GC Analysis of Volatiles in Limoncello on SLB®-5ms after SPME using a 100 μm PDMS Fiber
Materials
analytical column
SPME fiber
SPME fiber assembly Polydimethylsiloxane (PDMS)
df 100 μm(PDMS, needle size 24 ga, for use with manual holderrelated product
standard
CONDITIONS
sample/matrix
Limoncello diluted 1:100 in water, then 5 mL of this solution transferred to a 10 mL crimped vial spiked with 100 μL of a 100 ppm solution of nonane (internal standard)
SPME fiber
100 μm polydimethylsiloxane (57300-U)
extraction
headspace, with a pre-equilibration period of 10 min. at 40 °C, and then a fiber exposure of 30 min. at 40 °C, agitated in an alternate clockwise-anticlockwise rotation mode at 500 ppm
desorption process
250 °C for 5 min
column
SLB-5ms, 30 m x 0.25 mm I.D., 0.25 μm (28471-U)
oven
40 °C, 3 °C/min to 250 °C (2 min)
inj. temp.
250 °C
detector
FID, 260 °C (sampling rate 80 ms)
carrier gas
helium, 35.0 cm/sec
injection
splitless
liner
0.75 mm I.D. SPME (2633901)
sample
Limoncello liquor
Description
Analysis Note
In this application, SPME was used for the analysis of volatiles in limoncello using a headspace method. SPME is ideal for the analysis of aroma volatiles in flavored beverages such as liquors. A 100 μm PDMS fiber was inserted into the headspace of the limoncello sample for 30 minutes at 40 °C followed by GC analysis using FID detection. The SLB-5ms GC columns provide consistently low-bleed, inert, efficient, and durable separations.
Legal Information
SLB is a registered trademark of Merck KGaA, Darmstadt, Germany