Page 209 - Tandem Techniques

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In the plasma analysis 50 µ1 of standard was added to 1 ml of plasma and 1 ml of 10 M NaOH and the
mixture hydrolyzed at 100°C for 16 hours. 1 ml of water and 3 ml of toluene were then added and the
tube shaken for 10 minutes. A sample of the toluene layer was then worked up in the same way as that
used for the urine sample. A Carlo Erba GC equipped with an auto sampler was employed with a
capillary column 25 m long, 250 µm I.D. carrying a stationary phase film 0.25 µm thick. The column
was heated at 100°C for 1 minute, then heated to 300°C at 15 ° per minute and then maintained at 300°
C for two minutes. The mass spectrometer was the Trio 1000 quadrupole operated in the negative ion
chemical ionization mode using ammonia as the reagent gas. The interface temperature was maintained
at 300ºC and the ion source at 200 °C. Chromatograms, obtained by selected ion monitoring, from both
urine and blood serum samples from patients who had been exposed to 1.5 µmol of
4,4'methylenebisaniline are shown in figure 5.19.

Figure 5.19
Selected Ion Monitoring of Urine and Blood
Samples After Dermal Exposure to 1.5 µmol
of 4,4'-Methylene Bisaniline [ref. 18]