6
Large volume injections (LVI) can be used to determine flavor compounds in alcoholic
beverages such as malt whiskeys and grappas. Whiskey is distilled from a fermented
mashof grain, such as corn, rye, barley, orwheat.Thewhiskey is aged inbarrels or casks,
and it is during the aging process that whiskey obtains its characteristic color, flavor, and
aroma. Factors that influence the flavor of the final product include the characteristics of
the grain, the recipe, and how the whiskey is distilled. The flavor profiles of whiskeys
contain hundreds of compounds, including fatty acids, esters, alcohols, and aldehydes, in
a wide range of concentrations. An example of a malt whiskey profile, determined by
GC/MS, is shown in Figure 6.
Malt whiskey profile, determined by GC/MS, using a Stabilwax
®
-DA column and a large volume injection technique.
Figure 6
Stabilwax
®
-DA 30m, 0.18mm ID, 0.18µm (cat.# 550752)
Inj.:
10µL large volume injection (splitless),
at 10µL/min.
Std. conc.:
neat
Gerstel CIS Injector: 35°C (hold 2min.), to 300°C@
10°C/sec. (hold 5min.)
Helium vent flow:
600mL/minwith 1.8min. vent end time
Carrier gas:
helium
Linear velocity:
45cm/sec.
Oven temp.:
60°C (hold 2min.) to 100°C@
20°C/min., to 240°C@ 5°C/min.
(hold 10min.)
Det.:
MSD
Transfer line temp.:
240°C
Quadrupole temp.:
150°C
MS source temp.:
230°C
Scan range:
30–400amu
Ionization:
70eV
Mode:
EI
Chromatogram courtesy of KevinMacNamara, Ph.D., IrishDistilleries, Ltd.
1. ethyl octanoate
2. acetic acid
3. siloxane
4. 1-hydroxy-2,3-butadione
5. 1-hydroxy-2-propanone
acetate
6. furfural
7. formic acid
8. propionic acid
9. isobutyric acid
10. dimethyl sulfoxide
11. 5-methyl furfural
12. methyl decanoate +
unknown
13. butyric acid
14. siloxane
15. ethyl decanoate
16. furfuryl alcohol
17. isoamyl octanoate
18. isovaleric acid
19. 2-methylbutyric acid
20. diethyl succinate
21. 3-methyl-2(5H)-furanone
(possible)
22. valeric acid
23. ethyl undecanoate
24. isobutyl decanoate
25. 2(5H)-furanone
26. unknown
27. di(ethyleneglycol) butyl
ether
28. siloxane
29. methyl dodecanoate
30. 2-phenylethyl acetate
31. methylcyclopentenolone
32. hexanoic acid
33. ethyl dodecanoate
34. isoamyl decanoate
35. guaiacol
36. dodecyl acetate (possible)
37. whiskey lactone (1)
38. 2-phenylethanol
39. heptanoic acid
40. siloxane
41. dimethoxybenzene or
4-methylguaiacol
42. whiskey lactone (2)
43. dodecanol
44. unknown
45. phenol
46. methyl tetradecanoate
47. nerolidol
48. diethyl malate
49. ethyl tetradecanoate
50. octanoic acid
51. unknown
52.
p
-cresol
53. siloxane
54. diethyl octanedioate
55. monomethyl succinate (possible)
56. 3,5-dimethyl-2,4(5H)
furandione
57. nonanoic acid
58. diethyl 2-hydroxyglutarate
59 unknown
60. tetradecanol
61. 4-vinylguaiacol
62. diethyl nonanedioate
63. methyl hexadecanoate
64. ethyl
γ
-lactone
2-hydroxyglutarate
65. ethyl hexadecanoate
66. decanoic acid
67. ethyl 9-hexadecenoate
68. triacosan
69. unknown
70. phthalide
71. diethylphthalate
72. hexadecanol
73. 4-hydroxycinnamic acid
(decomp.)
74. methyl stearate
75. benzoic acid
76. methyl 8-octadecenoate
77. ethyl stearate
78. dodecanoic acid
79. hydroxymethylfurfural
80. ethyl linoleate
81. 4-allyl-2,6-dimethoxyphenol
82. diisobutyl phthalate
83. vanillin
84. sinapic acid (decomp.)
85. 2-phenylethyl decanoate +
2 unknowns
86. 4-propenyl-2,6-
dimethoxyphenol
87. ethyl vanillate
88. acetovanillone
89. vanillinmethyl ketone
90. tetradecanoic acid
91. ethyl homovanillate
92. propiovanillone
93. fatty acid ester
94. (similar to 4-allyl-2,6-
dimethoxyphenol)
95. unknown
96. hexadecanoic acid
97. syringealdehyde
GC_FF00603
