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  • Derivatisation and gas chromatography-chemical ionisation mass spectrometry of selected synthetic and natural endocrine disruptive chemicals.

Derivatisation and gas chromatography-chemical ionisation mass spectrometry of selected synthetic and natural endocrine disruptive chemicals.

Journal of chromatography. A (2003-04-22)
Oliver Lerch, Peter Zinn
ABSTRACT

Methods for ultra trace detection of endocrine disruptive chemicals (EDCs) are needed because of their low levels of impact. Twenty-one EDCs were selected, including 17beta-estradiol, 17alpha-ethinylestradiol, 17beta-testosterone and bisphenol A. Derivatisation with eight different fluorine containing compounds was examined. All EDCs could be derivatised automatedly (autosampler) with heptafluorobutyric acid (HFB) anhydride and trifluoroacetic acid (TFA) anhydride, respectively. The detection of these HFB and TFA derivatives in different chemical ionisation modes was studied. Fourteen different reagent gases, including methane, ammonia, acetone and water, were tested with the HFB and TFA derivatives in the negative chemical ionisation mode. Furthermore both types of derivatives were measured in positive chemical ionisation mode. Methane or water provide a good detection of all 21 TFA derivatives and create mass spectra with few fragmentation and characteristic mass peaks. This could serve as a basis for tandem or multiple mass spectrometric measurements.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Heptafluorobutyric anhydride, ≥98%
Supelco
Heptafluorobutyric anhydride, for GC derivatization, LiChropur, ≥99.0%
Supelco
Heptafluorobutyric anhydride, for GC derivatization, LiChropur, ≥99.0%