Field desorption mass spectrometry,fast atom bombardment mass spectrometry and fast atom bombardment tandem mass spectrometry of echinacoside,the main caffeoyl-glycoside from Echinacea angustifolia roots (Asteraceae)

The mass spectral fragmentation of echinacoside, a pharmacologically active caffeoyl-glycoside isolated from Echinacea angustifolia roots, has been investigated using different soft-ionization techniques, field desorption and fast atom bombardment (positive and negative ions) mass Spectrometry. Both ionization modes are successful in molecular mass determination and furnish approximately equivalent structural information. A fast atom bombardment tandem mass spectrometry approach (negative ions) was developed for the study of the fragmentation pathways and for the detection of echinacoside in crude plant extracts. The results demonstrate the usefulness of this technique for the rapid search of this important caffeoyl-glucoside directly in natural complex matrices.     

Simultaneous analysis of glycolipids and phospholids molecular species in avocado (Persea americana Mill) fruit

The molecular species of phospholipids (PLs) and glycolipids (GLs) were simultaneously characterized in the pulp and almond of the avocado fruit (Persea americana Mill) of four varieties by means of high performance liquid chromatography-electrospray ionisation ion-trap tandem mass spectrometry. In the pulp, the predominant species of monoglycosyldiglycerides (MGD) were m/z 796.6 (oleic/linolenic and linoleic/linoleic acids) and m/z 800.4 (stearic/linoleic and oleic/oleic acids). One of the main diglycosyldiglycerides (DGD) both in the pulp and almond was m/z 958.5 (oleic/linolenic); however, the pulp was also rich of m/z 962.4 (oleic/oleic), whereas in the almond, m/z 934.5 (palmitic/linoleic and palmitoleic/oleic) and m/z 960.5 (oleic/linoleic and stearic/linolenic) were more abundant. In the almond, the main PL classes (phosphatidic acid (PA), phosphatidylcholine (PC), phosphatidylethanolamine (PE) and phosphatidylinositol (PI)) contained always palmitic/linoleic acids. Alpha-linolenic acid was contained as MGD (linolenic/linolenic) and DGD (linolenic/linolenic), more present in the pulp than in the almond. The major molecular species of glycocerebrosides (GCer) in the pulp and almond carried hydroxy-palmitic acid (C(16h:0))/4,8-sphyngadienine (d(18:2)).     

Graphene transistors via in situ voltage-induced reduction of graphene-oxide under ambient conditions

Here, we describe a simple approach to fabricate graphene-based field-effect-transistors (FETs), starting from aqueous solutions of graphene-oxide (GO), processed entirely under ambient conditions. The process relies on the site-selective reduction of GO sheets deposited in between or on the surface of micro/nanoelectrodes. The same electrodes are first used for voltage-induced electrochemical GO reduction, and then as the source and drain contacts of FETs, allowing for the straightforward production and characterization of ambipolar graphene devices. With the use of nanoelectrodes, we could reduce different selected areas belonging to one single sheet as well.     

Mapping electric fields generated by microelectrodes using optically trapped charged microspheres

In this work, we show a new technique to measure the direction and amplitude of the electric field generated by microelectrodes in a liquid environment, as often used in microfluidic devices. The method is based on the use of optical tweezers as a force transducer. A trapped, charged particle behaves as a probe. With this technique, it is possible to obtain a detailed map of the electric field, even for very complex electrode structures with a resolution below a micrometre and with a sensitivity as low as a few hundreds of V m(-1).     

Communication: Conformation state diagram of polypeptides: a chain length induced α-β transition

By using a generic coarse grained polypeptide model, we perform multicanonical molecular dynamics simulations for determining the equilibrium conformation state diagram of a single homopolypeptide chain as a function of the chain length and temperature. The state diagram highlights the thermal regimes of stability for various conformational patterns in polypeptides, including swollen, random and collapsed coils, globular structures, extended and bended α helices, and compact β bundles. Remarkably, at low temperatures we observe a sharp transition from extended α helix to compact β bundles as the chain length increases. This finding indicates that the chain length is one of the intrisic factors that can trigger α-β transformations in a broad class of polypeptides.     

Rapid and selective determination of UV filters in seawater by liquid chromatography-tandem mass spectrometry combined with stir bar sorptive extraction

Fast liquid chromatography coupled to triple-quadrupole tandem mass spectrometry was employed for the determination of six UV filters in seawater. The separation of the analytes was achieved in less than 5 min; polarity switching was used as four of the analytes were ionized in positive mode and the remaining two in negative mode. Two ionization sources were employed and compared: atmospheric pressure chemical ionization (APCI) gave better results than electrospray ionization (ESI) for all analytes, with higher reproducibility and lower detection limits. Therefore APCI was chosen for the determination of the analytes in seawater samples using stir bar sorptive extraction-liquid desorption (SBSE-LD).Quantitative analysis was performed in multiple reaction monitoring (MRM) mode; fragmentation pathways of the analytes with regard to the formation of the MRM ions were also proposed.For the analysis of seawater samples, calibration curves were drawn using SBSE in spiked seawater. All figures of merit of the method were satisfactory; limits of detection were particularly low for the four analytes ionized in positive mode, being in the range 8-31 ng/L. The method was applied to the determination of the six UV filters in seawater samples from Liguria, Italy. Only benzophenone-3 (BP-3) and ethylhexyl methoxycinnamate (EHMC) were measured in the analyzed samples; some of the remaining analytes were also detected but always below the limit of quantitation.     

High-throughput tools for the study of protein-nanostructured surface interaction

The aim of this review is to describe and to analyze the ingredients that are necessary in order to develop a robust and effective experimental approach for the high-throughput characterization of protein-nanostructured surface interaction. In the first part of this paper we review the nanostructured surface synthesis methods that are potentially able to create nanostructured inorganic surface libraries. In the second part, we address another fundamental aspect consisting in the availability of high-throughput proteins detection methods. We describe in details new emerging analytical tools compatible with nanostructured surfaces, analyzing different possible strategies, depending on the objective of the experiment and on the library format.     

A variational view at the time-dependent minimal surface equation

We present a global variational approach to the L ²-gradient flow of the area functional of cartesian surfaces through the study of the so-called weighted energy-dissipation (WED) functional. In particular, we prove a relaxation result which allows us to show that minimizers of the WED converge in a quantitatively prescribed way to gradient-flow trajectories of the relaxed area functional. The result is then extended to general parabolic quasilinear equations arising as gradient flows of convex functionals with linear growth.     

Subpicometer length measurement using semiconductor laser tracking frequency gauge

We have demonstrated heretofore unattained distance precision of 0.14 pm (2 pm) incremental and 14 nm (2.9 μm) absolute in a resonant (nonresonant) interferometer at an averaging time of 1 s, using inexpensive telecommunications diode lasers. We have controlled the main source of error, that due to spurious reflection and the resulting amplitude modulation. In the resonant interferometer, absolute distance precision is well under λ/6. Therefore, after an interruption, an absolute distance measurement can be used to return to the same interferometer order.     

Reactivity of rimsulfuron in newly formed inclusion combinations by using cyclodextrin and zeolite

Extending our investigations on environment protection by agrochemicals diffusion and accumulation, newly formed inclusion combinations of rimsulfuron into zeolite-NaY (Z-NaY) and β-cyclodextrin (β-CD) were studied and compared. The reactivity of the included herbicide under UV-irradiation and in the dark was assessed. Many guest/host ratios were tested: the best results were found using 3?g (6.953?mmol) of rimsulfuron per kilogram of zeolite, with 80% inclusion success (5.562?mmol?kg^?1), and a 1:?2 molar ratio, 190?g of rimsulfuron per kilogram of β-CD with 58% inclusion success. The herbicide Z-NaY-combined underwent rapid and effective (halflive 2–7?h) degradation either catalytically or photochemically, giving rise to different identified by-products. On the contrary, β-CD was able to protect rimsulfuron totally both in the dark and under 24-h direct UV irradiation. On the basis of the obtained results, a different utilization of the two inclusion materials has been suggested.