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Journal of Flow Chemistry
Authors:
Giancarlo Pascali
,
Mariarosaria De Simone
,
Lidia Matesic
,
Ivan Greguric
, and
Piero A. Salvadori

Nucleophilic [18F]-fluorination reactions traditionally include a drying step of the labeling agent in order to achieve a successful substitution. This passage extends the time and complexity required for the whole radiotracer production, with increased hardware and detrimental effects on the radioactive recovery of such a short-lived (t ½=109 min) isotope. Because the performance of radiofluorination reactions conducted under microfluidic flow conditions have been demonstrated to be more effective in terms of reaction time and yields, we have tested the tolerance to water present in this specific reaction condition, in view of eliminating the drying step in the process. To this purpose, we tested different substrates selected from typical radiofluorination intermediates. Our results show that water could be tolerated in a microfluidic environment; in particular, we observed a slight decrease in the labeling of aromatic precursors and a significant increase for iodonium salts, whereas the radiochemical yields of the other compounds studied were virtually unchanged. These findings may open the way to the possibility of simpler and faster processes for the production of new 18F-fluorinated positron emission tomography tracers.

Open access

Two sensitive and selective chromatographic methods were developed for determination of finasteride and tamsulosin hydrochloride in bulk powder and a pharmaceutical formulation. The first method was based on high-performance liquid chromatography (HPLC) separation of the cited drugs in the presence of the acid degradation product of finasteride. The separation was achieved using a C18 column (300 mm × 3.9 mm; 10-μm particle size) and a mobile phase consisting of 0.04 M ortho-phosphoric acid (pH 3.5 ± 0.2 adjusted with triethylamine) and acetonitrile (50:50, v/v). Quantification was achieved with ultraviolet (UV) detection at 215 nm. Linearity was in the range of 10.00–110.00 μg/mL and 2.00–44.00 μg/mL for finasteride and tamsulosin hydrochloride, respectively. Thin-layer chromatography (TLC)–densitometric method was achieved on an aluminum plates pre-coated with silica gel 60 F254 using toluene–ethanol–diethylamine (8:2:1.5, by volume) as eluent, and the R F values of tamsulosin hydrochloride and finasteride were 0.57 and 0.64, respectively. Quantification was achieved with UV detection at 250 nm for finasteride and 280 nm for tamsulosin hydrochloride. Linearity was in the range of 1.00–40.00 and 0.2.00–20.00 μg per spot for finasteride and tamsulosin hydrochloride, respectively. The results obtained were validated according to the International Conference on Harmonisation (ICH) guidelines. A statistical comparison between the obtained results and the results of a reported method was carried out.

Open access

Abstract  

In the present work, results of γ-irradiation on normal and functionalized SBA-15 by aurintricarboxylic acid have been reported. Characterization of normal and functionalized SBA-15 particles before and after γ-irradiation was carried out using Fourier-transform infrared technique. Aurintricarboxylic acid ligand connected to SBA-15 was also analyzed using UV/Vis spectrophotometer. The modified sorbent was then used as a new sorbent for separation of trace amounts of praseodymium and lutetium ions from nuclear waste waters in batch techniques. Based on the results of distribution coefficients determination, and investigation of sorption process in various conditions, the parameters were optimized for separation lanthanides. It can be concluded that the functionalized SBA-15 is a promising sorbent for praseodymium and lutetium cations.

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A new and sensitive method, termed magnetic solid phase extraction combined with dispersive liquid–liquid microextracton (MSPE–DLLME), has been developed for the simultaneous determination of biphenyl and biphenyl oxide in water samples. Different parameters influencing the extraction efficiency, including the amount of sorbent, sorption time, type of elution solvent and its volume, type of extraction solvent and its volume, and elution time were optimized. The calibration curves were linear in the range of 0.5–100 μg/L for both of them. The limits of detection (LODs) were achieved, 0.03 μg/L for biphenyl and 0.07 μg/L for biphenyl oxide, respectively. Ultimately, the applicability of the method was successfully confirmed by the extraction and determination of biphenyl and biphenyl oxide in sea, river, tap, and water well.

Open access

Abstract  

Radiochemical results of U isotopes (234U, 235U and 238U) and their activity ratios are reported for well waters as local sources of drinking waters collected from the ten settlements around the Semipalatinsk Nuclear Test Site (SNTS), Kazakhstan. The results show that 238U varies widely from 3.6 to 356 mBq/L (0.3–28.7 μg/L), with a factor of about 100. The 238U concentrations in some water samples from Dolon, Tailan, Sarzhal and Karaul settlements are comparable to or higher than the World Health Organization’s restrictive proposed guideline of 15 μg (U)/L. The 234U/238U activity ratios in the measured water samples are higher than 1, and vary between 1.1 and 7.9, being mostly from 1.5 to 3. The measured 235U/238U activity ratios are around 0.046, indicating that U in these well waters is of natural origin. It is probable that the elevated concentration of 238U found in some settlements around the SNTS is not due to the close-in fallout from nuclear explosions at the SNTS, but rather to the intensive weathering of rocks including U there. The calculated effective doses to adults resulting from consumption of the investigated waters are in the range 1.0–18.7 μSv/y. Those doses are lower than WHO and IAEA reference value (100 μSv/y) for drinking water.

Open access

Abstract  

The development on neutron activation analysis (NAA) into a technique of practical interest effectively started about 60 years ago, when nuclear reactors became available and widely accessible as intense sources of neutrons. During 50 out these 60 years, the series of Modern Trends in Activation Analysis (MTAA) Conferences acted as a true companion and facilitator of this growth. As trendwatcher they signalized the many initiatives that contributed to the development of activation analysis and its applications. A period has come to an end of impressive development resulting from sometimes revolutionary changes in radiation detection and data processing, and much improved irradiation facilities, NAA has reached a full stage of development, with emphasis on routine application and with remaining developments of in marginal impact. NAA is being challenged increasingly in the last 30 years by alternative techniques for multi trace element analysis. The MTAA Conference and with it the ICAA, the International Committee on Activation Analysis, can play an important and active role in this process of identifying and selecting key areas, and even promoting concerted action in those areas. Such an evolution of focus from retrospective to prospective, from trendwatcher to trendsetter, may well allow the MTAA Conference to continue and even expand its role in future development of NAA and its applications. The ideas about the future of the MTAA Conferences and its organization are elaborated upon and some possible subjects for focused development activities are indicated.

Open access

Summary

A stability-indicating LC assay method was developed and validated for the quantitative determination of doripenem and biapenem in pharmaceutical dosage forms in the presence of degradation products formed during forced degradation studies. An isocratic RP-HPLC method was developed with a C-18 (250 mm × 4.6 mm, 5 μm) column and 12 mM ammonium acetate-acetonitrile (96:4 υ/υ) as mobile phase. The flow rate of the mobile phase was 1.0 mL min−1 for doripenem and biapenem. The determination was carried out at the wavelength of 295 nm. The carbapenems were subjected to stress conditions of degradation in aqueous solutions including hydrolysis, oxidation, photolysis, and thermal degradation. The developed method was validated with respect to linearity, accuracy, precision, selectivity, and robustness.

Open access

Summary

Two sensitive and selective chromatographic methods have been developed and validated for analysis of idrocilamide in the presence of its degradation products. Forced degradation studies were performed using HCl, NaOH, and 3% H2O2. The first method is based on thin-layer chromatographic separation of the intact drug from its degradation products, followed by densitometric measurement. The second method is based on isocratic reversed phase high-performance liquid chromatographic separation of the drug from its degradation products on a C18 column. The HPLC method was used to investigate the kinetics of alkaline degradation of the drug at different temperatures.

Open access

Mandela University (RSA) University of Cambridge (UK) Governmental and other research organizations University of Cardiff (UK

Open access

-resistant tuberculosis (MDR-TB) remains a huge health threat to TB treatment [ 2 – 3 ]. Also in 2017, the World Health Organization announced the number of Rifampicin-resistance new illnesses was 558,000, and of these, 82% belonged to MDR-TB. Thus, it is very important

Open access