Je. Woodrow et al., DETERMINATION OF ETHYLENE-OXIDE IN SPICES USING HEADSPACE GAS-CHROMATOGRAPHY, Journal of agricultural and food chemistry, 43(8), 1995, pp. 2126-2129
A method was developed for determining the residues of ethylene oxide
(ETO) in dry spices. These residues result from commercial fumigation
practices to control insect pests. The analytical method makes use of
a headspace gas chromatograph, equipped with a porous layer open tubul
ar (PLOT) megabore column, and sealed 22 mt headspace vials containing
1 g aliquots of the spices. The spice samples, containing added 1-oct
anol, are thermostated for 20 min at a temperature of 60 degrees C pri
or to injection of microliter aliquots of the equilibrated headspace.
By holding the PLOT column at 70 degrees C, ETO will elute in about 8
min, after which time the column is heated at 30 degrees C/min to 220
degrees C, at which the temperature is held for 5 min to clear the col
umn for the next injection. On the basis of spice matrix standards, re
coveries of ETO from a variety of different spices fell in the range 7
5-130% (av = 100%, n = 120) for spiking levels covering the range 1-10
00 ppm. The practical limit of detection was 1 ppm. By using an automa
ted headspace instrument, it is possible to analyze over 60 samples in
a 24-h period.