Comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry detection: analysis of amino acid and organic acid trimethylsilyl derivatives, with application to the analysis of metabolites in rye grass samples

First, standard mixtures of trimethylsilyl (TMS) derivatives of amino acid and organic acid are analyzed by comprehensive two-dimensional (2D) gas chromatography (GC) coupled to time-of-flight mass spectrometry (GC × GC/TOFMS) in order to illustrate important issues regarding application of the technique. Specifically of interest is the extent to which the peak capacity of the 2D separation space has been utilized and the procedure by which the derivative standards are identified in the 2D separations using the mass spectral information. The resulting 2D separation is found to make extensive use of the GC × GC separation space provided by the complementary stationary phases employed.Second, in order to demonstrate GC × GC/TOFMS on two real sample types, trimethylsilyl metabolite derivatives were analyzed from extracts of common lawn grass samples (i.e., perennial rye grass), as a means to provide insight into both the pre and post harvest physiology. Various chemical components in the two rye grass extract samples were found to either emerge or disappear in relation to the trauma response. For example, a significant difference in the peak for the TMS derivative of malic acid was found. The successful analysis of various components was readily facilitated by the 2D separation, while a 1D separation would have produced too much peak overlap, thus impeding the analysis. The importance of using a GC × GC separation approach for the analysis of complex samples, such as metabolite extracts, is therefore demonstrated. The real-time analysis capability of GC × GC/TOFMS for multidimensional metabolite analysis makes this technique well suited to the high-throughput analysis of metabolomic samples, especially compared to slower, stopped-flow type separation approaches.     

Separation, recovery and recycling of a fluorous-tagged nickel catalyst using fluorous solid-phase extraction

Highly efficient separation, recovery and recycling of the fluorous-tagged catalyst, [Ni[F13C6C(O)CHC(O)C6F13]2], can be achieved with fluorous solid-phase extraction, after the Lewis acid catalysed synthesis of enaminodiones in conventional organic solvents.     

Halochrome Molekeln. Synthese und acidobasisches Verhalten substituierter 3′,6′-Bis (dimethylamino)-spiro [5H-imidazo [2, 1-α]-isoindolin-5,9′-xanthene]

Halochromic Molecules. Synthesis and Acidobasic Behaviour of Substituted 3′,6′-Bis(dimethylamino)-spiro [5H-imidazo [2,1-α]isoindolin-5,9′-xanthenes] Substituted 3′,6′-Bis (dimethylamino)-spiro [5H-imidazo [2, 1-α]isoindolin-5,9′-xanthenes] are prepared and their ¹H-NMR. spectra are discussed. An investigation of the complex protonation equilibria is made by stopped flow kinetic and spectrophotometric methods. pK values are determined and the results are discussed.     

Reactions of transition-metal carbonyls with anhydrous HF

The reactions of a wide range of transition-metal carbonyls with anhydrous HF are described. In particular, Ru₃(CO)₁₂, Os₃(CO)₁₂ and Ir₄(CO)₁₂ give the solution stable [Ru₃(CO)₁₂H]⁺, [Ru(CO)₅H]⁺, [Os₃(CO)₁₂H]⁺, [Os(CO)₅H]⁺ and [Ir₄(CO)₁₂H₂]²⁺ respectively, which have been characterised by a combination of ¹H and ¹³C NMR spectroscopy.     

Über die katalytische Spaltung von Orthoestern an Aluminiumoxyd

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Über das Tabakaroma

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Futtermittel

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