Gas-liquid chromatographic-mass spectrometric determination of alpha- and beta-naphthylamines in FD&C Red No. 2 (amaranth)

A method is described for the simultaneous quantitation of trace amounts of alpha- (alpha-NA) and beta-naphthylamines (beta-NA) with detectability in the 0.1 ppb range and sensitivity of 50 picomoles in certified food grade amaranth (FD&C Red No. 2; C.I. Food Red 9; CI 16185). The amaranth sample is extracted with benzene, and the evoporated residue is derivatized with perfluorooctanoic anhydride. The resulting derivatives are separated by gas-liquid chromatography and identified and quantitated by mass spectrometric monitoring of the m/e at 539.04. The method was used for quantitation of alpha-NA and beta-NA in randomly chosen samples of amaranth. Of 11 samples from different manufacturers, 5 were free of the beta-isomer; the remaining samples contained up to 1.2 ppb beta-NA. The concentration of alpha-NA ranged from no detectable amount to 970 ppb; the majority of the samples contained less than 7 ppb.     

Gas chromatographic method for determination of fenitrothion in technical and in emulsifiable concentrate and water-dispersible powder formulations: collaborative study

A variety of column packings and internal standards were evaluated to determine the most satisfactory system to use in a gas chromatographic (GC) method for analysis of fenitrothion, technical and formulations. Fenitrothion and the most closely related isomer, O,O-dimethyl O-(4-methyl-3-nitrophenyl) phosphorothioate, were resolved on columns packed with OV-210 and with polyphenyl ether, 6-ring (PPE-6R). A method based on the separation of fenitrothion on a PPE-6R column with fluoranthene as internal standard was selected for use in a limited collaborative trial and later for use in a full-scale collaborative trial with 21 collaborators participating. Each collaborator was furnished matched pairs of samples of technical fenitrothion, emulsifiable concentrate, and water-dispersible powder. The coefficients of variation (CV) for the paired samples were 1.02, 1.11, and 1.01, respectively, for technical fenitrothion, emulsifiable concentrates, and water-dispersible powders. Data are also presented for an alternative method in which compounds are separated on an OV-210 column with dibutyl sebacate as the internal standard. The method has been adopted official first action.     

Coast live oak, Quercus agrifolia, susceptibility and response to goldspotted oak borer, Agrilus auroguttatus, injury in southern California

Oak mortality is often associated with a complex of decline factors. We describe the morphological and physiological responses of coast live oak, Quercus agrifolia Née, in California to an invasive insect, the goldspotted oak borer (GSOB), Agrilus auroguttatus Schaeffer (Coleoptera: Buprestidae), and evaluate drought as a potential inciting factor. Morphological traits of 356 trees were assessed and physiological traits of 70 of these were monitored intensively over one growing season. Morphological characteristics of tree health included crown thinning and dieback; bole staining resulting from larval feeding; density of GSOB adult exit holes; and holes caused by woodpecker feeding. These characteristics were used to rank GSOB infestation/injury into four classes, and taken together, they explained 87% of the variation in a principal component analysis. Drought stress on various size/age and infestation classes of Q. agrifolia was measured by assessing branchlet pre-dawn and solar noon xylem water potential, leaf cell turgor potential, and water use efficiency over one growing season. Both morphological and physiological traits were highly variable in mature and old growth trees. Early summer plant water status (branchlet xylem water potential and water use efficiency) was similar between uninfested and newly colonized trees, suggesting that GSOB are not pre-selecting drought-stressed Q. agrifolia for oviposition. By late summer, leaf water and cell turgor potentials were lower in infested than in uninfested mature trees, suggesting that GSOB infestation causes drought stress in these trees. Among the tree size/age classes, infested old growth trees exhibited the greatest change in water use efficiency over the growing season, and showed greater morphological injury symptoms of decline than infested mature trees. Morphological attributes of decline in Q. agrifolia associated with GSOB were correlated weakly with increasing physiological drought stress among infestation classes of trees. We propose that the collection of morphological responses of Q. agrifolia to GSOB described here can be used to monitor the future expansion of the GSOB distribution as well as the GSOB-induced decline of Q. agrifolia in California.     

Lipoprotein patterns in acrylamide gel electrophoresis

Lipoproteins of serum stained before electrophoresis gave distinct patterns in acrylamide gel of 3-percent concentration. Samples compared in parallel on gel slabs showed qualitative differences in migration rates of beta-lipoprotein bands.     

The relation between major histocompatibility complex (MHC) restriction and the capacity of Ia to bind immunogenic peptides

The capacity of purified I-Ad, I-Ed, I-Ak, and I-Ek to bind to protein derived peptides that have been previously reported to be T cell immunogens has been examined. For each of the 12 peptides studied strong binding to the relevant Ia restriction element was observed. All the peptides bound more than one Ia molecule; however, for 11 of 12 peptides, the dominant binding was to the restriction element, whereas in one instance the dominant binding was to a nonrestriction element. When the peptides were used to inhibit the presentation of antigen by prefixed accessory cells to T cells, an excellent correlation was found between the capacity of a peptide to inhibit the binding of an antigen to purified Ia and the capacity of the peptide to inhibit accessory cell presentation of the antigen. Thus, the binding of peptide to purified Ia is immunologically relevant, and Ia seems to be the only saturable molecule on the surface of the accessory cell involved in antigen presentation. Inhibition analysis also indicated that all peptides restricted to a particular Ia molecule competitively inhibited one another, suggesting that each Ia restriction element has a single binding site for antigen. Cross-linking of labeled peptides to Ia followed by electrophoretic analysis and autoradiography suggested that this single binding site is made up of portions of both alpha and beta chains of Ia.     

Scanning probe evolution in biology

Twenty years ago the first scanning probe instrument, the scanning tunneling microscope, opened up new realms for our perception of the world. Atoms that had been abstract entities were now real objects, clearly seen as distinguishable individuals at particular positions in space. A whole family of scanning probe instruments has been developed, extending our sense of touching to the scale of atoms and molecules. Such instruments are especially useful for imaging of biomolecular structures because they can produce topographic images with submolecular resolution in aqueous environments. Instruments with increased imaging rates, lower probe-specimen force interactions, and probe configurations not constrained to planar surfaces are being developed, with the goal of imaging processes at the single-molecule level-not only at surfaces but also within three-dimensional volumes-in real time.