Determination of iphosphamide and seven metabolites in blood plasma,as stable trifluoroacetyl derivatives,by electron capture chemical ionization GC-MS

A method is described for the determination of the antitumor agent iphosphamide and seven of its metabolites in the plasma of cancer patients by multiple ion monitoring (MIM) GC-MS, mainly using the electron capture chemical ionization mode, of stable methyl and/or trifluoroacetyl derivatives. The metabolites determined were 2- and 3-dechloroethyliphosphamide, 4-ketoiphosphamide, carboxyiphosphamide, iphosphamide mustard, and two previously undetected metabolites, chloroethylamine and 1,3-oxazolidine-2-one. The isolation of the acidic and neutral metabolites was performed by solid phase extraction on to C₁₈ adsorbent at pH 4. The weakly acidic iphosphamide mustard, isolated under these conditions with a yield of ca 50%, was measured as a stable methyltrifluoroacetyl derivative, in contrast to the corresponding phosphoramide mustard of the isomer cyclophosphamide which decomposes during derivatization. Chloroethylamine and 1,3-oxazolidine-2-one were isolated with high yield by liquid extraction with ethyl acetate at pH 10. Selective measurement of several metabolite derivatives with similar retention times was performed by multiple ion monitoring MS of specific ion masses, using a methyl phenyl siloxane capillary column previously employed in the study of cyclophosphamide metabolites. Quantitation of metabolites in patient plasma samples could be performed in the concentration range 3 ng to 20 μg per ml of original plasma.     

A contribution to the ternary phase diagram Co-Sb-Te

The melting behaviour, some phase boundaries and the lattice parameters in the region of the NiAs-type phase in the ternary system cobalt-antimony-tellurium have been determined by differential thermal analysis and X-ray diffraction. A projection of the liquidus surface and the phase relationships in different sections with constant antimony/tellurium ratios are presented. The peculiar variation of the lattice parameters with the composition of the nonstoichiometric NiAs-type phase is discussed in terms of the defect structure.Dedicated to Prof. K. L. Komarek on the occasion of his 65th birthday     

Multiplicities of interpoint distances in finite planar sets

What is the maximum number of unit distances between the vertices of a convex n-gon in the plane? We review known partial results for this and other open questions on multiple occurrences of the same interpoint distance in finite planar subsets. Some new results are proved for small n. Challenging conjectures, both old and new, are highlighted.