Simultaneous determination of fluoroquinolones,sulfonamides and tetracyclines in sewage sludge by pressurized liquid extraction and liquid chromatography electrospray ionization-mass spectrometry

A new scheme for the quantitative determination of traces of fluoroquinolones (FQs), tetracyclines (TCs) and sulfonamides (SAs) in sewage sludge was developed. The compounds were simultaneously extracted from sewage sludge by pressurized liquid extraction (PLE). A novel and effective method for PLE was developed. Solid-phase extraction was used for cleaning up the extracts. Identification and quantification of the compounds was done using high-performance liquid chromatography with electrospray ionization mass spectrometry in selected reaction monitoring mode. The best recovery of FQs and TCs was obtained by using hydrophilic–lipophilic balance cartridges, recoveries ranged 59% for norfloxacin to 82% for ofloxacin and 95% for doxycycline; for SAs strong cation-exchange cartridges were more efficient, recoveries were 96% for sulfamethoxazole and 43% for sulfadimethoxine. Limit of quantification ranged from 0.1 ng/g for SAs to 160 ng/g for tetracycline. Method precision for TCs was 5.06% and 1.12%, and for SAs 0.43% and 2.01%. FQs precision ranged from 0.77% to 1.89%.     

Isomerism,total decay energies,and absolute γ-ray intensities of the heavy Pd and Ag isotopes

The decays of^{113, 114, 115g, 115m, 116}Pd have been studied with an emphasis on the determinations of total decay energies and absoluteγ-ray intensities. The experiments also provided improved data on these quantities for the decays of^{114, 115g, 115m, 116m}Ag. A search for isomeric transitions using a high resolution electron detector resulted in the identification of isomericE3 transitions in¹¹⁵Pd and^{113, 115, 116, 117}Ag. The isomeric branching was determined in all cases. TheQ _β-values of^113–116Pd and^113–116Ag have been measured using aβγ-coincidence method.     

Fragmentation of 370 MeV/n 20Ne and 470 MeV/n 24Mg in light targets

Total charge-changing cross sections and cross sections for the production of projectile-like fragments were determined for fragmentation reactions induced by 370 MeV/n ²⁰Ne ions in water and lucite, and 490 MeV/n ²⁴Mg ions in polyethylene, carbon and aluminum targets sandwiched with CR-39 plastic nuclear track detectors. An automated microscope system and a track-to-track matching algorithm were used to count and recognize the primary and secondary particles. The measured cross sections were then compared with published cross sections and predictions of different models. Two models and the three-dimensional Monte Carlo Particle Heavy Ion Transport Code System (PHITS) were used to calculate total charge-changing cross sections. Both models agreed within a few percent for the system ²⁴Mg + CH₂, however a deviation up to 20% was observed for the systems ²⁰Ne + H₂O and C₅H₈O₂, when using one of the models. For all the studied systems, PHITS systematically underestimated the total charge-changing cross section. It was also found that the partial fragmentation cross sections for ²⁴Mg + CH₂ measured in present and earlier works deviated up to 20% for Z = 6–11. Measured cross sections for the production of fragments (Z = 4–9) for ²⁰Ne + H₂O and C₅H₈O₂ were compared with predictions of three different semi-empirical models and JQMD which is used in the PHITS code. The calculated cross sections differed from the measured data by 10–90% depending on which fragment and charge was studied, and which model was used.     

Applicability of particle and heavy ion transport code PHITS to the shielding design of spacecrafts

Development of HZE particle transport codes is severely required for the shielding design of spacecrafts. One-dimensional deterministic codes are generally adopted in the shielding calculation because of their reasonable computational time, but three-dimensional Monte Carlo codes are also to be employed especially in the final step of the design with fully optimized geometries. We are therefore developing a general-purpose Monte Carlo code PHITS, which can deal with the transports of all kinds of hadrons and heavy ions with energies up to . For the purpose of examining the applicability of PHITS to the shielding design, neutron and charged particle spectra inside the Space Shuttle were calculated for an imaginary vessel whose shielding distribution is fitted to that of the real shuttle. Absorbed doses and dose equivalents were estimated from the spectra by applying fluence to dose conversion coefficients. The agreements between the calculated spectra or doses and the corresponding experimental data were generally satisfactory, especially for the neutron spectra, which have been barely reproduced by other studies. We therefore concluded that PHITS has a great possibility of playing an important role in the design study of spacecrafts.     

Cathodic stripping voltammetry of nickel: sonoelectrochemical exploitation of the Ni(III)/Ni(II) couple

The exploitation of the Ni(III)/Ni(II) transition as a means of quantifying the concentration of nickel within industrial samples was assessed. The methodology relies upon the reagentless electrodeposition of Ni onto a glassy carbon electrode and the subsequent oxidative conversion of the metallic layer to Ni(III). The analytical signal is derived from a cathodic stripping protocol in which the reduction of the Ni(III) layer to Ni(II) is monitored through the use of square wave voltammetry. The procedure was refined through the introduction of an ultrasonic source which served to both enhance the deposition of nickel and to remove the nickel hydroxide layer that results from the measurement process. A well-defined stripping peak was observed at +0.7 V (vs. AgAgCl) with the response found to be linear over the range 50 nM to 1 μM (based on a 30 s deposition time). Other metal ions such as Cu(II), Mn(II), Cr(III), Pb(II), Cd(II), Zn(II), Fe(III) and Co(II) did not interfere with the response when present in hundred fold excess. The viability of the technique was evaluated through the determination of nickel within a commercial copper nickel alloy and validated through an independent comparison with a standard ICP-AES protocol.     

PHITS—a particle and heavy ion transport code system

The paper presents a summary of the recent development of the multi-purpose Monte Carlo Particle and Heavy Ion Transport code System, PHITS. In particular, we discuss in detail the development of two new models, JAM and JQMD, for high energy particle interactions, incorporated in PHITS, and show comparisons between model calculations and experiments for the validations of these models. The paper presents three applications of the code including spallation neutron source, heavy ion therapy and space radiation. The results and examples shown indicate PHITS has great ability of carrying out the radiation transport analysis of almost all particles including heavy ions within a wide energy range.     

Production of a fluorescence probe in ion-beam radiolysis of aqueous coumarin-3-carboxylic acid solution—2: Effects of nuclear fragmentation and its simulation with PHITS

The G(OH) values in aqueous coumarin-3-carboxylic-acid (3-CCA) solutions irradiated with ¹²C⁶⁺ beams having the energies of 135, 290 and 400 MeV/u were measured by a fluorescent method around the Bragg peak, with 0.6 mm intervals, and quartz cells of 1 cm optical lengths, at the Heavy Ion Medical Accelerator in Chiba, National Institute of Radiological Sciences (NIRS). For each ion, the G(OH) has been calculated as a function of dose average LET and position. The calculated results have been compared to measurements, and the results, reproducibility and reliability of the calculations are discussed in the paper.     

Two fluoroalcohols as components of basic buffers for liquid chromatography electrospray ionization mass spectrometric determination of antibiotic residues

Two fluoroalcohols--1,1,1,3,3,3-hexafluoro-2-propanol (HFIP) and 1,1,1,3,3,3-hexafluoro-2-methyl-2-propanol (HFTB)--were evaluated for the first time as volatile buffer acids in the basic mobile phase for reversed-phase chromatography with electrospray ionization-mass spectrometric (LC-ESI-MS) detection of five antibiotics. Chromatographic separation as well as positive and negative ion ESI-MS intensities using these novel buffer components were compared to traditional buffer systems. Overall, the highest signal intensities and best chromatographic separation for the five antibiotics (ciprofloxacin, norfloxacin, ofloxacin, sulfadimethoxine and sulfamethoxazole) were achieved using 5 mM HFIP as the buffer acid to methanol : water mobile phase (pH of the aqueous component adjusted to 9.0 with ammonium hydroxide). Comparable results were achieved using 5 mM HFTB (pH adjusted to 9.0 with ammonium hydroxide). The suitability of HFIP for analysis of antibiotic residues in lettuce is demonstrated.