Rapid Fluorometric Screening of Antibiotics in Seafood

Simple and rapid fluorometric screening methods have been developed based on the competitive binding between the target and an intercalating fluorophore dye to double-stranded-DNA (dsDNA). In this study, the long-wavelength fluorescente dye TOTO-3 was employed as the indicator. Compounds that interact with dsDNA will affect the binding of TOTO-3 to the nucleic acid thereby changing the fluorescence intensity. The analyte concentration is indirectly determined by the decrease in fluorescence intensity. A fiber optic fluorescence screening system was developed for rapid and convenient sample processing. Lambda DNA (48.5 kb) was chosen as a suitable sensing nucleic acid material. Detection of sulfathiazole and chloramphenicol in shrimps using this method was studied in the range of 0.5–25 ng mL⁻¹ of sulfathiazole and of 1–50 ng mL⁻¹ of chloramphenicol. Detection limits of 0.5 ng mL⁻¹ of sulfathiazole and 1 ng mL⁻¹ of chloramphenicol were achieved. This approach is useful as a routine test in the monitoring of antibiotics in the environment or aquaculture products. The easy operation and the rapid and sensitive detection make this a potential high-throughput screening method.     

(11)C] Carbon monoxide in selenium-mediated synthesis of (11)C-carbamoyl compounds

Using either amines, amino alcohols, or alcohols in selenium-mediated synthesis with [(11)C]carbon monoxide, 3 ureas, 6 carbamates, and 1 carbonate were labeled. Tetrabutylammonium fluoride ((TBA)F) was discovered to form a soluble and reactive complex with selenium and drastically increase the radiochemical yields. Of the selected carbamoyl compounds, one was a receptor ligand, one was an enzyme inhibitor, and one was a muscular relaxant pharmaceutical. The (11)C-target compounds were obtained in radiochemical yields ranging from low to almost quantitative and with specific radioactivity up to 1300 GBq/micromol. The radiochemical purity of the final products exceeded 98%. In one case, the corresponding (13)C-substituted compound was produced to verify the position of the (11)C-label. In a typical experiment starting with 16.4 GBq [(11)C]carbon monoxide, 7.0 GBq of LC-purified 5-phenyl-1,3-oxazolidin-[2-(11)C]-2-one was obtained within 20 min from start of the carbonylation reaction (84% decay-corrected radiochemical yield). The presented approach is an interesting alternative to the use of [(11)C]phosgene in labeling chemistry.     

Photo-degradation and photo-stabilisation of the two-phase system poly(vinyl chloride)-polybutadiene

The photo-oxidative degradation of poly(vinyl chloride) (PVC)/polybutadiene (PB) blends has been studied. After uv irradiation, photo-grafting of the PVC and PB phases was observed. Photolysis of PVC accelerates cis-trans isomerisation of PB. Both phases, PVC and PB, are photo-degraded according to free radical oxidation mechanisms. The rates of these processes can be decreased by the addition of metal chelates, such as commercially produced Cyasorb uv light absorber 1084 (2,2′-thiobis(4-t-octylphenolato)-n-butylamine nickel(II)) and Cyasorb uv light absorber 2548 (cobalt dicyclohexyldithiophosphinate).     

Melt-photografting polymerization of maleic anhydride onto LDPE film

Maleic anhydride (MAH) was photografted onto low density polyethylene substrates at temperatures above the melting point of MAH. The effects of some principal factors including irradiation temperature, photoinitiators, the intensity of UV radiation, and the far UV radiation on the grafting polymerization were investigated in detail. Percent conversion and grafting efficiency of the polymerizations were determined by the gravimetric method. The contact angles of the grafted film PE-g-PMAH against water and the FTIR spectrum of the grafted film were measured as characterization. The results show that the photografting polymerization of MAH can proceed smoothly at temperatures higher than the melting point of MAH; the far UV radiation and the intensity of the UV radiation affect the grafting polymerization greatly; the photoinitiators also have influence on the polymerization. According to the FTIR spectra, it is clearly confirmed that the grafted film samples contain anhydride groups. The contact angles demonstrate that the wettability of the grafted films is enhanced obviously, especially to those grafted film samples through hydrolysis.     

Radical-mediated carboxylation of alkyl iodides with [11C]carbon monoxide in solvent mixtures

[reaction: see text] [carboxyl-(11)C]Carboxylic acids were prepared from alkyl iodides via photoinitiated radical reactions using 10(-)(8) mol of [(11)C]carbon monoxide in binary and ternary homogeneous solvent mixtures. Short- (isobutyric), medium-, and long-chain saturated fatty acids (heptadecanoic) were labeled with isolated decay-corrected radiochemical yields ranging from 55% to 70% in 5-7-min reactions. The conversion of [(11)C]carbon monoxide to products reached 80-90%. To obtain good yields in the reactions performed in water-acetonitrile and water-THF mixtures, the addition of tetrabutylammonium hydroxide or potassium hydroxide was essential. The carboxylation was efficient for primary and secondary alkyl iodides. The carboxylation of tertiary iodides was feasible for 1-iodoadamantane but not for tert-butyl iodide. The dependence of the radiochemical yields on reaction time, photoirradiation conditions, and organic and inorganic additives was studied. The method provides a one-step route to [carboxyl-(11)C]carboxylic acids; traditional methods, in contrast, would require several steps. For example, using the devised reaction conditions, 3.19 GBq of purified [1-(11)C]1,10-decanedicarboxylic acid (specific radioactivity 188 GBq/mumol) was obtained within 35 min of the end of 10 muAh bombardment. (1-(13)C)4-Phenylbutyric acid was synthesized using ((13)C)carbon monoxide for identifying the labeling position with (1)H and (13)C NMR.     

Mass spectrometric investigation of isomeric 1,2,3,4-tetrahydro-4-oxoquinazolines

Six isomeric methylphenyl-1,2,3,4-tetrahydro-4-oxoquinazolines have been prepared and their fragmentation patterns upon electron impact studied. Deuterium labelling and high-resolution measurements were performed in order to facilitate the interpretation of the spectra. The dissociation of the molecular ion follows two main routes, the fragmentation being governed by the position of the phenyl group.     

Effect of salt on the performance of immobilized pH gradient isoelectric focusing gels

The effect of salt and buffer ions in the sample or in an immobilized pH gradient (IPG) on sample entry into the gel and on the final focused pattern are presented. During the initial phase of electrofocusing, ions present in the gel, either as counter ions to the immobilized charge groups of the IPG gel or added to the gel matrix during the rehydration process, are transported toward the electrodes. For ions present at a concentration exceeding approximately 1 mM the transport can be followed by the refractile line marking the trailing edge of an ion-containing zone. Gradual sample entry may be achieved by applying the sample at a site (near the anode or cathode) opposite to that from which the sharpest refractile line, marking the ion present in the highest concentration, approaches the sample. Additionally, lateral band spreading of the sample is avoided. Thus, sample applied at the cathode for IPG gels rehydrated with 1-2 mM Tris base, or at the anode for gels rehydrated with 1-2 mM acetic acid or sodium acetate, enters the gel matrix gradually without lateral band spreading. In contrast, sample applied at the anode, for Tris-containing gels, or at the cathode, for acetate-containing gels, enters rapidly in a sharp zone when the refractile line reaches the sample zone. This results in a high local protein concentration in the zone immediately behind the boundary with lateral band spreading.(ABSTRACT TRUNCATED AT 250 WORDS)     

N,N,N′,N′-tetramethylethylene diamine as a co-catalyst in the anionic polylymerization of methyl methacrylate

Anionic polymerization of methyl methacrylate in toluene solution has been studied. The polymerizations were initiated by fluorenyllithium as well as by butyl-, benzyl-, and phenylmagnesium halides, and carried out in the presence of polar additives. Especially the organomagnesium initiators gave generally rise to highly isotactic polymers (mm = 0.90-0.95) in the absence of solvating additives. In the presence of the bidentate ligand N,N,N′,N′-tetramethylethylene diamine (TMEDA) at molar ratios of 1–2 relative to magnesium, highly syndiotactic polymers were obtained at ?78°C (rr = 0.8–0.9), while at higher temperatures stereoblock polymers or stereocomplexes were formed. It is proposed that at low temperatures the magnesium cations are strongly solvated under the influence of TMEDA, with the formation of monomeric ion pairs. The large solvated magnesium cations will not have any directional influence on the monomer in the propagation step, with syndiotactic propagation as a result.