process.

Isomerized -acid bitterness

BEER HOP EXTRACTION disintegrates during storage, since -
RUDY BASKETTE, SUPERCRITICAL FLUID
TECHNOLOGIES, INC
acids emerge during the later stages of
the brewing process; they provide a
more biting bitter flavor.
INTRODUCTION Hops have certain flavor profiles
ranging from citrusy, woodsy, spicy, or
The practice of beer brewing is fruity. The essential oils aspect of the
seven thousand years old and has out hops is where these different scents lie.
survived most of the cultures that drank Adding hops in to the early stages of
it. While the ancient Babylonians, boiling wort degrades all essential oils.
Romans, Assyrians, and Incan cultures So, dry hops are added to the end
can no longer partake in the nectar of stages of boiling wort or after the wort is
the gods, striving to brew the best beer cooled to harness the scents in the
is still a prevalent goal. One of the beer.
methods to improve the flavor of a beer To extract maximal flavor profiles,
is to enhance the intensity of the hops. SFT developed a lab-scale method
Supercritical carbon dioxide hop using the SFT-110 SFE to extract hop
extraction is a method to obtain hop oil oil. A two-step supercritical carbon
extracts with high concentrations (both dioxide extraction allows the separation
yield and purity) and quality (less of the aromatic/essential oils from the
artifacts). bittering agents in
There are 3 major chemical hops. The SFT-110
components to hops: produces a natural,
unaltered oil extract
that amplifies natural
hop flavor profiles.
Using this method,
brewers can acquire
a truly enhanced
flavor for their customers to enjoy.
The SFT-110 utilizes pressurized
-acids, -acids, and essential oils. carbon dioxide, allowing extraction to
When hops are added to boiling wort, - take place in room temperature
acids such as humulone, thermally environments, so a purer, less thermally
degrade to their iso- form. Isomerized decomposed extract is generated.
- acids induce bitter flavoring for the Carbon dioxide is also advantageous,
beer, as well as providing a slight because it does not introduce any
antibiotic effect against gram positive residual organic chemicals, meaning
bacteria. Unlike -acids, -acids do not that all extracts are safe to consume.
isomerize during the wort boiling CO 2 extraction extends the life of
process. -acids, such as lupulone, hop flavors. Hop pellets easily degrade,
leisurely oxidize during the fermentation but the integrity of a hop oil extract can
and storage phases of the brewing be maintained in a veritable climate.
Carbon dioxide extraction using the Brewer hop pellets were utilized for this
SFT-110 can separate the oils in a experiment. All the samples were
clean, energy efficient fashion. harvested in 2011 and bought from
Label Peelers Inc.
EQUIPMENT Weigh 20 grams of hop pellets on
Analytical Balance an analytical balance. Grind up pellets
SFT-110 SFE Unit to 1mm x 1mm and load into the SFT
SFT 100 cc Sample Vessel 100 cc Sample Bag. Place the SFT 100
SFT 100 cc Sample Bag cc Sample Bag into a SFT 100 cc
sample vessel (10kpsi, 200C
operation).
MATERIALS Seal the vessel and set into a SFT-
Hop pellets 110 SFE unit. Two fractions of oil will be
2 SFT Collection Vials collected via
1 SFT Vent Tube multiple (10)
soak and
dynamic flow
steps. Place
a chilled pre-
weighed SFT
collection vial
on the flow
line. Extract
the samples
according to the following parameters:

EXTRACTION PARAMETERS
Two fractions of oil will be collected
via multiple soak and dynamic flow
cycles according to the guidelines
below.

FRACTION 1: ESSENTIAL OIL EXTRACT

Figure 1. SFT-110 SFE Unit
Pressure: 2180 psi
Temperature: 40C
EXPERIMENTAL PROCEDURE CO 2 Flow Rate: 4mL/min
A simple two-step SFE extraction 10 static and dynamic steps for
method using the SFT-110 was 15 minutes apiece
employed to separate aromatic from
bitter components of hops. Four After Fraction 1, change out the
samples: Sorachi Ace, Summit, U.S. collection vial and replace with another
Brewers Gold, and U.S. Northern clean, tared vial for fraction 2 products.
 commonly used for its lemon and dill
FRACTION 2: BITTERING COMPOUNDS essence in IPA and Pale Ale, has the
Pressure: 4350 psi highest total yield of products. Summit,
Temperature: 40C U.S. Northern Brewer, and U.S. brewer
CO 2 Flow Rate: 4mL/min Gold respectively followed in yield
10 static and dynamic steps for product.
15 minutes apiece

After Fraction 2, you can remove the

SFT 100 cc sample bag from the SFT-
100 cc vessel and proceed to clean the
SFT-110 SFE.

RESULTS
The aromatic extracts will yield a
distinctly different color product than the
bittering extract. Fraction 1, the
essential oil and aromatic hop Figure 2. SFE-CO 2 Extraction of Sorachi Ace
extraction, will yield a bright yellow
product. Fraction 2, the bittering Figure 2 is the extraction yield
compound extraction product, will yield results for Sorachi Ace at 2180 and
a dark yellow, light brownish color. 4350 psi. Basically this table is serving
to indicate the yield of SFE CO 2 hop
Hop Type Yield @ Yield @ Total extraction at specific time intervals.
2180 psi 4350 psi Yield

(g/100 g) (g/100g)

Sorachi Ace 13.65 9.79 23.44

Summit 12.94 8.31 21.25

U.S. Brewer's 9.89 8.66 18.55

Gold

U.S. Northern 12.20 4.59 16.79

Brewers
Figure 3. GC/MS Sorachi Ace extract @ 4350 psi
Table 1. SFE-CO 2 Hop Variety Extraction Yields
Figure 3 is the GC/MS
Table 1 is the extraction yield chromatograph of Sorachi Ace extract at
results for the 4 hop types at 2180 and 4350 psi. Notice the presence of
4350 psi. These particular hops were lupulone and lupulone constituents, i.e.
chosen specifically for their high oil -acids.
content. As you can see Sorachi Ace,
CONCLUSIONS
Aromatic and bitter components of
hops can be extracted using the lab-
scale SFT-110 SFE Unit. Supercritical
CO 2 extraction can isolate specific
components with slight adjustments to
temperature or pressure. Regarding
hops, aromatic compounds/essential
oils are extracted at 2180 psi, and bitter
components are extracted at 4350 psi.
Sorachi Ace yielded the highest
aromatic and bitter fractions. GC/MS
analysis of Sorachi Ace bitter oil fraction
yielded lupulone and lupulone
constituents. These compounds are
solely characteristic of bitter fractions.
Distinctive aromatic compounds, i.e.
humulone or its isomers were present in
the GC/MS analysis of Sorachi Ace at
2180 psi, indicating that the 2-phase
extraction was indeed successful in
separating aromatic and bitter
components.

REFERENCES
Zoran, Zekovic, Pfaf-Sovljanski Ivana,
and Grujic Olgica. "Supercritical Fluid
Extraction of Hops." Journal of the
Serbian Chemical Society 72.1 (2007):
81-87.
<http://www.doiserbia.nb.rs/img/doi/035
2-5139/2007/0352-51390701081Z.pdf>.