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Showing papers in "Analyst in 2008"


Journal ArticleDOI
01 Jan 2008-Analyst
TL;DR: This review uses evidence from the literature to consider the usefulness and limitations of sequential extraction, and discusses typical applications from the recent literature for which sequential extraction can provide useful and meaningful information.
Abstract: Since their introduction in the late 1970s, sequential extraction procedures have experienced a rapid increase in use. They are now applied for a large number of potentially toxic elements in a wide range of sample types. This review uses evidence from the literature to consider the usefulness and limitations of sequential extraction and thereby to assess its future role in environmental chemical analysis. It is not the intention to provide a comprehensive survey of all applications of sequential extractions or to consider the merits and disadvantages of individual schemes. These aspects have been covered adequately in other, recent reviews. This review focuses in particular on various key issues surrounding sequential extractions such as nomenclature, methodologies, presentation of data and interpretation of data, and discusses typical applications from the recent literature for which sequential extraction can provide useful and meaningful information. Also covered are emerging developments such as accelerated procedures using ultrasound- or microwave energy-assisted extractions, dynamic extractions, the use of chemometrics, the combination of sequential extraction with isotope analysis, and the extension of the approach to non-traditional analytes such as arsenic, mercury, selenium and radionuclides.

554 citations


Journal ArticleDOI
09 Sep 2008-Analyst
TL;DR: An intuitive description of the complex physics of plasmons and near-field interactions is provided and how these effects will result in new classes of experimental procedures, novel probes, bioassays and devices are suggested.
Abstract: Fluorescence spectroscopy is widely used in biological research. Until recently, essentially all fluorescence experiments were performed using optical energy which has radiated to the far-field. By far-field we mean at least several wavelengths from the fluorophore, but propagating far-field radiation is usually detected at larger macroscopic distances from the sample. In recent years there has been a growing interest in the interactions of fluorophores with metallic surfaces or particles. Near-field interactions are those occurring within a wavelength distance of an excited fluorophore. The spectral properties of fluorophores can be dramatically altered by near-field interactions with the electron clouds present in metals. These interactions modify the emission in ways not seen in classical fluorescence experiments. In this review we provide an intuitive description of the complex physics of plasmons and near-field interactions. Additionally, we summarize the recent work on metal-fluorophore interactions and suggest how these effects will result in new classes of experimental procedures, novel probes, bioassays and devices.

541 citations


Journal ArticleDOI
01 Jan 2008-Analyst
TL;DR: The CuO nanowire modified electrode allows highly sensitive, low working potential, stable, and fast amperometric sensing of glucose, thus is promising for the future development of non-enzymatic glucose sensors.
Abstract: CuO nanowires have been prepared and applied for the fabrication of glucose sensors with highly enhanced sensitivity. Cu(OH)(2) nanowires were initially synthesised by a simple and fast procedure, CuO nanowires were then formed simply by removing the water through heat treatment. The structures and morphologies of Cu(OH)(2) and CuO nanowires were characterised by X-ray diffraction, X-ray photoelectron spectroscopy, scanning electron microscopy, and transmission electron microscopy. The direct electrocatalytic oxidation of glucose in alkaline medium at CuO nanowire modified electrodes has been investigated in detail. Compared to a bare Cu electrode, a substantial decrease in the overvoltage of the glucose oxidation was observed at the CuO nanowire electrodes with oxidation starting at ca. 0.10 V vs. Ag/AgCl (saturated KCl). At an applied potential of 0.33 V, CuO nanowire electrodes produce high and reproducible sensitivity to glucose with 0.49 microA/micromol dm(-3). Linear responses were obtained over a concentration range from 0.40 micromol dm(-3) to 2.0 mmol dm(-3) with a detection limit of 49 nmol dm(-3) (S/N = 3). The CuO nanowire modified electrode allows highly sensitive, low working potential, stable, and fast amperometric sensing of glucose, thus is promising for the future development of non-enzymatic glucose sensors.

445 citations


Journal ArticleDOI
20 May 2008-Analyst
TL;DR: Recent developments in antibody immobilization methods are discussed with a particular focus on the strengths and limitations of reported approaches, and thereby provide a useful guideline for the selection of suitable antibody coupling procedures.
Abstract: Antibody immobilization on a solid support is an essential process for the development of most immune-based assay systems. The choice of the immobilization method greatly affects antibody–antigen interactions on the assay surface. For the past several years, numerous strategies have been reported to control antibody immobilization, mainly by directing the orientation, stability, and density of bound antibodies on different assay platforms. Here we discuss recent developments in antibody immobilization methods with a particular focus on the strengths and limitations of reported approaches, and thereby provide a useful guideline for the selection of suitable antibody coupling procedures.

256 citations


Journal ArticleDOI
20 Oct 2008-Analyst
TL;DR: This communication reports that three prostate cancer cells of differing metastatic potential were discriminated based on their Young's moduli which were determined using AFM and the Hertz model.
Abstract: This communication reports that three prostate cancer cells of differing metastatic potential were discriminated based on their Young's moduli (LNCaP - 287 +/- 52 N m(-2), PC-3 - 1401 +/- 162 N m(-2) and BPH - 2797 +/- 491 N m(-2)) which were determined using AFM and the Hertz model.

250 citations


Journal ArticleDOI
24 Jun 2008-Analyst
TL;DR: Techniques for the characterization of the nanoparticle-doped materials and methods for the determination of their efficacy against biofilm formation are described.
Abstract: Anti-microbial materials have multiple applications in medicine, industry and commercial products. Recent research has proposed the use of nanoparticles in a range of materials, as some metal nanoparticles are known to possess antibacterial properties. The development of such materials presents both the chemist and the biologist with the challenge to effectively choose analytical methods that provide relevant information regarding these materials. Herein, we describe techniques for the characterization of the nanoparticle-doped materials and methods for the determination of their efficacy against biofilm formation.

244 citations


Journal ArticleDOI
09 Sep 2008-Analyst
TL;DR: This Highlight article provides an introduction to the field, and showcases the different ionization approaches reported since 2004, with an emphasis on the most recent developments.
Abstract: Ambient ionization techniques enable the interrogation of a variety of samples in their native state by mass spectrometry, and are rapidly advancing all fields where screening for the presence of various analytes in a broadband and/or high-throughput fashion is desirable. This Highlight article provides an introduction to the field, and showcases the different ionization approaches reported since 2004, with an emphasis on the most recent developments.

222 citations


Journal ArticleDOI
21 Apr 2008-Analyst
TL;DR: The review focusses on the use of antibodies, enzymes, biologically-inspired synthetic ligands and whole-cell biosensors, providing a flavour of the range of technology, formats and approaches that can be used to detect explosives using biological systems.
Abstract: This article provides a review of the published literature describing the use of biosensors and biologically-inspired systems for explosives detection. The review focusses on the use of antibodies, enzymes, biologically-inspired synthetic ligands and whole-cell biosensors, providing a flavour of the range of technology, formats and approaches that can be used to detect explosives using biological systems.

158 citations


Journal ArticleDOI
20 May 2008-Analyst
TL;DR: This review focuses on the mass spectral analysis of glycopeptides, after subjecting the glycoprotein to proteolysis, which is useful in characterizing glycan heterogeneity and correlating glycan compositions to their attachment sites on the protein.
Abstract: Glycosylation is one of the most important post-translational modifications found in nature. Identifying and characterizing glycans is an important step in correlating glycosylation structure to the glycan's function, both in normal glycoproteins and those that are modified in a disease state. Glycans on a protein can be characterized by a variety of methods. This review focuses on the mass spectral analysis of glycopeptides, after subjecting the glycoprotein to proteolysis. This analytical approach is useful in characterizing glycan heterogeneity and correlating glycan compositions to their attachment sites on the protein. The information obtained from this approach can serve as the foundation for understanding how glycan compositions affect protein function, in both normal and aberrant glycoproteins.

153 citations


Journal ArticleDOI
21 Jul 2008-Analyst
TL;DR: The behaviour of the method of standard additions under a range of conditions is looked at, and it is found that, if executed optimally, there is no noteworthy loss of precision.
Abstract: Standard additions is a calibration technique devised to eliminate rotational matrix effects in analytical measurement. Although the technique is presented in almost every textbook of analytical chemistry, its behaviour in practice is not well documented and is prone to attract misleading accounts. The most important limitation is that the method cannot deal with translational matrix effects, which need to be handled separately. In addition, because the method involves extrapolation from known data, the method is often regarded as less precise than external calibration (interpolation) techniques. Here, using a generalised model of an analytical system, we look at the behaviour of the method of standard additions under a range of conditions, and find that, if executed optimally, there is no noteworthy loss of precision.

149 citations


Journal ArticleDOI
24 Jun 2008-Analyst
TL;DR: M WCNT-BPPGE and MWCNT-SPE are successfully utilized for the determination of capsaicin in real samples, such as a few commercially available hot pepper sauces, and the determined values are in excellent agreement and correlation with the average Scoville unit values reported in the literature for these sauces.
Abstract: A sensitive electroanalytical methodology for the determination of capsaicin using adsorptive stripping voltammetry (AdsSV) at a multiwalled carbon nanotube modified basal plane pyrolytic graphite electrode (MWCNT-BPPGE) is presented. This analytical method is then further developed using a multiwalled carbon nanotube screen-printed electrode (MWCNT-SPE) demonstrating the proof-of-concept that this approach can easily be incorporated into a sensing device which is both facile to use and inexpensive to produce. Capsaicin is the chemical responsible for the hot taste of chilli peppers, and measuring the concentration of capsaicin is an indicator of how hot any given chilli pepper, hot sauce and other related foodstuffs are. Standard additions plots for AdsSV of capsaicin at open circuit potential at a MWCNT-BPPGE exhibits two linear ranges, from 0.5 to 15 μM and from 15 to 60 μM. Using the first range of calibration curve, a detection limit of 0.31 μM (based on 3σ) is obtained. The plot of standard additions of capsaicin determined using the disposable MWCNT-SPE shows a linear range between 0.5 and 35 μM and a detection limit of 0.45 μM. MWCNT-BPPGE and MWCNT-SPE are successfully utilized for the determination of capsaicin in real samples, such as a few commercially available hot pepper sauces, and the determined values are in excellent agreement and correlation with the average Scoville unit values reported in the literature for these sauces. To the best of our knowledge, this is the first electroanalytical method using MWCNT-BPPGE or MWCNT-SPE reported for the determination of capsaicin. This method offers advantages such as precision and objectivity over the well-known but potentially subjective Scoville method (based on organoleptic testing by human tasting panels) and is facile and inexpensive compared to existing HPLC methods.

Journal ArticleDOI
20 May 2008-Analyst
TL;DR: This review summarizes the spectrum of both, DNA-modification techniques used for assay enhancement and the resulting key applications of the highly sensitive immuno-PCR method, which focuses on chimeric conjugates of specific antibodies and nucleic acid molecules.
Abstract: The versatility of immunoassays for the detection of antigens can be combined with the signal amplification power of nucleic acid amplification techniques in a broad range of innovative detection strategies. This review summarizes the spectrum of both, DNA-modification techniques used for assay enhancement and the resulting key applications. In particular, it focuses on the highly sensitive immuno-PCR (IPCR) method. This technique is based on chimeric conjugates of specific antibodies and nucleic acid molecules, the latter of which are used as markers to be amplified by PCR or related techniques for signal generation and read-out. Various strategies for the combination of antigen detection and nucleic acid amplification are discussed with regard to their laboratory analytic performance, including novel approaches to the conjugation of antibodies with DNA, and alternative pathways for signal amplification and detection. A critical assessment of advantages and drawbacks of these methods for a number of applications in clinical diagnostics and research is conducted. The examples include the detection of viral and bacterial antigens, tumor markers, toxins, pathogens, cytokines and other targets in different biological sample materials.

Journal ArticleDOI
21 Jul 2008-Analyst
TL;DR: Recent progress in the use of microarrays for high-throughput biomarker profiling is highlighted and some of the challenges associated with these efforts are discussed.
Abstract: The application of protein biomarkers as an aid for the detection and treatment of diseases has been subject to intensified interest in recent years. The quantitative assaying of protein biomarkers in easily obtainable biological fluids such as serum and urine offers the opportunity to improve patient care via earlier and more accurate diagnoses in a convenient, non-invasive manner as well as providing a potential route towards more individually targeted treatment. Essential to achieving progress in biomarker technology is the ability to screen large numbers of proteins simultaneously in a single experiment with high sensitivity and selectivity. In this article, we highlight recent progress in the use of microarrays for high-throughput biomarker profiling and discuss some of the challenges associated with these efforts.

Journal ArticleDOI
25 Feb 2008-Analyst
TL;DR: It is shown that OFRR can detect M13 with high specificity and sensitivity and will lead to development of novel OFRR-based, sensitive, rapid, and low-cost micro total analysis devices for virus detection.
Abstract: We have demonstrated sensitive label-free virus detection using the opto-fluidic ring resonator (OFRR) sensor. The OFRR is a novel sensing platform that integrates the microfluidics and photonic sensing technology with a low detection limit and small volume. In our experiment, filamentous bacteriophage M13 was used as a safe model system. Virus samples were flowed through the OFRR whose surface was coated with M13-specific antibodies. We studied the sensor performance by monitoring in real-time the virus and antibody interaction. It is shown that OFRR can detect M13 with high specificity and sensitivity. The detection limit is approximately 2.3 × 103 pfu mL−1 and the detection dynamic range spanned seven orders of magnitude. Theoretical analysis was also carried out to confirm the experimental results. Our study will lead to development of novel OFRR-based, sensitive, rapid, and low-cost micro total analysis devices for virus detection.

Journal ArticleDOI
28 Jan 2008-Analyst
TL;DR: Infrared laser-assisted desorption electrospray ionization (IR LADESI) mass spectrometry was used for the direct analysis of water-containing samples under ambient conditions and yielded mass spectra similar to those obtained by conventional electrosPRay.
Abstract: We have used an infrared laser for desorption of material and ionization by interaction with electrosprayed solvent. Infrared laser-assisted desorption electrospray ionization (IR LADESI) mass spectrometry was used for the direct analysis of water-containing samples under ambient conditions. An ion trap mass spectrometer was modified to include a pulsed Er:YAG laser at 2.94 microm wavelength coupled into a germanium oxide optical fiber for desorption at atmospheric pressure and a nanoelectrospray source for ionization. Analytes in aqueous solution were placed on a stainless steel target and irradiated with the pulsed IR laser. Material desorbed and ablated from the target was ionized by a continuous stream of charged droplets from the electrosprayed solvent. Peptide and protein samples analyzed using this method yield mass spectra similar to those obtained by conventional electrospray. Blood and urine were analyzed without sample pretreatment to demonstrate the capability of IR LADESI for direct analysis of biological fluids. Pharmaceutical products were also directly analyzed. Finally, the role of water as a matrix in the IR LADESI process is discussed.

Journal ArticleDOI
28 Jan 2008-Analyst
TL;DR: FTIR spectral imaging was applied on formalin-fixed paraffin-embedded biopsies from colon and skin cancerous lesions and tumour areas were successfully demarcated from the rest of the tissue in both Colon and skin independently of the embedding material and of the substrate.
Abstract: FTIR spectral imaging was applied on formalin-fixed paraffin-embedded biopsies from colon and skin cancerous lesions. These samples were deposited onto different substrates (zinc selenide and calcium fluoride respectively) and embedded using two types of paraffin. Formalin fixation followed by paraffin embedding is the gold standard in tissue storage. It can preserve molecular structures and it is compatible with immunohistochemistry. However, paraffin absorption bands are significant in the mid-infrared region and can mask some molecular vibrations of the tissue. Direct data processing was applied on spectral images without any chemical dewaxing of the tissues. Extended Multiplicative Signal Correction was used to correct the spectral contribution from paraffin. For this purpose, the signal of paraffin was modelled using Principal Component Analysis and paraffin spectra were removed from the raw images based on an outlier detection. Then, pseudo-colour images were computed by K-means clustering in order to highlight histological structures of interest. This robust chemometrics methodology was applied on the two samples. Tumour areas were successfully demarcated from the rest of the tissue in both colon and skin independently of the embedding material and of the substrate.

Journal ArticleDOI
20 Oct 2008-Analyst
TL;DR: The first multiplexed simultaneous detection of six different DNA sequences, corresponding to different strains of the Escherichia coli bacterium, each labelled with a different commercially available dye label is reported, with the aid of multivariate analysis.
Abstract: The labelling of target biomolecules followed by detection using some form of optical spectroscopy has become common practice to aid in their detection. This approach has allowed the field of bioanalysis to dramatically expand; however, most methods suffer from the lack of the ability to discriminate between the components of a complex mixture. Currently, fluorescence spectroscopy is the method of choice but its ability to multiplex is greatly hampered by the broad overlapping spectra which are obtained. Surface enhanced resonance Raman scattering (SERRS) holds many advantages over fluorescence both in sensitivity and, more importantly here, in its ability to identify components in a mixture without separation due to the sharp fingerprint spectra obtained. Here the first multiplexed simultaneous detection of six different DNA sequences, corresponding to different strains of the Escherichia coli bacterium, each labelled with a different commercially available dye label (ROX, HEX, FAM, TET, Cy3, or TAMRA) is reported. This was achieved with the aid of multivariate analysis, also known as chemometrics, which can involve the application of a wide range of statistical and data analysis methods. In this study, both exploratory discriminant analysis and supervised learning, by partial least squares (PLS) regression, were used and the ability to discriminate whether a particular labelled oligonucleotide was present or absent in a mixture was achieved using PLS with very high sensitivity (0.98–1), specificity (0.98–1), accuracy (range 0.99–1), and precision (0.98–1).

Journal ArticleDOI
01 Dec 2008-Analyst
TL;DR: BMAA was successfully identified and quantified in cycad seeds, whereas previously reported findings of BMAA in samples of cyanobacteria could not be confirmed, and the presence of alpha-,gamma-diamino butyric acid (DAB), an isomer ofBMAA, was confirmed in one sample.
Abstract: A highly specific method for the analysis of β-N-methylamino-L-alanine (BMAA) by LC-MS/MS (liquid chromatography tandem mass spectrometry) has been developed and applied for cycad seeds and cyanobacteria. BMAA was analysed as a free fraction or as total BMAA after acidic hydrolysis to release any protein-bound BMAA. Deuterium labelled BMAA was synthesised and used as internal standard. The method comprises HILIC (hydrophilic interaction chromatography) and positive electrospray ionisation of the native compound, i.e. no derivatisation was used. For safe identification five specific product ions (m/z 102, 88, 76, 73 and 44), all derived from a precursor ion of m/z 119 and originating from different parts of the molecule, were detected (typical relative abundance 100%, 16%, 14%, 12% and 22% respectively). Cyanobacteria or muscle tissue was spiked with BMAA (10 to 1000 µg g−1) to validate the method (accuracy 95% to 109%, relative standard deviation 1% to 6%). The detection limit for free and total BMAA in tissue was <1 µg g−1 and <4 µg g−1 respectively. BMAA was successfully identified and quantified in cycad seeds, whereas previously reported findings of BMAA in samples of cyanobacteria could not be confirmed. Instead, the presence of α-,γ-diamino butyric acid (DAB), an isomer of BMAA, was confirmed in one sample. The possible implications of this finding are discussed.

Journal ArticleDOI
28 Jan 2008-Analyst
TL;DR: It is demonstrated that although challenging, the application of an improved water suppression technique allows NMR spectra of DOM to be obtained directly (i.e without pre-concentration) for major bodies of water, including rivers, lakes and the ocean.
Abstract: Nuclear magnetic resonance (NMR) spectroscopy arguably provides the greatest insight into the overall chemical composition of dissolved organic matter (DOM). However, in a standard 5 mm NMR probe, a sample of sea water at natural abundance only contains ca. 500–600 ng of organic matter, distributed among the heterogeneous components of DOM. Additionally, the intensity of the water signal, which may be many orders of magnitude greater than the signals from DOM, makes the detection and analysis of DOM at natural abundance extremely demanding. Here, we demonstrate, that although challenging, the application of an improved water suppression technique allows NMR spectra of DOM to be obtained directly (i.e without pre-concentration) for major bodies of water, including rivers, lakes and the ocean. The technique described here provides a compositional overview of an intact sample, permitting researchers to investigate and assess the impact of concentration, isolation and extraction procedures that are employed routinely. Also the technique permits NMR to be performed on ‘precious’ samples for which traditional isolations are not possible, for example, water from ice cores and pore water, which are key in hydrology and for paleoclimatic reconstruction.

Journal ArticleDOI
25 Feb 2008-Analyst
TL;DR: The novelty of this system lies in the cost-effective integration of microfluidics, optics, and electronics to realize a fully portable and inexpensive system for performing both genetic amplification and analysis - the basis of many medical diagnostics.
Abstract: We present an inexpensive, portable and integrated microfluidic instrument that is optimized to perform genetic amplification and analysis on a single sample. Biochemical reactions and analytical separations for genetic analysis are performed within tri-layered glass-PDMS microchips. The microchip itself consists of integrated pneumatically-actuated valves and pumps for fluid handling, a thin-film resistive element that acts simultaneously as a heater and a temperature sensor, and channels for capillary electrophoresis (CE). The platform is comprised of high voltage circuitry, an optical assembly consisting of a laser diode and a charged coupled device (CCD) camera, circuitry for thermal control, and mini-pumps to generate vacuum/pressure to operate the on-chip diaphragm-based pumps and valves. Using this microchip and instrument, we demonstrate an integration of reverse transcription (RT), polymerase chain reaction (PCR), and capillary electrophoresis (CE). The novelty of this system lies in the cost-effective integration of microfluidics, optics, and electronics to realize a fully portable and inexpensive system (on the order of $1000 in component costs) for performing both genetic amplification and analysis - the basis of many medical diagnostics. We believe that this combination of portability, cost-effectiveness and performance will enable more accessible healthcare.

Journal ArticleDOI
15 Aug 2008-Analyst
TL;DR: In this article, recent techniques developed for phosphoproteome analysis are reviewed with an emphasis on the new developments in this field in China.
Abstract: Protein phosphorylation is one of the most biologically relevant and ubiquitous post-translational modifications. The analysis of protein phosphorylation is very challenging due to its highly dynamic nature and low stoichiometry. In this article, recent techniques developed for phosphoproteome analysis are reviewed with an emphasis on the new developments in this field in China. To improve the performance of phosphoproteome analysis, many novel methods, either by application of new separation mechanisms or by adoption of new separation materials, were developed to specifically enrich phosphopeptides from complex protein digests. A series of new materials, including nanostructure materials, magnetic materials, and monolithic materials, were applied to prepare immobilized affinity chromatography or metal oxide affinity chromatography to improve the performance of phosphopeptide enrichment. Besides, new software tools were also developed to validate phosphopeptide identification and predict kinase specific phosphorylation sites.

Journal ArticleDOI
21 Jul 2008-Analyst
TL;DR: This work presents here, in a non-exhaustive way, the recent advances in the two steps of immobilization and detection that rely upon increasing integration of the number of reading points or/and of the reading strategy.
Abstract: The concept of DNA biosensors is sustained by the need for rapid and highly sensitive analytical tools for genetic detection. Their implementation is based on three key steps: (i) immobilization of single-stranded oligonucleotide probes onto a substrate; (ii) hybridization and (iii) reading. These steps involve complementary knowledge in various disciplinary fields such as surface physics and chemistry, molecular electrochemistry, micro-technologies, optics, electronics and biochemistry. We present here, in a non-exhaustive way, the recent advances in the two steps of immobilization and detection that rely upon increasing integration of the number of reading points or/and of the reading strategy.

Journal ArticleDOI
21 Jul 2008-Analyst
TL;DR: This finding is a significant contribution to the efforts aiming at overcoming one of the most significant drawbacks of the solid-state ISEs, that is the potential drift observed during continuous measurements, and could lead to the development of both cation- and anion-sensitive systems.
Abstract: In this work, C60fullerene is used as an electrochemical mediator for the development of an all-solid-state ISE. The unique electrochemical characteristics of the fullerenes allow for the facile ion-to-electron transduction across the ionically active polymeric ion-selective membrane and the electrochemically active glassy carbon transducer. The interfacial ion-to-electron charge transfer was investigated by Electrochemical Impedance Spectroscopy. The study of the analytical characteristics of a model potassium-selective electrode, together with the EIS studies, reveals that, indeed, the interfacial C60 electrochemically active layer facilitates the ion-to-electron transduction, providing a stable and reversible solid-state ISE system. This finding is a significant contribution to the efforts aiming at overcoming one of the most significant drawbacks of the solid-state ISEs, that is the potential drift observed during continuous measurements, and could lead to the development of both cation- and anion-sensitive systems.

Journal ArticleDOI
20 Oct 2008-Analyst
TL;DR: This review covers publications involving AC-SECM from its beginning to date and the findings of several research groups are thematically structured along with the specific experimental procedures to enable researchers to rationally choose purposeful parameters for their AC- SECM experiments.
Abstract: Alternating current scanning electrochemical microscopy (AC-SECM) is a growing branch within the variety of SECM methods. This review covers publications involving AC-SECM from its beginning to date. The findings of several research groups are thematically structured along with the specific experimental procedures. This should enable researchers to rationally choose purposeful parameters for their AC-SECM experiments.

Journal ArticleDOI
25 Feb 2008-Analyst
TL;DR: The combination of the environmentally inert, aqueous nanoparticle dispersion with the inkjet printing technique allowed the rapid fabrication of sensors based on polyaniline that was not easily achievable in the past due to the lack of processability of bulk forms of the conducting polymer.
Abstract: A sensor for the amperometric detection of aqueous ammonia was fabricated using the inkjet printing of dodecylbenzene sulfonate (DBSA)-doped polyaniline nanoparticles (nanoPANI) onto a screen-printed carbon paste electrode. The combination of the environmentally inert, aqueous nanoparticle dispersion with the inkjet printing technique allowed the rapid fabrication of sensors based on polyaniline that was not easily achievable in the past due to the lack of processability of bulk forms of the conducting polymer. The resulting modified electrode was characterised with respect to its operating pH and number of print layers and was found to perform optimally at near neutral pH with four nanoPANI inkjet-printed layers. The sensor was tested in a flow injection system for its response to aqueous ammonia using amperometric detection at −0.3 V vs. Ag/AgCl pseudo-reference and was found to have reproducibility to injections of ammonia of below 5% RSD and good sensitivity with an experimental detection limit of 20 µM and a theoretical detection limit of 3.17 µM (0.54 ppm). The sensor was also tested for its day-to-day stability and its response towards a range of interferents common to refrigerant waste waters. This system allows the rapid production of an ultra-low-cost, solid state, polyaniline-based aqueous ammonia sensor.

Journal ArticleDOI
20 Oct 2008-Analyst
TL;DR: Desorption electrospray ionization was used to examine cotton transfer swabs used for travel security sample collection in the screening process and high throughput quantitative analysis of fabric surfaces for targeted analytes is reported.
Abstract: Desorption electrospray ionization (DESI) is applied to the rapid, in-situ, direct qualitative and quantitative analysis of mixtures of explosives and drugs from a variety of fabrics, including cotton, silk, denim, polyester, rayon, spandex, leather and their blends The compounds analyzed were explosives: trinitrohexahydro-1,3,5-triazine (RDX), octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine (HMX), 2,4,6-trinitrotoluene (TNT), pentaerythritol tetranitrate (PETN) and the drugs of abuse: heroin, cocaine, and methamphetamine Limits of detection are in the picogram range DESI analyses were performed without sample preparation and carried out in the presence of common interfering chemical matrices, such as insect repellant, urine, and topical lotions Spatial and depth profiling was investigated to examine the depth of penetration and lateral resolution DESI was also used to examine cotton transfer swabs used for travel security sample collection in the screening process High throughput quantitative analysis of fabric surfaces for targeted analytes is also reported

Journal ArticleDOI
21 Apr 2008-Analyst
TL;DR: A colorimetric bioassay based on the aggregation of carbohydrate-stabilised gold nanoparticles which has been used to detect Ricinus communis Agglutinin 120 (RCA(120) - a ricin surrogate is presented.
Abstract: Ricin is a toxic lectin which presents a potential security threat. Its rapid detection is highly desirable. Here we present a colorimetric bioassay based on the aggregation of carbohydrate-stabilised gold nanoparticles which has been used to detect Ricinus communis Agglutinin 120 (RCA120) – a ricin surrogate. To achieve a stable and robust sensing system the anchor chain length and the density of the assembled carbohydrates on the gold particle surface has been examined to determine the optimal coverage for maximal aggregation with both RCA120 and Concanavalin A (Con A) lectins. Gold nanoparticles were stabilised with either a thiolated galactose derivative (9-mercapto-3,6-diaoxaoctyl-β-D-galactoside) or a thiolated mannose derivative (9-merapto-3,6-dioxaoctyl-α-D-mannoside), for RCA120 and Con A respectively, diluted in each instance with varying ratios of a thiolated triethylene glycol derivative. Aggregation was induced with the respective cognate lectin with the reaction monitored by UV-visible spectrophotometry. The results obtained show that a particle surface with at least 7.5% galactose is required for aggregation with RCA120 and 6% mannose coverage is required for aggregation with Con A. For each lectin the sensitivity of the assay could be controlled by adjustment of the carbohydrate density on the gold nanoparticles, but with differing results. Maximal aggregation with Con A was achieved with a monolayer consisting of 100% mannose, whereas for RCA120 maximal aggregation occurred with 70% coverage of galactose. The limit of detection for RCA120 using the optimally presented galactose-stabilised nanoparticles was 9 nM.

Journal ArticleDOI
09 Sep 2008-Analyst
TL;DR: FT-IR with PLSR was able to acquire a metabolic fingerprint rapidly and quantify the microbial load of milk samples accurately, with very little sample preparation, and it is believed that metabolic fingerprinting using FT-IR has very good potential for future use in the dairy industry as a rapid method of detection and enumeration.
Abstract: Microbiological safety plays a very significant part in the quality control of milk and dairy products worldwide. Current methods used in the detection and enumeration of spoilage bacteria in pasteurized milk in the dairy industry, although accurate and sensitive, are time-consuming. FT-IR spectroscopy is a metabolic fingerprinting technique that can potentially be used to deliver results with the same accuracy and sensitivity, within minutes after minimal sample preparation. We tested this hypothesis using attenuated total reflectance (ATR), and high throughput (HT) FT-IR techniques. Three main types of pasteurized milk – whole, semi-skimmed and skimmed – were used and milk was allowed to spoil naturally by incubation at 15 °C. Samples for FT-IR were obtained at frequent, fixed time intervals and pH and total viable counts were also recorded. Multivariate statistical methods, including principal components-discriminant function analysis and partial least squares regression (PLSR), were then used to investigate the relationship between metabolic fingerprints and the total viable counts. FT-IR ATR data for all milks showed reasonable results for bacterial loads above 105 cfu ml−1. By contrast, FT-IR HT provided more accurate results for lower viable bacterial counts down to 103 cfu ml−1 for whole milk and, 4 × 102 cfu ml−1 for semi-skimmed and skimmed milk. Using FT-IR with PLSR we were able to acquire a metabolic fingerprint rapidly and quantify the microbial load of milk samples accurately, with very little sample preparation. We believe that metabolic fingerprinting using FT-IR has very good potential for future use in the dairy industry as a rapid method of detection and enumeration.

Journal ArticleDOI
25 Feb 2008-Analyst
TL;DR: An electrochemical sensors employing superparamagnetic iron oxide (Fe3O4) nanoparticles with a surface functionalization of dimercaptosuccinic acid (DMSA) has been developed that could detect background level of Pb and yielded linear responses from 0 to 50ppm, excellent reproducibility, and Pb concentrations comparable to those measured by ICP-MS.
Abstract: Urine is universally recognized as one of the best non-invasive matrices for biomonitoring exposure to a broad range of xenobiotics, including toxic metals. Detection of metal ions in urine has been problematic due to the protein competition and electrode fouling. For direct, simple, and field-deployable monitoring of urinary Pb, electrochemical sensors employing superparamagnetic iron oxide (Fe3O4) nanoparticles with a surface functionalization of dimercaptosuccinic acid (DMSA) has been developed. The metal detection involves rapid collection of dispersed metal-bound nanoparticles from a sample solution at a magnetic or electromagnetic electrode, followed by the stripping voltammetry of the metal in acidic medium. The sensors were evaluated as a function of solution pH, the binding affinity of Pb to DMSA–Fe3O4, the ratio of nanoparticles per sample volume, preconcentration time, and Pb concentrations. The effect of binding competitions between the DMSA–Fe3O4 and urine constituents for Pb on the sensor responses was studied. After 90 s of preconcentration in samples containing 25 vol.% of rat urine and 0.1 g L−1 of DMSA–Fe3O4, the sensor could detect background level of Pb (0.5 ppb) and yielded linear responses from 0 to 50 ppb of Pb, excellent reproducibility (%RSD of 5.3 for seven measurements of 30 ppb Pb), and Pb concentrations comparable to those measured by ICP-MS. The sensor could also simultaneously detect background levels (<1 ppb) of Cd, Pb, Cu, and Ag in river and seawater.

Journal ArticleDOI
15 Aug 2008-Analyst
TL;DR: Anodic electrochemiluminescence of CdSe quantum dots in a neutral system was for the first time observed at a relatively low potential by using sulfite as a co-reactant to produce the ECL emission at an indium tin oxide (ITO) electrode.
Abstract: Anodic electrochemiluminescence (ECL) of CdSe quantum dots (QDs) in a neutral system was for the first time observed at a relatively low potential by using sulfite as a co-reactant to produce the ECL emission at an indium tin oxide (ITO) electrode, which could be used for the sensitive detection of ECL quenchers using dopamine (DA) as a model molecule.