Determination of zearalenone and ochratoxin A in soil

Mycotoxins are secondary metabolites, formed by the action of fungi on agricultural crops in the field or during storage. These metabolites are highly toxic to animals and humans and high levels have been measured in agricultural crops. In order to evaluate human risks due to ingestion of mycotoxin-contaminated food different methods have been developed for analysis of mycotoxins in cereals and maize. In this project the focus was on mycotoxins in agricultural soil and the fate of these toxins in the soil-water-plant system. Two different mycotoxins were selected in the study: zearalenone (ZON) produced by species of Fusariumor Aspergillusand ochratoxin A (OTA) produced by species of Penicillium. We developed a method for analysis of these toxins in soil. Soil samples were extracted with methanol-water (9:1) and purified by solid-phase extraction (SPE, C8-columns). The final extract was analysed using high-pressure liquid chromatography (HPLC) with fluorescence detection. A Phenyl Hexyl column was used to separate the toxins. The detection limits obtained were 0.1 and 1.0 microg kg(-1) dry weight (dw) for OTA and ZON, respectively. The developed method has been used for analysis of different soils in connection with growth chamber experiments. The soil types used in the growth chamber experiments were a sandy soil, a sandy clay soil, and a soil with high content of organic matter. The recovery was determined as 85.8 and 93.4% and the repeatability to 5.1 and 12.8% for OTA and ZON, respectively. The reproducibility obtained was 8.5 and 15.0% for soil samples, representing concentration levels from 0.2-30 microg kg(-1) dw (OTA) and from 1.0-100 microg kg(-1) dw (ZON).     

Synthesis, spectroscopic and thermal studies of the copper(II) aspartame chloride complex

Aspartame adduct of copper(II) chloride Cu(Asp)₂Cl₂·2H₂O (Asp=aspartame) is synthesized and characterized by elemental analysis, FT IR, UV/vis, ESR spectroscopies, TG, DTG, DTA measurements and molecular mechanics calculations. Aqueous solution of the green solid absorbs strongly at 774 and 367 nm. According to the FT IR spectra, the aspartame moiety coordinates to the copper(II) ion via its carboxylate ends, whereas the ammonium terminal groups give rise to hydrogen bonding network with the water, the chloride ions or neighboring carboxylate groups. The results suggest tetragonally distorted octahedral environment of the copper ions.     

Equilibrium and NMR Studies of Noncovalent Interactions in Binary Systems: Uridine,Adenosine, Cytidine and Thymidine,and Adenosine (or Cytidine) 5′-Monophosphate in Aqueous Solution

The molecular complex formation reactions of uridine (Urd) with adenosine (Ado), cytidine (Cyd), thymidine (Thd), adenosine 5-monophosphate (AMP) and cytidine 5-monophosphate (CMP) have been studied at 20°C. It was found that the main positive noncovalent centers of ion–dipole and dipole–dipole type interactions are the protonated N(3) atoms of Urd, whereas the negative centers are the endocyclic atoms of the bases characterized by high electron density from the second molecule involved in the reaction. Moreover, NMR results indicate the occurrence of stacking in the complex (Urd)H(Cyd), whereas in the complex, (Urd)H₂(Thd), it is the only type of interaction. Deprotonation of the latter species brings about a change in the character of the reaction and ion–dipole interactions have been detected in the adduct, (Urd)H(Thd). Interestingly, no involvement of the phosphate groups in the formation of AMP and CMP adducts has been evidenced and the main centers of the reactions were found to be the N(7)and N(1) atoms of AMP, or the N(3) atoms of CMP and Urd. Moreover, in the Urd/CMP system the NMR results suggest stacking-type interactions.     

Synthesis and nitration of 4,6(4,8)-dimethyl-4-methyl-6(8)-methoxy-1,2,3,4-tetrahydrospiro [quinoline-2-cyclohexanes]

The cydization of 1-allyl-1-arylaminocyclohexanes under conditions of acid catalysis afforded 1,2,3,4-tetrahydro-4-methylspiro [quinoline-2-cyclohexanes] methyl (methoxy)-substituted in the phenylene ring. Their mono- and dinitro derivatives were synthesized, and their structure was established. Propositions on the direction of the nitration reaction of these heterocyclic compounds were expressed.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 6, pp. 784–788, June, 1993.     

Pyrazolines — Derivatives of 2-nitrochalcone

By the reaction of 2-nitrochalcone with hydrazine hydrate, 5-(2-nitrophenyl)-3-phenyl-1H-2-pyrazoline (I) and the hydrazone of 3-(5-(2-nitrophenyl)-3-phenyl-2-pyrazolin-1-yl)-3-(2-nitrophenyl)propiophenol (II) have been prepared. The acylation of both compounds I and II leads to N-acyl derivatives of the first. The acylating ability of formamide and N,N-dimethylformamide was observed in reactions with pyrazoline I. An x-ray structural study was carried out on compound II.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 3, pp. 360–366, March, 1993.     

Voltammetric sizing of a sphere.

The size of a glass sphere positioned in the center of a microdisk electrode is determined by using a simple electrochemical procedure and is confirmed, additionally, by a microscopical measurement of the sphere at the time of the electrochemical measurement. The cyclic voltammetric response of the naked electrode and of the electrode with the sphere positioned in its center is recorded over a wide range of scan rates (0.002-1.5 V s(-1)). The size of the sphere is then determined by comparison of the experimental voltammogram with simulations for each individual scan rate.     

Selenomethionine contents of NIST wheat reference materials

Values of the total selenium and selenomethionine (Semet) content of four wheat-based reference materials have been obtained by gas chromatography-stable isotope dilution mass spectrometry methods. The total Se method is an established one, and the results obtained with it are consistent with previously-assigned values. The Semet method (previously reported by our laboratory) is based on reaction with CNBr. Our data indicate that the four wheat samples (wheat gluten, durum wheat, hard red spring wheat, and soft winter wheat), though having a 30-fold range in total Se content, all have about 45% of their total Se values in the form of selenomethionine. Investigation of the CNBr-based method suggests that additional experiments are needed to verify that all selenomethionine in the wheat samples is accounted for, but also indicates that the values obtained are within 15% of the true values. As the form in which Se occurs in foods and dietary supplements is important from a nutritional perspective, adding information about Se speciation to total Se values in appropriate reference materials makes these materials more valuable in relevant analytical work.     

Flocculation of a Synthetic Rubber Latex with Homopolymers and Copolymers of N-Vinylcaprolactam and N-Vinylimidazoles

Flocculation of a latex of SKS-30 ARK commercial rubber with homopolymers and copolymers of N-vinylcaprolactam, 1-vinyl-2-methylimidazole, and its quaternization product was studied. The flocculating power of the nonionic polymers in acid solution was evaluated. The performance of the copolymers grows with increasing content of cationic units in the macromolecules and on adding an acid.