US EPA

5916695 

Journal Article 

Derivatives of diethylstilbestrol (DES), mass spectral properties and their use in biological analysis 

Ryan, JJ; Miles, WF 

1978 

Yes 

International Journal of Environmental Analytical Chemistry
ISSN: 0306-7319
EISSN: 1029-0397 

5 

2 

133-142 

HEEP COPYRIGHT: BIOL ABS. A series of perfluoroester and chloroacetate derivatives of diethylstilbestrol (DES) were prepared from the corresponding anhydride using trimethylamine as a catalyst. In all cases, accurate mass measurements by high resolution electron impact (EI) mass spectrometry of mug or less quantities showed a strong base peak which corresponded to the disubstituted product. Gas chromatography-mass spectrometric (GC-MS) analysis of DES derivatives showed no change in any of the patterns due to thermal instability for the cis or trans isomers. Beef liver samples containing 2 ng/g of DES were analyzed by the trifluoroacetate (TFA) and heptafluorobutyrate (HFB) derivatives using GC-EC (gas chromatography-electron capture) and GC-MS with single ion monitoring. For HFB, no interference was observed by either detection mode but, for the TFA, interferences which showed up by GC-EC were absent on GC-MS. Due to the stability and good mass spectral patterns of the derivatives, GC-MS lends itself well to the confirmation of these DES derivatives in biological samples.