Synthesis and properties of esters and amido esters of 1-(2-thienyl)-2,2,2-trichloroethylphosphorous acid

Conclusions The esterification of amido- and ester-amidophosphites with 1-(2-thienyl)-2,2,2-trichloroethanol gave the l-(2-thienyl)-2,2,2-trichloroethyl dialkyl- and 1-(2-thienyl)-2,2,2-trichloroethyl alkylamidophosphites, which easily add sulfur or are oxidized to the corresponding thiophosphates and phosphates.Translated from Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, No. 1, pp. 182–187, January, 1981.     

Separation and detection of oxidation products of fluorodeoxyglucose and glucose by high-performance liquid chromatography-electrospray ionisation mass spectrometry

2-Deoxy-2-[18F]fluoro-D-glucose ([18F] FDG), the most popular positron emitting radiopharmaceutical, may oxidise by autoradiolysis in aqueous solution. The aim of this work was to use LC-MS for determination of the oxidation products of fluorodeoxyglucose and glucose (Glc) obtained by oxidation with Fenton's reagent. Asahipak NH2P-50 polyamide silica column and acetonitrile-0.025% aqueous ammonium formate (80:20 (v/v)) eluent were utilised with an Agilent 1100 HPLC-MS instrument. Ten major oxidation products of FDG and Glc were separated and identified by mass spectrometry: 2-fluorogluconic acid, 2-fluoroglucuronic acid, 2-oxoerythronic acid, arabinose, arabonic acid, araburonic acid, erythrose, erythrulose, gluconic acid, and glucuronic acid. The most intensive electrospray ionisation signals were found in the negative ion spectra and were due to HCOO- adducts, the other acids being in their lactone forms.     

Determination of four nitroimidazole residues in poultry meat by liquid chromatography-mass spectrometry

A multi-residue liquid chromatography-mass spectrometry (LC-MS) assay method is described for the determination of four nitroimidazoles in poultry muscle. The extraction procedure is based on liquid-liquid extraction with ethyl acetate followed by an evaporation step. A deuterated internal standard is used. The LC separation was made on a C18 bonded silica column with an aqueous formic acid (0.2%) solution-methanol-acetonitrile (81:13:6) mobile phase. Following electrospray ionization, the protonated molecular ion [M+H]+ is obtained for each compound. Monitoring several ions for each nitroimidazole provides the specificity required for confirmatory assay. Validation of the method was performed to estimate linearity, intra-day and inter-day repeatability, accuracy and detection limit. The present method is capable of identifying nitroimidazole residues in muscle at levels below 5 microg/kg.     

Ring closure of some O-aryl ethers of ketoximes to benzofurans

The action of alcohol solutions of hydrogen chloride on aryl ethers of the oximes of N-substituted 4-piperidones (Ia-c) yielded rearrangement products — 3-(2-hydroxyaryl)-4-piperidones (IIa, b) and (or) 4a-aikoxy-l,2,3,4,4a,9b-hexahydrobenzofuro[3,2-c]pyridines (IIIa-c), which, under certain conditions, are readily converted to 1,2,3,4-tetrahydrobenzofuro[3,2-c]pyridines (IVa, b). Ketones of the II type are ketalized to dihydrobenzofurans III by alcohol solutions of hydrogen chloride.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 12, pp. 1596–1600, December, 1971.     

Austausch von Chrom(III) mit Chrom(II) und Szilard—Chalmers-Reaktion von Kaliumchromat

Zusammenfassung Durch Versuche mit⁵¹Cr wird gezeigt, daß Cr³⁺ mit Cr²⁺ austauscht, wenn man ein Chrom(III)-Salz in wässeriger Cr²⁺-Lösung auflöst, d. h. die Hydratation zum reaktionsträgen [Cr(H₂O)₆]³⁺ verläuft relativ langsam. Die Bedeutung dieses Austausches für dieSzilard—Chalmers-Reaktion von Chromat wird diskutiert.

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Experiments with⁵¹Cr prove the exchange of Cr³⁺ with Cr²⁺ when a Cr(III)-salt is dissolved in an aqueous solution of Cr²⁺. This indicates that the hydration to the inert [Cr(H₂O)₆]³⁺ is relatively slow. The importance of this exchange for theSzilard—Chalmers reaction of chromate is discussed.

     

Platinum(II) Mono-N1-(2"-Tetrahydrofuranyl)-5-Fluorouracilate Complexes with Ammonia

The reaction between cis-[Pt(NH₃)₂Cl₂], N¹-(2"-tetrahydrofuranyl)-5-fluorouracil (HL), and NaOH (taken in a molar ratio of 1 : 1 : 1) or between cis-[Pt(NH₃)₂Cl₂], HL, and Ag₂O (taken in the molar ratio of 1 : 1 : 0.5) was used to synthesize complexes Ia (in the case of NaOH) or Ib (in the case of Ag₂O) with composition Pt(NH₃)₂LCl. The model complex [Pt(NH₃)₃L]NO₃ (II) was synthesized by the reaction between [Pt(NH₃)₃Cl]Cl, HL, AgNO₃, and Ag₂O (1 : 1 : 1 : 0.5). The obtained compounds were characterized by chemical analysis, chromatography, thermogravimetry, conductometry, potentiometry, IR, electronic, and NMR spectroscopies. Complexes Ia and Ib were found to have both similar and different properties. The structures of the compounds and the type of L^– coordination to platinum(II) were suggested. Cytotoxic properties of Iaand Ib were studied.     

Catalytic Titrations of Silver(I) Using an Iodide-Catalyzed Mn(IV)-As(III) Indicator Reaction in the Presence of Sulfuric Acid with Detecting the End-Point by Methods with Two Polarized Electrodes

Catalytic bipotentiometric and biamperometric methods for determining silver(I) with the use of the new manganese(IV)-arsenic(III) indicator reaction catalyzed by iodide ions in the presence of sulfuric acid have been developed. The effects of the sulfuric acid concentration of some ionic species, of the mole ratio of manganese(IV) to arsenic(III) in the solution titrated, and of the titrand temperature, as well as of the current and potential difference, respectively, used for polarization of the indicator electrodes on the conditions for determinations of silver(I) of various concentrations were investigated. The error in the determination of 1.0 g/cm³ silver(I) do not exceed 2%, and the precision of the results is high for both methods.     

Cellular adhesion and proliferation on poly(3,4-ethylenedioxythiophene): Benefits in the electroactivity of the conducting polymer

Cell adhesion and proliferation in poly(3,4-ethylenedioxythiophene), an electroactive polythiophene derivative generated by anodic polymerization, has been investigated. Results show that epithelial cells Hep-2 present significant activity on the surface of poly(3,4-ethylenedioxythiophene) electrodeposited on stainless steel electrodes, no sign of cytotoxicity being detected for this conducting polymer. Indeed, seeded and cultured cells bound better to poly(3,4-ethylenedioxythiophene) than to uncoated stainless steel, the latter substrate being used as a control. Furthermore, the electrochemical characteristics of poly(3,4-ethylenedioxythiophene) covered with cells was determined in different biological media using cyclic voltammetry experiments. Results reveal a significant increase in the electroactivity of this material when it is covered with a cellular monolayer. The overall of the results evidences not only the biocompatibility of poly(3,4-ethylenedioxythiophene) with Hep-2 cells but also their electrocompatibility.     

k0-measurements and related nuclear data compilation for (n, γ) reactor neutron activation analysis

Recommended k₀-factors and related nuclear data for use in (n, γ) activation analysis are given for 72 isotopes. In addition the basic nuclear constants and experimental parameters needed in the k₀ standardization method are reviewed. For convenient data reduction, computer programs were developed.