Simultaneous microchemical analysis of glycerol,fatty acid,and phosphorus in complex lipids

A single, small glycerol-containing lipid sample (50–200 nmoles) after a mild hydrolysis could be used for analysis of fatty acids, glycerol, and phosphorus. The range of the assays was from 10–500 nmoles for each lipid.     

Microanalysis of serum triglycerides with or without separation by thin-layer chromatography

A manual colormetric procedure for the determination of tissue or serum triglyceride is described. This procedure utilizes very stable reagents and will allow for analysis of triglycerides after separation by TLC without prior extraction from the silica gel. Serum triglyceride analysis requires only 20 μl.     

Gas-phase synthesis, submillimeter spectra, and precise structure of monomeric, solvent-free CuCH3

The most-studied organocopper, methylcopper (CH(3)Cu), has been synthesized for the first time as a monomer, free of other ligands or coordinated solvent, and detected using millimeter-wave rotational spectroscopy. The molecule was created in the gas phase by the reaction of copper vapor and several different precursors, including CH(4) and tetramethylsilane. An obvious symmetric top pattern was observed, indicative of C(3)(v) symmetry. For confirmation, rotational spectra of four isotopically substituted species, (65)Cu(12)CH(3), (63)Cu(12)CD(3), (63)Cu(13)CH(3), and (65)Cu(13)CH(3), were recorded as well, following large-scale syntheses of specifically labeled precursors. From this data set, accurate spectroscopic constants and a structure for CH(3)Cu were derived. The r(m)((2)) geometry shows the shortest alkyl carbon-copper(I) bond length known (1.8809 A) and a rather large H-C-H angle in the methyl group (109.88 degrees). The measured rotational and distortion constants are well reproduced by QCISD calculations. This study should allow further refinement of theoretical calculations on methylcopper and other organocopper derivatives, which are valuable synthetic intermediates in organic chemistry.