Determination of mercury in seafood by flow injection-cold vapor atomic absorption spectrometry after microwave digestion: NMKL interlaboratory study. Nordic Committee on Food Analysis

Ten laboratories participated in an interlaboratory method-performance (collaborative) study of a method for the determination of mercury in foods of marine origin by flow injection-cold vapor atomic absorption spectrometry after wet digestion using a microwave oven technique. The study was preceded by a training round of samples of known identity. The method was tested on a total of 7 seafood products: blue mussel (Mytilus edulis), cod muscle (Gadus morhua), crab (Cancer pagurus), scampi (Nephrops norwegicus), black scabbard fish (Aphnopus carbo), longnose velvet dogfish (Centroscymus crepidater), and Portuguese dogfish (Cenbroscymus coelolepis) with mercury concentrations of 0.14, 0.24, 0.35, 0.59,11.42, 4.2, and 13.2 microg/g, respectively. The materials were presented to the participants in the study as blind duplicates, and the participants were asked to perform single determinations on each sample. Repeatability relative standard deviations (RSDr) for mercury ranged from 2.4 to 14.0%. Reproducibility relative standard deviations (RSDR) ranged from 7.7 to 16.6%. HORRAT values for all samples were <1.0.     

Versatile solid-phase synthesis of secondary amines from alcohols. Development of an N-Boc-(o-nitrobenzene)sulfonamide linker

The development of a versatile amine releasing linker based on the modified o-nitrobenzene sulfonamide protective group is described. This new N-Boc-o-nitrobenzenesulfonamide (Boc-ONBS) linker enables the elaboration on resin of primary and secondary amines by sequential substitution of the sulfonamide moiety using the Mitsunobu reaction. A 16-member array of secondary and Boc protected primary amines was then prepared using this linker.     

Alkylamino- und Dialkylamino-phenoxy-methylsilane

Zusammenfassung Alkyl-und Dialkylamino-phenoxy-methylsilane ließen sich sowohl durch Umsetzung von Phenoxy-methyl-chlorsilanen mit primären und sekundären Aminen unter Cl/NRR-Austausch als auch durch Reaktion von Phenoxymethylsilanen mit substituierten Alkaliamiden unter C₆H₅O/NRR-Austausch gemäß den Gl. (1) bis (6) darstellen. Ihre Eigenschaften sind aus Tab. 1 zu ersehen.

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We succeeded in preparing alkyl- and dialkylamino-phenoxymethylsilanes by reaction of phenoxy-methyl-chlorosilanes with primary and secondary amines (Cl/NRR-exchange) as well as by reaction of phenoxymethylsilanes with substituted alkaliamides (C₆H₅O/NRR-exchange)according equations (1) to (6). Their properties are to be seen in table 1.

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53. Mitt.:U. Wannagat undG. Schreiner, Mh. Chem.96, 1902 (1965).

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Mit Auszügen aus der DissertationG. Schreiner und der DiplomarbeitJ. Pohl, Techn. Hochsch. Graz, 1964.     

Studies of the reactions between indole-2,3-diones (isatins) and 2-aminobenzylamine

Reflux of equimolecular amounts 2-aminobenzylamine and isatins in acetic acid produced indolo[3,2-c]quinolin-6-ones in good yields. A proposed mechanism involving initial formation of a spiro compound is given. This isolable intermediate subsequently rearranges via a sequential isocyanate ring opening and a cyclisation process to a urea derivative which finally cyclized to the indolo[3,2-c]quinolin-6-ones. The urea derivative could be prepared separately and cyclized selectively to indolo[3,2-c]quinolin-6-one. Reaction of N-acetylisatin with 2-aminobenzylamine at room temperature yielded the 1,4-benzodiazepinone 3-(2-acetamidophenyl)-1,5-dihydro-1,4-benzodiazepin-2-one whereas its isomer 2(2-acetamidophenyl)-4,5-dihydro-1,4-benzodiazepin-3-one was obtained from 2-(2-acetylaminophenyl)-N-(2-aminobenzyl)-2-oxoacetamide in acetic acid at room temperature.The previously unknown linear isomer of indolo[3,2-c]quinolin-6-one, i.e. indolo[2,3-b]quinolin-11-one, has been prepared by thermal (260°C) cyclization of methyl 2-phenylamino indole-3-carboxylate, which in turn was prepared in two steps from methyl indole-3-carboxylate.     

Monitoring of ethanol during fermentation using a microbial biosensor with enhanced selectivity

The present study is concerning the construction of ferricyanide-mediated Gluconobacter oxydans cell ethanol biosensor. The size exclusion effect of a cellulose acetate membrane was used for elimination of glucose interferences during ethanol assays in real samples. A typical response time of the biosensor was 13 s with a high sensitivity of 3.5 microA mM(-1). The microbial biosensor exhibits a very low detection limit of 0.85 microM and a wide linear range from 2 to 270 microM. The operational stability was excellent. During 8.5 h of repetitive ethanol assays, no decrease in the sensor sensitivity was observed. The biosensor was successfully used in the off-line monitoring of ethanol fermentation with a good agreement with HPLC measurements (R(2)=0.998).     

Compehensive two-dimensional gas chromatography (GC×GC) and its applicability to the characterization of complex (petrochemical) mixtures

In general, petrochemical products contain only a limited number of chemical classes of compounds (sample dimensionality). The enormous number of individual components within these classes, however, soon puts limitations upon a single chromatographic technique when it comes to adequate characterization of these products. Comprehensive two-dimensional gas chromatography (GC×GC) clearly opens the possibility of estimating the composition of hydrocarbon mixtures in a far more detailed fashion than hitherto possible. Although the emphasis of papers of GCxGC thus far almost exclusively applies to the unsurpassed peak-capacity, in the oil industry there is a need for characterization, rather than for analyzing all the individual compounds. In principle a GCxGC system can provide an almost perfect match between its intrinsic properties and the dimensionality of oil samples. To establish the applicability of GCxGC towards petrochemical analytical challenges, a commercially aavailable prototype instrument was subjected to an exhaustive characterization of a typical hydrocarbon precess stream and a fast characterization of a light gas oil. Although there are no fundamental limitations towards the quantitative aspects of a GCxGC system, this paper confines itself to qualitative results only. Quantitative aspects of GCxGC will be published in a forthcoming paper.     

Analysis of anthracycline antitumour drugs in tissues and body fluids using liquid chromatography

Anthracyclines, with doxorubicin as the major representative, are amongst the most important chemotherapeutic agents used in cancer therapy. In order to reduce the severe side effects associated with their use, and to increase therapeutic efficacy, analogue development still continues, and analytical requirements change concomitantly. The available methods for bioanalysis of anthracyclines are summarized, with emphasis on high-performance liquid chromatography. Attention is paid to sample pretreatment, the possibilities of liquid—liquid and solid-phase extraction, and the chromatographic behaviour of the anthracyclines.