Ja. Field et al., DETERMINATION OF ESSENTIAL OILS IN HOPS BY HEADSPACE SOLID-PHASE MICROEXTRACTION, Journal of agricultural and food chemistry, 44(7), 1996, pp. 1768-1772
A solid-phase microextraction (SPME) method is described for the deter
mination of the essential oils, humulene and caryophyllene, in the hea
dspace of female hop cones and male hop lupulin samples. Optimized SPM
E sampling parameters for the determination of the humulene to caryoph
yllene (H/C) ratio for female hops (50 mg) and male lupulin (25 mg) sa
mples include a 100 mu m poly(dimethylsiloxane) SPME fiber and a 4 h s
ample exposure period at a temperature of 50 degrees C. Increasing the
temperature to 90 degrees C or increasing the length of sample exposu
re at 50 degrees C promoted caryophyllene oxidation, In a survey of fi
ve female hop varieties, good agreement was found between the H/C rati
o obtained by headspace SPME and conventional steam distillation. The
H/C ratio for 10 male lupulin varieties determined by headspace SPME a
nd pentane extraction also indicated good agreement between the two ex
traction methods.