Determination of mitomycin C in plasma, serum and urine by high-performance liquid chromatography with ultra-violet and electrochemical detection

The performance of a number of normal phase and reversed-phase systems, with ultraviolet detection at 360 nm, has been investigated with respect to their applicability to pharmacokinetic studies of mitomycin C (MMC). The reversed-phase system developed was also combined with a polarographic detector in order to compare the sensitivity and selectivity of ultraviolet and electrochemical detection. A simple isolation procedure, based on the adsorption of MMC on a non-ionogenic resin, has been developed. The developed assay is applied to a pharmacokinetic study from which some examples are given.     

Arsenic compounds in a marine food chain

A three-organism food chain within a rock pool at Rosedale, NSW, Australia, was investigated with respect to arsenic compounds by high performance liquid chromatography – hydraulic high pressure nebulization – inductively coupled plasma mass spectrometry (HPLC-HHPN-ICP-MS). Total arsenic concentration was determined in the seaweed Hormosira banksii (27.2 μg/g dry mass), in the gastropod Austrocochlea constricta (74.4 μg/g dry mass), which consumes the seaweed, and in the gastropod Morula marginalba (233 μg/g dry mass), which eats Austrocochlea constricta. The major arsenic compounds in the seaweed were (2′R)-dimethyl[1-O-(2′,3′-dihydroxypropyl)-5-deoxy-β-d-ribofuranos-5-yl]arsine oxide and an unidentified compound. The herbivorous gastropod Austrocochlea constricta transformed most of the arsenic taken up with the seaweed to arsenobetaine. Traces of arsenite, arsenate, dimethylarsinic acid, arsenocholine, the tetramethylarsonium cation, and several unknown arsenic compounds were detected. Arsenobetaine accounted for 95% of the arsenic in the carnivorous gastropod Morula marginalba. In Morula marginalba the concentration of arsenocholine was higher, and the concentrations of the minor arsenic compounds lower than in the herbivorous gastropod Austrocochlea constricta.     

The temperature-dependent red-shift of the visible absorption spectra of crystal violet in alcohol solutions

The visible absorption spectrum of the triphenylmethane dye, crystal violet, in various alcohol solutions at several temperatures has been recorded and subsequently analyzed by computer fitting. The observed spectral changes do not sustain either the earlier temperature-dependent absorption results of Lewis and co-workers or the concept of two ground-state species in equilibrium.     

Modulation des flammenspektrometrischen Signals mittels intermittierender Probenzufuhr zur Flamme

Zusammenfassung An Stelle eines Choppers wird zur Modulation des flammenspektrometrischen Signals die Probenflüssigkeit periodisch der Flamme zugeführt (intermittierende Zerstäubung). Es wird zunächst über die beobachtete Eigenmodulation der Zerstäubung berichtet und danach über die intermittierende Zerstäubung mit Frequenzen bis zu 50 Hz. Anschließend wird an Hand von Beispielen gezeigt, daß sich die intermittierende Zerstäubung als besonders vorteilhaft in der Absorptions-Flammenspektrometrie erweist. Wird das Gleichlicht des Hintergrundstrahlers mittels der intermittierenden Zerstäubung in der Flamme moduliert und ein Wechselstromverstärker verwendet, so fallen der 0- und 100%-Durchlässigkeitspunkt zusammen. Bei der Registrierung über die Wellenlänge werden dann nur solche Linien angezeigt, welche in der Flamme das eingestrahlte Licht absorbieren.

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Summary For modulating the flame spectrometric signal without using a chopper the sample is introduced into the flame periodically (intermittent atomisation). First, the observed self-modulation of the atomisation is described and subsequently the intermittent atomisation with frequencies up to 50 cps. Some examples demonstrate that intermittent atomisation proves to be especially advantageous in absorption flame spectrometry. When modulating the light of the dc-operated line source by means of intermittent atomisation and using ac-amplification of the modulated signal the 0- and 100%-transmittance points of the transmittance scale are the same. When scanning over the wave length only such lines are detected which absorb the light of the background source.

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Der Fa. Siemens-Reiniger Werke AG., Erlangen, und insbesondere Herrn Ing. Engel danken wir auch an dieser Stelle für die leihweise Überlassung des Flüssigkeitsstrahloscillographen Cardirex 31 B. — Herrn K. RÜdiger danken wir für die wertvollen Hinweise und für die Durchführung der Werkstattarbeiten.     

Amperometric titration of boron with fructose

Aqueous solutions of boratei can be titrated amperometrically with standard fi uctose solutions This procedure may be used to determine the boron content of various types of samples after conversion of the boron to the borate form The methode is based upon the observation that the polarographic wave of fructose. in a o I M LiCl, 001 N'LiOH solution is deprcssed by the presence of borate ions Under the prescribed conditions the methode is sensitive to a few hundredths of a milligram of boron The few comnonly occurring intcrferenes can be conveniently removed prior to the titration     

E-olefin dipeptide isostere incorporation into a polypeptide backbone enables hydrogen bond perturbation: probing the requirements for Alzheimer's amyloidogenesis

Herein, we report a stereospecific E-olefin dipeptide isostere synthesis that can be used to make gram quantities of the Phe-Phe isostere desired for eliminating a specific backbone H-bond donor and acceptor in the Alzheimer's disease related Abeta peptide. The Phe19-Phe20 E-olefin analogue of Abeta(1-40) was prepared by solid-phase peptide synthesis and was subjected to amyloidogenesis conditions. This analogue can aggregate into spherical morphologies but does not progress on to form protofibrils or fibrils as is the case for the all-amide sequence, providing insight into the structural requirements for amyloidogenesis.     

Synthesis of diterpene glycosides

Summary Mono-, di-, and linear triglycosides of a diterpene alcohol, derived from abietic acid and glucose have been synthesized employing peracetylbromo--D-glucose (4) and maltose derivatives5 and8 as glycosyl donors. The triglycoside14 exhibits slight haemolytic activity.

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Synthese von Diterpenglycosiden

Zusammenfassung Es wird die Synthese von Mono-, Di-, und linearen Triglycosiden aus einem von Abietinsäure abgeleiteten Diterpenalkohol beschrieben. Als Glycosyldonoren wurden neben Peracetobrom--D-glucose (4) die Maltosederivate5 und8 verwendet. Das Triglycosid14 zeigt schwache hämolytische Aktivität.

     

An investigation of catalytic activity in mixed metal oxide nanophase materials

We present preliminary evidence for catalytic activity by unsupported mixed metal oxide nanocrystalline materials. The results of this study show that a nanophase form of Li-MgO has begun to exhibit catalytic activity by 300 °C. This is at least 200 degrees below the temperature at which conventional Li-MgO catalysts exhibit comparable activity. Furthermore, at higher temperatures, the same nanophase composition shows enhanced activities and somewhat improved hydrocarbon selectivities over conventional Li-MgO catalysts.     

Darstellung,Struktur und magnetisches Verhalten von Alkali-metallmanganchalkogeniden A6MnX4 mit A Na oder K und X S,Se oder Te

Inhaltsübersicht. Die Verbindungen Na₆MnS₄, Na₆MnSe₄, Na₆MnTe₄, K₆MnS₄, K₆MnSe₄ und K₆MnTe₄ wurden durch Umsetzungen von Alkalimetallcarbonaten mit Chalkogen und Mangan bzw. Mangancarbonat in einem mit Chalkogen beladenen Wasserstoffstrom erhalten. Röntgenstrukturuntersuchungen an Einkristallen ergaben, daß alle sechs Verbindungen isotyp kristallisieren (Na₆ZnO₄-Typ, Raumgruppe P6₃mc). Als charakteristische Baugruppen treten “isolierte” tetraedrische [MnX₄]-Einheiten auf. Die Temperaturabhängigkeiten der magnetischen Suszeptibilitäten führen zu einem Curie-WeissVerhalten. Erst bei tiefen Temperaturen treten offensichtlich antiferromagnetische Kopplungen auf. Dabei sind die Wechselwirkungen in den Tellurverbindungen stärker als in den Schwefelverbindungen und in den Kaliumverbindungen stärker als in den Natriumverbindungen ausgeprägt. Synthesis, Structure, and Magnetic Properties of Alkali Metal Manganese Chalcogenides A₆MnX₄ with A Na or K and X S, Se or Te The compounds Na₆MnS₄, Na₆MnSe₄, Na₆MnTe₄, K₆MnS₄, K₆MnSe₄ and K₆MnTe₄ were synthesized by the reaction of alkali metal carbonates with chalcogen and Mn or MnCO₃ in a stream of hydrogen charged with chalcogen. Structural investigations on single crystals show that all six compounds crystallize in isotypic atomic arrangements (Na₆ZnO₄-type, space group P6₃mc), which are characterized by isolated [MnX₄] tetrahedra. The magnetic susceptibilities show Curie-Weiss behaviour. At low temperatures there are obviously antiferromagnetic interactions increasing from the sulfides to the tellurides and from the sodium compounds to the potassium compounds.