Flow-injection determination of nonylphenol in liquid media using a piezoelectric immunosensor

A piezoelectric flow immunosensor for the rapid determination of nonylphenol in aqueous solutions was developed. An aminophenol-protein conjugate (4-AP-GA-BSA) immobilized on the presilanized surface of a silver electrode was used as a bioreceptor coating of the sensor. The effects of the nature and concentration of monoclonal and polyclonal antibodies on the analytical signal of the sensors were studied; the activity of immunoreagents was evaluated based on the binding constants K _b. The cross reactions of various phenols with antibodies were studied and the cross reaction percentages were found. A procedure for the flow-injection determination of nonylphenol in liquid media was developed using a piezoelectric immunosensor as a detector. The calibration graph was linear over the concentration range 1–20 ng/mL; the detection limit for nonylphenol was 0.8 ng/mL.     

Neurotrope und psychotrope Substanzen, 5. Mitt.: Synthese neuer Aminoderivate von 10,11-Dihydrodibenzo-[a,d]cyclohepten und 10,11-Dihydrodibenzo[b,f]thiepin

Zusammenfassung Im Rahmen der Suche nach neuen neurotropen und psychotropen Substanzen, besonders nach antidepressiv wirkenden Psychopharmaka, wurde eine systematische präparative Arbeit in den Gruppen der 10-substituierten Derivate des 10,11-Dihydrodibenzo[a,d]cycloheptens (I) und des 10,11-Dihydrodibenzo[b,f]-thiepins (II) unternommen. Im ersten Fall war die Ausgangssubstanz das Keton XIV, das mit üblichen Methoden zum basischen Äther XVI, zu Aminen und Derivaten XVIII–XXII und schließlich in dieMannich-Base XXVI übergeführt wurde. DieBeckmannsche Umlagerung des Oxims XVII eröffnete den Weg zu Derivaten eines neuen Systems, des 5,6,7,12-Tetrahydrodibenz[b,e]azocins (Verbindungen XXVIII, XXX und XXXI). Auch im zweiten Fall bildete das entsprechende Keton (XXXVIII) die Schlüsselsubstanz, die einerseits zu Aminen mit der Aminogruppe in der Seitenkette (XXXIX, XL, XLII, LV, LVI), anderseits zu Aminen mit der direkt am Skelett haftenden Aminogruppe (XLIV–LIII) umgesetzt wurde. Außer den angeführten Aminen wurde in allen drei Gruppen eine Reihe von neutralen Verbindungen hergestellt (Zwischenprodukte und Nebenprodukte), deren Struktur meistens mit Hilfe der Spektren geklärt wurde. Die vorläufigen Ergebnisse der pharmakologischen Prüfung einiger Produkte deuten interessante Wirksamkeit an, besonders vom Standpunkt der erwarteten neurotropen und psychotropen Eigenschaften aus.

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In the effort to find new neurotropic and psychotropic substances a systematic chemical study was undertaken in the groups of the 10-substituted derivatives of 10,11-dihydrodibenzo[a,d]-cycloheptene (I) and 10,11-dihydrodibenzo[b,f]thiepine (II). In the first case the ketone XIV was transformed by usual methods into the basic ether XVI, to the amines and derivatives XVIII–XXII, and to theMannich base XXVI. TheBeckmann rearrangement of the oxime XVII opened the way to derivatives of a new system — 5,6,7,12-tetrahydrodibenz[b,e]azocine (compounds XXVIII, XXX and XXXI). In the second case (derivatives of II) the syntheses started from the ketone XXXVIII and two series of amines were prepared: with the amino group in the side chain (XXXIX, XL, XLII, LV, LVI) and with the amino group attached directly to the skeleton (XLIV–LIII). In addition to the amines several neutral compounds in either group were synthesized (intermediates and byproducts), the structure of which was elucidated mainly by means of the spectra. Preliminary results of the pharmacological testing show a rather important degree of activity of some substances, especially in the line of the expected neurotropic and psychotropic properties.

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mit technischer Hilfe von

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Herrn Professor Dr.Hermann Bretschneider zum 60. Geburtstag gewidmet

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4. Mitt.:J. O. Jílek, K. Pelz, D. Pavlíková undM. Protiva, Coll. Czechoslov. Chem. Commun.30, im Druck (1965).     

Determination of the elemental composition of cyanobacteria cells and cell fractions by atomic emission and atomic absorption spectrometry

An approach to studying the elemental composition of cyanobacteria Spirulina platensis and Nostoc commune using a set of complementary analytical methods (ICP-AES, PAAS, and ETAAS) is proposed. The procedures were adapted for the determination of macro- and microelements (Na, K, Mg, Ca, Fe, Mn, Cu, Mo, Zn, B, and Se) in the biomass of cyanobacteria and separated cell fractions (chloroform and water-methanol extracts and precipitates). The conditions for the mineralization of biological materials were optimized for autoclave and microwave sample preparation procedures. The evaporation and atomization of Se and Mo in a graphite furnace in the presence of chloroform and methanol were studied. The use of combined analytical methods and the interpretation of analytical results allow one to draw conclusions about the ability of cyanobacteria to accumulate biologically important microelements (B, Mo, Se, and Zn) and to optimize technological processes for manufacturing biologically active substances.Translated from Zhurnal Analiticheskoi Khimii, Vol. 60, No. 1, 2005, pp. 35–40.Original Russian Text Copyright © 2005 by Sedykh, Lyabusheva, Tambiev, Bannykh.     

The rotational mobility of fulleropyrrolineoxyl in toluene solution

The rotational mobility of a stable fullerene-based nitroxyl radical (fulleropyrrolineoxyl) in toluene was studied. The rotational correlation time of fulleropyrrolineoxyl was found to be about eight times longer than that of 4-oxy-2,2,6,6-tetramethylpiperidine-1-oxyl. The activation energy of the rotational motion of both probes was determined and their hydrodynamic radii estimated.     

Zur Auswertung von im Übermikroskop aufgenommenen Elektronenbeugungsdiagrammen

Zusammenfassung Es wird ein Überblick über Fehlermöglichkeiten bei der Beugungsanalyse pulverförmiger Präparate im Übermikroskop gegeben. Die Netzebenenabstände können bei Anwendung eines geeigneten Simultanbeugungsverfahrens relativ rasch und sicher auf ±1 genau bestimmt werden. Einfache Beugungsaufnahmen hingegen lassen kaum eine exakte Auswertung zu. Die relativen Intensitäten der einzelnen Interferenzen können im allgemeinen zur Identifizierung nur bedingt verwendet werden. Die geringe Eindringtiefe der Elektronenstrahlen im Vergleich zur Teilchengröße bzw. Massendicke der gegebenen Präparate bringt eine Beschränkung des Verfahrens in der praktischen Anwendung mit sich. Bei der Ausdeutung der Diagramme treten unter Umständen Schwierigkeiten auf, die bei nicht genügend kritischer Behandlung zu Fehlschlüssen führen können. Werden die Grenzen des Verfahrens im Auge behalten, so stellt die dauernde Heranziehung der Beugungsanalyse, die bei den modernen Geräten ohne jeden zusätzlichen Aufwand in rascher Folge möglich ist, bei übermikroskopischen Untersuchungen an anorganischen Objekten ein recht nützliches Hilfsmittel dar.Mit 2 Abbildungen     

Laser Doppler methods in electrophoresis

Electrophoretic motion of particles, molecules, and biological cells can be readily measured by laser Doppler techniques. Small frequency shifts associated with the motion of the scatterers are detected by heterodyne detection of the scattered laser light. The principles of laser light scattering and heterodyne detection are reviewed. The central experimental problems associated with the application of electric fields to conducting solutions are considered in detail. Various types of laser Doppler spectrometers and electrophoresis chambers are compared both from fundamental physical points of view as well as in terms of resolving power of standard marker cells. As applications of the laser Doppler technique, measurements on proteins, virtues, nucleic acids, bioparticles and biological cells are reviewed.     

Anodic synthesis and molecular structure of dodecaethylhexaamidobisphosphonium diperchlorate

The electrochemical oxidation of hexaethyl triamidophosphite in the absence of nucleophiles specially introduced into the electrolyte was studied by anodic voltamperometry and preparative electrolysis. The reversible one-electron oxidation of the triamidophosphite molecule gives an unstable radical-cation, which reacts with a molecule of the starting compound to give a dimeric radical-cation, whose subsequent oxidation leads to dodecaethylhexaamidobisphosphonium diperchlorate. This product is the first example of an acyclic, doubly charged bisphosphonium cation with a . The crystal structure of this compound was obtained by x-ray diffraction structure analysis.Translated from Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, No. 3, pp. 664–669, March, 1990.     

The stereochemistry of the hydroboration rearrangement.

Hydroboration of 1,2-dimethylcyclopentene with BH₃·THF affords a product in which boron migrates $\text{stereospecifically}$ at low temperature into the cyclopentane ring. At higher temperatures subsequent (non-stereospecific) isomerisation occurs via a competing reaction mechanism.     

Determination of total sulphur in coal by x-ray fluorescence spectrometry

A precise x-ray fluorescence method for the determination of sulphur in coat. The sample is mixed with calcium oxide and active carbon and is gradually heated to 900°C. After coding, lithium tetraborate and lead oxide are added and a prepared. The Pb M_α line is used as an internal standard for the KK_α line. The results for coal have a relative standard deviation of approximately 1% and exhibit.     

Kristallographische Daten einiger Vanadin-Bromapatite

Zusammenfassung An Hand der Pulverdiagramme wurden die Gitterkonstanten von Ca₅(VO₄)₃Br, Sr₅(VO₄)₃Br und Ba₅(VO₄)₃Br ermittelt. Alle drei Verbindungen kristallisieren hexagonal und besitzen die Apatitstruktur. Mit den erhaltenen Daten werden einige kristallchemische Betrachtungen sowie Vergleiche mit anderen verwandten Verbindungen gemacht.

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Crystallographic data of some vanadium bromoapatites

The unit cell parameters of Ca₅(VO₄)₃Br, Sr₅(VO₄)₃Br and Ba₅(VO₄)₃Br, calculated by means of powder diagramms, are given. The compounds belong to the hexagonal system and crystallize with the apatite structure. With the obtained data, some comparisons are made and some aspects of the crystal chemistry of these and related compounds are discussed.

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7. Mitt. der Reihe Orthovanadate und verwandte Verbindungen; 6. Mitt.:E. J. Baran undP. J. Aymonino, Z. anorg. allgem. Chem.390, 77 (1972).