Generalized evaluation subgroups of product spaces relative to a factor

For any -complexes and , we show that . We use this fact to compute generalized evaluation subgroups of generalized tori relative to a sphere.

     

New hydrolysis method for extremely small amount of lipids and capillary gas chromatographic analysis as n(O)-tert.-butyldimethylsilyl fatty acid derivatives compared with methyl ester derivatives

The organic basic solution, 1 M tetramethylammonium hydroxide (TMAH) in methanol, was employed for the hydrolysis of extremely small amounts of lipids compared to the classical inorganic basic solution, 1 M KOH in ethanol. The hydrolysed fatty acids were derivatized as N(O)-tert.-butyldimethylsilyl (tBDMSi) esters with N-methyl-N-(tert.-butyldimethylsilyl) trifluoroacetamide (MTBSTFA) and compared with the classical derivatives, the methyl esters, made by the BF3-methanol method. Recoveries of fatty acids determined on the standard fatty acids and soybean oil hydrolysed with TMAH were high: about 1.1-2.1- and 2.0-5.4-times, respectively, in all fatty acids compared with the hydrolysis by KOH regardless of derivatization method. The relative standard deviations (RSDs) on the recoveries of standard fatty acids were less than 5% when hydrolysed with TMAH, regardless of derivatives, but when hydrolysed with KOH, RSDs were more than 5% for most fatty acids, especially for long-chain fatty acids. The RSDs on the recoveries of fatty acids on the soybean oil were also very high in the KOH hydrolysis. Fatty acid compositions of soybean oil were similar in the main fatty acids regardless of hydrolysis methods, but showed slightly different values, depending on the methods of derivatization. RSDs were also very high in the KOH hydrolysis. In view of these results, precision of analysis by KOH hydrolysis was very poor, so we could not rely on the data. On the other hand, the reliability of data by TMAH hydrolysis method was very high, so it is a useful new hydrolysis method for extremely small amounts of lipid samples. Both derivatives of 35 standard fatty acids were successfully separated on a HP-1 nonpolar capillary column. tBDMSi derivatives were completely resolved in 70 min by 295 degrees C. In the methyl ester derivatives it took about 80 min to get satisfying resolution, but these derivatives were completely resolved by 250 degrees C. The sensitivity of tBDMSi derivatives was about 1.5-6.3-times higher than that with methyl ester derivatives. The stability of tBDMSi derivatives was constant for about 144 h except arachidic, docosahexanoic, behenic and heneicosanoic acids, which were stable for only 86 h.     

Gas chromatographic study of the urinary codeine-to-morphine ratios in controlled codeine consumption and in mass screening for opiate drugs

The urinary codeine-to-morphine ratios in fifteen volunteers administered codeine tablets at intervals were studied by gas chromatography (GC) and compared with one month's GC results for enzyme multiplied immunoassay technique (EMIT)-screened urine specimens in a mass-screening programme for abuse of opiate drugs, particularly heroin. It appears that when M less than 2 and C/M greater than 0 or when M greater than 2 and C/M greater than 0.5, where C and M are codeine and morphine concentrations in micrograms per 10 ml of urine, codeine consumption has to be presumed.     

Study of hydantoin. III . Mass spectrometric behaviour in the electron impact of 2-imino-4-thiazolidinone derivatives

The mass spectral decomposition modes of a series of 2-imino-4-thiazolidinone derivatives are reported and discussed. The fragmentation patterns and mechanisms postulated have been confirmed by the analysis of the MIKE spectra and using DADI technique and the effects of heteroatoms and substituents on the MIKE spectrum of these compounds are compared with that of 3-substituted hydantoins.     

π-Allyl palladium approach toward the diazabicyclo[3.2.1]octane core of the naphthyridinomycin alkaloids

A novel and efficient protocol for the synthesis of the 3,8-diazabicyclo[3.2.1]octane system found in the naphthyridinomycin, dnacin, and tetrazomine families of alkaloids is described. The key transformation involves an intramolecular palladium-catalyzed allylic alkylation. The cyclization proceeds smoothly under mild conditions (20 mol % Pd₂dba₃, 1.5 equiv DBU, 65 °C, THF, 20 min) to afford 3,8-diazabicyclo[3.2.1]octanes in excellent yields (94-98%).     

The structure of new lignans from the seeds of phytolacca americana

From the seeds of Phytolacca americana two new lignans, Americanin B and D, have been isolated and their structures elucidated mainly by spectroscopic methods     

Application of AM SURE™ resin to solid-phase peptide synthesis

A core-shell structure was found in AM SURE™ resin, in which most amino groups were located at the skin layer. The AM SURE™ resin revealed better synthetic efficiency, compared to the noncore-shell type resin in the synthesis of the fragment 65-74 of acyl carrier protein, the fragment 27-35 of HIV (human immunodeficiency virus) fusion inhibitor (T-20) and the Jung-Redemann 10-mer.