Cyclohexane residues in extracts (concretes, oleoresins, resinoids, etc.) – Determination by headspace capillary gas chromatography/mass spectrometry with selected ion monitoring (SIM)

1997 ◽  
Vol 204 (5) ◽  
pp. 397-397
Author(s):  
1988 ◽  
Vol 34 (8) ◽  
pp. 1597-1599 ◽  
Author(s):  
D A Herold ◽  
P K Anonick ◽  
M Kinter ◽  
F G Hayden

Abstract Rimantadine is a synthetic antiviral agent used in prophylaxis and in treating the early stages of uncomplicated influenza A illness. We describe a stable isotope-dilution assay involving capillary gas chromatography/mass spectrometry. We used 200 ng of d3-rimantadine, added to 1 mL of plasma, as the internal standard. The rimantadine was extracted from the plasma with a Bond-Elut CN column, the column was washed with water, and the rimantadine was eluted with methanol, dried, and treated to form the t-butyldimethylsilyl derivative. The mass spectrometer was operated in the selected ion monitoring mode. Ions at m/z 236 and m/z 239 were monitored, corresponding to the loss of C4H9 from the rimantadine derivative and d3-rimantadine, respectively. Within-run precision (CVs) ranged from 8.9% at 29 micrograms/L to 3.2% at 1666 micrograms/L. Corresponding data for between-run precision were 5.4% and 1.7%. Treated volunteers (n = 86) provided plasma samples with a concentration range of 153 to 1127 micrograms/L. This simplified method allows rapid, precise assay of rimantadine in plasma.


Sign in / Sign up

Export Citation Format

Share Document