Synthesis of new gramine-type analogs of CC-1065

Preparation of two new analogs 5 and 6 of the antitumor antibiotic CC-1065 1 are described. These compounds represent structural modifications of the active analogs 3 and 2 respectively, in which the dienone A-unit has been replaced by the tricyclic achiral gramine unit 4 . Modest cytotoxicity was exhibited by compounds 5 and 6 .     

Investigation of a flat sheet membrane desolvator for aqueous solvent removal with inductively coupled plasma atomic emission spectrometry

Results obtained from a preliminary investigation of the performance of a flat sheet membrane desolvator (FSMD) utilizing dual hydrophobic polypropylene membranes with an average pore size of 0.05 mum and a 50 +/- 5 mum thickness are reported. The membranes have a desolvation area of 241 cm(2). The volume-to-surface area ratio is 0.3 cm. Using the FSMD with an ultrasonic nebulizer (USN), aqueous solvent desolvation efficiencies of greater than 99.9% were obtained at all nebulizer gas flow rates investigated (0.8, 1.2, and 1.8 l min(-1)). This efficient desolvation occurred when the countercurrent gas flow rate was equal to or slightly greater than the applied nebulizer gas flow rate. Under these conditions preconcentration factors of 18, 44, and 590 were observed with flows of 0.8, 1.2 and 1.8 l min(-1), respectively. Operating with countercurrent gas flow rates much higher than the nebulizer gas flow rates leads to a significant reduction in analyte flux, thus increasing detection limits. Depending on the nebulizer and countercurrent gas flow rate conditions, the FSMD contributed between 10-40% to the overall analyte loss in the system. The lowest detection limit observed for aqueous copper with the USN-FSMD system is 0.4 ppb at nebulizer and countercurrent gas flow rates of 1.2 and 1.4 l min(-1), respectively. At this nebulizer gas flow rate, replacing the FSMD in the system with a commercial tubular membrane desolvator, MDX100, gave a lowest Cu detection limit of 0.2 ppb at a countercurrent gas flow rate of 1.2 l min(-1). These detection limits represents improvements over the 0.7 and 8 ppb obtained with USN and pneumatic nebulization, respectively.     

Determination of metals in composite diet samples by inductively coupled plasma-mass spectrometry

A study was conducted to evaluate the applicability of inductively coupled plasma-mass spectrometry (ICP-MS) techniques for determination of metals in composite diets. Aluminum, cadmium, chromium, copper, lead, manganese, nickel, vanadium, and zinc were determined by this method. Atmospheric pressure microwave digestion was used to solubilize analytes in homogenized composite diet samples, and this procedure was followed by ICP-MS analysis. Recovery of certified elements from standard reference materials ranged from 92 to 119% with relative standard deviations (RSDs) of 0.4-1.9%. Recovery of elements from fortified composite diet samples ranged from 75 to 129% with RSDs of 0-11.3%. Limits of detection ranged from 1 to 1700 ng/g; high values were due to significant amounts of certain elements naturally present in composite diets. Results of this study demonstrate that low-resolution quadrupole-based ICP-MS provides precise and accurate measurements of the elements tested in composite diet samples.     

Membrane desolvation for the analysis of organic solutions and liquid chromatographic samples with low power helium microwave induced plasma atomic emission detection

A flat sheet membrane desolvator (FSMD) was used to extend the applicability of a 120 W helium microwave induced plasma (He-MIP) to elemental analysis of organic-solvent-based samples and element selective liquid chromatographic detection. With the FSMD on-line, methanol could be nebulized with a sample flow rate of 1.5 ml/min and a carrier gas flow rate of 1.2 l/min without extinguishing the plasma. Under these conditions, applying desolvator countercurrent gas flows in the range 0–8 l/min restored of the original pink color of the pure helium MIP from the bluish-green caused by methanol. Significant reductions in the emission intensities of C₂ species at 436.5, 473.7, 512.9, and 563.6 nm were observed with the application of the FSMD. The intensities of chlorine analyte emission lines at 479.5, 481.0 and 481.9 nm increased with increasing countercurrent gas flow rates and reached a maximum intensity with a flow rate of 5.0 l/min. Detection limits for Cl and Pb were 2.1 and 0.1 ppm using a 1 m focal length monochromator. Other elements and solvent combinations were also examined. Element selective liquid chromatographic detection was preliminarily examined by monitoring 2,6-dichlorobenzene and 5,7-dichlorohydroxyquinoline at the 479.5 nm Cl atomic emission line. Chlorine detection limits in the 3–7 μg range (70–190 ng/s) were obtained.