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[Determination of indolalkylamines after selective derivatisation (author's transl)].

Journal of chromatography (1977-04-11)
M Donike, R Gola, L Jaenicke
PMID192749
ABSTRACT

The 1N-TMS-omegan-TFA-derivatives of indolalkylamines are suitable for estimation by combined gas chromatography and mass spectrometry for two reasons, viz. (1) Under electron impact charge stabilisation at the indole nucleus is favoured, so structure-specific ions form the base peak. For unsubstituted indoles m/e values of 202 are found and for hydroxyl-substituted indoles m/e values of 290. (2) The calibration curves of the derivatives are linear, even in the femtomole range. The 1N-TMS-omegan-derivatives can easily be obtained by trimethylsilylation with N-methyl-N-trimethylsilyltrifluoroacetamide containing catalytic amounts of N-trimethylsilylimidazole followed by acylation with N-methyl bis(trifluoroacetamide). The serotonin concentrations in different rat tissues are determined by this method of selective omegaN-trifluoroacylation-1N-trimethylsilylation and compared with the values obtained by pertrimethylsilylation.

MATERIALS
Product Number
Brand
Product Description

Supelco
N-Methyl-N-(trimethylsilyl)trifluoroacetamide, for GC derivatization, LiChropur, ≥98.5%
Supelco
N-Methyl-bis(trifluoroacetamide), for GC derivatization, LiChropur, ≥99.0% (GC)