticed when 31P-post-labelling was employed.

Keywords: DNA adducts; Inductively-coupled-plasma mass spectrometry (ICP–MS)31P monitoring; Styrene oxide


Characterizing ablation and aerosol generation during elemental fractionation on absorption modified lithium tetraborate glasses using LA-ICP-MS by Peter Weis; Horst P. Beck; Detlef Günther (pp. 212-224).
The influence of sample matrix composition, absorption behavior and laser aerosol particle size distribution on elemental fractionation in laser ablation inductively coupled plasma mass spectrometry was studied for nanosecond laser ablation at a wavelength of 266 nm. To this end, lithium tetraborate glass samples with different iron oxide contents and trace amounts of a group of 11 elements were prepared synthetically. The samples were characterized in terms of optical absorbance, melting points, trace element concentrations and homogeneity. UV/VIS spectra showed that sample absorption rises with increasing Fe2O3 content. Crater depths and time-dependent particle size distributions were measured, and ablated and transported sample volumes were estimated. Furthermore, the laser aerosol was filtered using a particle separation device and transient ICP-MS signals were acquired with and without filtering the aerosol. The results demonstrate that the amount of ablated sample is related to the absorption coefficient of the sample and therefore to the optical penetration depth of the laser beam into the sample. The higher energy densities resulting from the shorter penetration depths result in smaller average particle sizes for highly absorbing samples, which allows more efficient transport to and atomization and excitation of the ablated material within the ICP. The particle size distribution changes continuously with ablation time, and larger particle fractions occur mainly at the beginning of the ablation, which leads to particle-related fractionation processes at the beginning of the transient signal. Exceeding a critical depth to diameter ratio, laser-related elemental fractionation processes occur. Changes in the volatile to non-volatile element intensity ratio after the aerosol is filtered indicate that particle size-related enrichment processes contribute to elemental fractionation.

Keywords: Laser ablation; ICP-MS; Elemental fractionation; Transient signals; Particle size distribution


Membrane protein and peptide sample handling for MS analysis using a structured MALDI target by Theres Redeby; Åsa Emmer (pp. 225-232).
Different sample handling methods for hydrophobic proteins and peptides were evaluated in association with the utilization of a structured matrix-assisted laser/desorption ionization (MALDI) target for increased sensitivity. The fluorinated organic solvent hexafluoroisopropanol (HFIP) was used for the solubilization of both the full-length protein bacteriorhodopsin (BR) and a cyanogen bromide digest thereof, and compared to the performance of the non-ionic detergents octyl-β-d-glucopyranoside (OG), dodecyl-β-d-maltoside (DM), and Triton X-100. A concentrating effect was seen when using the structured MALDI plate for BR dissolved in all the different detergents, of which OG generated the best-quality spectra for the full-length integral membrane protein as well as for the hydrophobic peptides. However, the uneven analyte distribution obtained with the detergent preparations required selective and thus time-consuming acquisition of spectra. When instead HFIP was used as sample solvent, a tenfold increase in sensitivity was achieved for full-length BR. Addition of acids to the HFIP-solubilized sample, or to the MALDI matrix solution, improved the signals for a few of the peptides, while degrading the spectra of others. Consequently, the addition of acid could be used as a complementary sample preparation method for hydrophobic peptides. On-target washing to remove contaminants (e.g., salt) was performed, and a recrystallization protocol for signal improvement specifically suited for hydrophobic peptides is described. Results from digestion and solubilization in different micro centrifuge tubes were examined to determine the influence of different materials on the possible sample loss due to wall adhesion. Studies of sample solution storage times suggest immediate analysis after solubilization to obtain best results.

Keywords: Structured sample support; MALDI-MS; Hydrophobic peptides; Integral membrane proteins; Sample handling


Generation of antiserum to Irgarol 1051 and development of a sensitive enzyme immunoassay using a new heterologous hapten derivative by Ramadan A. Abuknesha; Hannah M. T. Griffith (pp. 233-243).
A polyclonal antiserum to Irgarol 1051 was developed in sheep and used to construct an enzyme immunoassay method for the measurement of the antifouling compound in river and seawater samples. The antiserum was generated by a hapten derivative, 2-(tert-butylamino)-4-(cyclopropylamino)-6-(thiopropionic acid)-1,3,5-triazine, coupled to a mixture of keyhole limpet hemocyanin and bovine serum albumin, and the competitive enzyme immunoassay was constructed using a plate-coating antigen made of a heterologous new hapten derivative, 2-(tert-butylamino)-4-(cyclopropylamino)-6-(phenoxybenzoic acid)-1,3,5-triazine, linked to gelatine. The assay showed a sensitivity of about 5 ng L−1 in river and seawater matrices with reasonable specificity with respect to commonly used triazines such as atrazine (3%), simazine (>0.1%) and desethylatrazine (>0.01%). However, high cross-reactivity levels were found with ametryn (56%) and prometryn (60%). Tests on the effects of organic solvents on assay performance indicated a high tolerance to methanol but much less so to acetonitrile. The assay was found to be highly reproducible and robust owing to the stability of the sheep antibody and the highly optimised competitive assay reagents which included the use of the new triazine-O-phenoxybenzoic acid derivative.

Keywords: Irgarol 1051; Hapten; Homology; Heterology; Organic solvents


Comparison of the analysis of corticosteroids using different techniques by E. Pujos; M. M. Flament-Waton; O. Paisse; M. F. Grenier-Loustalot (pp. 244-254).
In this work we have optimized the analysis of 18 human corticosteroids, some endogenous (tetrahydrocortisol, tetrahydrocortisone, cortisol, and cortisone) and others synthetic (betamethasone, budesonide, cortisone acetate, desonide, dexamethasone, dexamethasone acetate, flunisolide, fluocinolone acetonide, halcinonide, methylprednisolone, prednisolone, prednisone, triamcinolone, and triamcinolone acetonide). Three analytical techniques were developed: ELISA, gas chromatography coupled with mass spectrometry (GC–MS), and liquid chromatography coupled with mass spectrometry (LC–MS). Several sample-preparation methods were optimized for each technique and enabled compounds of interest to be extracted from small urine samples (several mL). The results enabled us to assess the possibilities and the sensitivity of each technique for application to doping tests.

Keywords: Steroids; Metabolites; Urine; Extraction; GC-MS


A simple and fast micromethod for the analysis of polychlorinated biphenyls in air by sorbent enrichment and ultrasound-assisted solvent extraction by Ruth Barro; Sergio Ares; Carmen Garcia-Jares; Maria Llompart; Rafael Cela (pp. 255-260).
A combination of sorbent enrichment and ultrasound-assisted solvent extraction has been used to determine polychlorinated biphenyls in air. Analytes were sampled by pumping a known volume of air through a porous polymer (Tenax TA). The enriched adsorbent was transferred into a glass vial, and ultrasound-assisted extraction of the analytes was then performed in n-hexane. Quantification was carried out by using gas chromatography coupled to tandem mass spectrometry. Breakthrough volume of the sampling step was studied, indicating that 10 m3 of air could be processed without losses of the most volatile compounds. Good recoveries (75–96%) were obtained, and limits of detection at the sub ng m−3 were achieved for all the analytes. The proposed method is very simple and fast, avoiding the use of large solvent volumes and time-consuming preconcentration steps.

Keywords: Air analysis; Polychlorinated biphenyls; Gas chromatography–mass spectrometry; Ultrasound-assisted extraction


Characterization and discrimination of pollen by Raman microscopy by N. P. Ivleva; R. Niessner; U. Panne (pp. 261-267).
The chemical characterization and discrimination of allergy-relevant pollen (common ragweed (Ambrosia artemisiifolia), white birch (Betula pendula), English oak (Quercus robur), and European linden (Tilia cordata)) has been studied by Raman microscopy. Spectra were obtained at different excitation wavelengths (514, 633, and 780 nm) and various methods were examined to minimize the strong fluorescence background. The use of a He–Ne laser (633 nm) for excitation yields high-quality single pollen Raman spectra, which contain multiple bands due to pollen components such as carotenoids, proteins, nucleic acids, carbohydrates, and lipids. Multivariate classification, i.e. principal component analysis (PCA) and hierarchical cluster analysis, demonstrated the validity of the approach for discrimination between different pollen species.

Keywords: Raman spectroscopy; Pollen; Multivariate classification


LC-MS/MS method for the confirmatory determination of aromatic amines and its application in textile analysis by P. Sutthivaiyakit; S. Achatz; J. Lintelmann; T. Aungpradit; R. Chanwirat; S. Chumanee; A. Kettrup (pp. 268-276).
A confirmation method for the determination of 18 aromatic amines originating from azo dyes after reductive cleavage was developed. The method is based on the use of high-performance liquid chromatography/tandem mass spectrometry with atmospheric-pressure chemical ionization. For the identification of the analytes one precursor ion and two daughter ions (multi-reaction monitoring, MRM) were selected and the LC-MS/MS parameters optimized to obtain high sensitivity and selectivity. The linear ranges varied from 0.1–1 to 30–50 μg mL−1 with correlation coefficients of 0.99 or better. The applicability of the method to determine o-tolidine (3,3′-dimethylbenzidine) and 3,3′-dimethoxybenzidine in textiles following reductive cleavage of acid red 114, trypan blue, and Chicago sky blue 6B was demonstrated.

Keywords: Atmospheric-pressure chemical ionization (APCI); High-performance liquid chromatography (HPLC); Tandem mass spectrometry (MS/MS); Aromatic amines; Azo dye; Textile analysis
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