Theoretical aspects of a preparative continuous chromatograph

Summary Equipment which has been used or suggested for preparative scale chromatography is reviewed. Particular attention is paid to one form of equipment for continuous counter-current chromatography which employs a moving mechanical seal. The theoretical effects of practical operating conditions and the mode of operation of this equipment are discussed. The influence of these effects on polymer fractionation is also considered. A theoretical model, based on the equilibrium stage concept, is proposed for the simulation of continuous gel permeation chromatography of a binary feed on such an apparatus. Examples of the results obtained from the computer simulation are given.     

The Nitrosation of Primary Aliphatic Diazocarbonyl Compounds: Formation of α-carbonyl nitrile oxides. Preliminary communication

Aqueous nitrosation of primary α-carbonyl diazo compounds (ethyl diazoacetate, diazoacetone, diazoacetophenones) yields α-carbonyl nitrile oxides, R? CO? CNO; their formation is demonstrated by 1,3-dipolar addition reactions.     

Über die flüchtigen Anteile der Ananas

A gas chromatographic investigation of the volatile part of a pineapple concentrate led to the identification of 59 substances, 35 of which were not previously found in pineapple. The identifications and syntheses of some esters (Δ³- and Δ⁴-unsaturated, β-hydroxy, β-acetoxy, and δ-acetoxy) and of a new sulfur compound are given.     

Decarbonylation of N-carbazolylacetyl chloride in the friedel-crafts acylation reaction

Reaction products of N-carbazolylacetyl chloride under Friedel-Crafts reaction conditions include carbon monoxide, the reaction product from carbazole and formaldehyde (CF condensate), and carbazole. It is postulated that decarbonylation of N-carbazolylacetyl chloride involves intermediate formation of a N-carbazolylmethyl cation.     

Analyse qualitative et quantitative de melanges complexes de chlorures de lanthanides,en utilisant la dispersion rotatoire magnetique

The general features of a new physical process for the qualitative and quantitative routine analysis of rare earth mixtures are given. The characteristic sharp lines in the magneto-optical rotation spectra of these elements are utilized. The recording photoelectric spectropolarimeter used is described briefly. A comparison is made with two other physical processes-absorption and X-ray fluorescence spectrometry. The proposed method appears to be the best when a mixture with more than 3 or 4 elements must be analysed. The sensitivity and accuracy are given for 9 rare earths. Improvements of the process are suggested.     

Consequence of boar edible tissue consumption on urinary profiles of nandrolone metabolites. II. Identification and quantification of 19-norsteroids responsible for 19-norandrosterone and 19-noretiocholanolone excretion in human urine

In previous work (Le Bizec et al., Rapid Commun. Mass Spectrom. 2000; 14: 1058), it was demonstrated that a boar meal intake could lead to possible false accusations of abuse of 17beta-nortestosterone in antidoping control. The aim of the present study was to identify and quantify endogenous 19-norsteroids in boar edible tissue at concentrations that can alter the steroid urinary profile in humans, and lead to excretion of 19-norandrosterone (19-NA) and 19-noretiocholanolone (19-NE). The samples were analysed in two laboratories. The methodologies used for extraction and detection (GC/MS(EI) and LC/MS/MS(APCI+)) are compared and discussed. 19-Norandrostenedione (NAED), 17beta- and 17alpha-nortestosterone (bNT, aNT), and 17beta- and 17alpha-testosterone (bT, aT) were quantified. The largest concentrations of NAED and bNT were observed in testicles (83 and 172 microg/kg), liver (17 and 63 microg/kg) and kidney (45 and 38 microg/kg). A correlation between the bNT and NAED content of a typical meal prepared with boar parts and the excreted concentrations of 19-NA and 19-NE in human urine was demonstrated.     

Trennung von Spurenelementaktivitäten aus Neutronenbestrahltem Selen mit Hilfe der Gegenstrom-Ionenwanderung

For the determination of trace elements in neutron irradiated, selenium by gamma-ray spectrometry the separation of the matrix activity is often necessary. In model experiments the decontamination of cation and anion impurities from the matrix solution was investigated by the counter current ion migration. After a processing of 3 hrs the trace activities of Co, Cr, Ga, Na and Zn were decontaminated from Se with a factor of >10³. For the trace elements As and Te representing the anionic constituents, a decontamination factor of 3·10² was obtained.     

Synthesis and reactions of some dihydro and tetrahydro-4H-imidazo[5,4,1-ij]quinoline derivatives

Reaction of phenyl N-(8-quinolinyl)carbamate with sodium borohydride afforded 1,2-dihydro-4H-imidazo-[5,4,1-ij]quinolin-2-one, 2a . The 5,6-double bond of 2a was functionalized by reaction with nitrosyl chloride to give the nitroolefin 4 and by reaction with hypobromous acid to give the trans-bromohydrin 5 . Reaction of 5 with sodium azide led to the rearranged trans-6-azido-5-ol 7 , the structure of which was determined by ¹H nmr studies.