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Journal ArticleDOI

N-Methyl-N-trimethylsilyl-trifluoracetamid, ein neues Silylierungsmittel aus der Reihe der silylierten Amide.

01 Jan 1969-Journal of Chromatography A (Elsevier BV)-Vol. 42, Iss: 1, pp 103-104
About: This article is published in Journal of Chromatography A.The article was published on 1969-01-01. It has received 118 citations till now.
Citations
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Journal ArticleDOI
TL;DR: The mechanism of the silylation reaction and the methods of synthesis and properties of silylating agents are discussed in this paper, together with the Silylation of various classes of compounds in relation to the most characteristic substances.
Abstract: The mechanism of the silylation reaction and the methods of synthesis and properties of silylating agents are discussed together with the silylation of various classes of compounds in relation to the most characteristic substances. The bibliography includes 186 references.

263 citations

Journal ArticleDOI
TL;DR: Main derivatization procedures for opiates, cocaine, cannabis, amphetamines, benzodiazepines and LSD have been reviewed and papers describing the analyses of drugs of abuse in matrixes other than blood, such as hair or sweat, have received special attention.

237 citations

Journal ArticleDOI
TL;DR: Advances in silylation as a powerful tool used for increasing the volatility, thermal and thermo-catalytic stability, and chromatographic mobility of polar and unstable organic compounds are described.
Abstract: This is the first of a series of reviews on the application of derivatization in mass spectrometry. A description is given of advances in silylation as a powerful tool used for increasing the volatility, thermal and thermo-catalytic stability, and chromatographic mobility of polar and unstable organic compounds. In addition to chemical aspects of silylation, mass spectral properties of silyl derivatives useful for structure determination and quantitation of various organic and biologically-active compounds, mainly by GC/MS, are described. Practically all tested and widely used silylating agents are described. The role of comprehensive libraries containing reference mass spectra for various silyl derivatives and search systems in structure determination is emphasized. Applications of silylation for particular analyses are summarised.

213 citations

Journal ArticleDOI
TL;DR: The cloning of the first bacterial steroid biosynthesis gene, cas, encoding the cycloartenol synthase (Cas) of S. aurantiaca is described, indicating a close evolutionary relationship between myxobacterial and eukaryotic steroids biosynthesis.
Abstract: Summary Steroids, such as cholesterol, are synthesized in almost all eukaryotic cells, which use these triterpenoid lipids to control the fluidity and flexibility of their cell membranes. Bacteria rarely synthesize such tetracyclic compounds but frequently replace them with a different class of triterpenoids, the pentacyclic hopanoids. The intriguing mechanisms involved in triterpene biosynthesis have attracted much attention, resulting in extensive studies of squalene-hopene cyclase in bacteria and (S)-2,3-oxidosqualene cyclases in eukarya. Nevertheless, almost nothing is known about steroid biosynthesis in bacteria. Only three steroid-synthesizing bacterial species have been identified before this study. Here, we report on a variety of sterol-producing myxobacteria. Stigmatella aurantiaca is shown to produce cycloartenol, the well-known first cyclization product of steroid biosynthesis in plants and algae. Additionally, we describe the cloning of the first bacterial steroid biosynthesis gene, cas, encoding the cycloartenol synthase (Cas) of S. aurantiaca. Mutants of cas generated via site-directed mutagenesis do not produce the compound. They show neither growth retardation in comparison with wild type nor any increase in ethanol sensitivity. The protein encoded by cas is most similar to the Cas proteins from several plant species, indicating a close evolutionary relationship between myxobacterial and eukaryotic steroid biosynthesis.

167 citations


Cites methods from "N-Methyl-N-trimethylsilyl-trifluora..."

  • ...…HP 5890 A series II) and GC-MS analysis (GC: Carlos Erba; MS: Kratos MS 50 or Finnigan MAT GCQ) of the extracts after silylation with MSTFA (Donike, 1969) or acetylation with acetic acid anhydride or trifluoroacetic acid anhydride against various standards as described previously…...

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  • ..., 1963; Claude, 1966), by their retention time in GC (Hewlett-Packard HP 5890 A series II) and GC-MS analysis (GC: Carlos Erba; MS: Kratos MS 50 or Finnigan MAT GCQ) of the extracts after silylation with MSTFA (Donike, 1969) or acetylation with acetic acid anhydride or trifluoroacetic acid anhydride against various standards as described previously (Ogunkoya, 1981)....

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  • ...Squalene, di- and tetrahydrosqualene and sterols were identified by comparative TLC against standards (Radin, 1981) using either rhodamine 6G or ZAK reagent for detection (Avigan et al., 1963; Claude, 1966), by their retention time in GC (Hewlett-Packard HP 5890 A series II) and GC-MS analysis (GC: Carlos Erba; MS: Kratos MS 50 or Finnigan MAT GCQ) of the extracts after silylation with MSTFA (Donike, 1969) or acetylation with acetic acid anhydride or trifluoroacetic acid anhydride against various standards as described previously (Ogunkoya, 1981)....

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Journal ArticleDOI
TL;DR: A total of 116 anabolic steroid positives were found in this laboratory in 1995 via GC-MS and GC-HRMS screening of 6700 human urine specimens collected at national and international sporting events and at out-of-competition testing.

129 citations

References
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Journal ArticleDOI
TL;DR: In this paper, the silylation of amides, ureas, and amino acids, as well as hindered phenols, carboxylic acids, and enols, is described.
Abstract: Silyl-proton exchange reactions with bis(trimethylsilyl)acetamide proceed rapidly and quantitatively under mild conditions. The preparative silylation of amides, ureas, and amino acids, as well as hindered phenols, carboxylic acids, and enols, is described. Examples of silylation as a protective measure and a means of preparing reactive intermediates are included.

353 citations