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Shellhammer Laboratory
Department of Food Science and Technology
Daniel Sharp, Ph.D.
Director of Brewing Operations
Ninkasi Brewing Company
Stone Fruit
DH HHA DH Simcoe
WP HHA Floral
Citrus
Tropical Fruit
Overall
F2 (20.37%)
Simcoe WP
Amarillo WP
Citra DH
Galaxy DH
Amarillo DH
Galaxy WP catty/sweaty
Nelson Sauvin WP Mosaic DH
Control Cascade WP Hallertau MF DH
F2 (8.5%)
green/vegetal OHAI
pine/resinous
herbal/spicey citrus
tropical fruit
Huell Melon WP Citra
floral Simcoe DH WP
Nugget DH fruity Mosaic WP
Nugget WP Cascade DH
Hallertau MF WP
Saaz WP Chinook WP
Chinook DH
Saaz DH
Huell Melon DH
F1 (79.5%)
Simcoe WP
Amarillo WP
Citra DH
Galaxy DH
Amarillo DH
Galaxy WP catty/sweaty
Nelson Sauvin WP Mosaic DH
Cascade WP Hallertau MF DH
F2 (8.5%)
green/vegetal OHAI
pine/resinous
herbal/spicey citrus
tropical fruit
Huell Melon WP floral Citra WP
Simcoe DH
Nugget DH fruity Mosaic WP
Nugget WP Cascade DH
Hallertau MF WP
Saaz WP Chinook WP
Chinook DH
Saaz DH
Huell Melon DH
F1 (79.5%)
Sharp, 2016
PCA biplot of Descriptive Data
Nelson Sauvin DH
Simcoe WP
Amarillo WP
Citra DH
Galaxy DH
Amarillo DH
Galaxy WP catty/sweaty
Nelson Sauvin WP Mosaic DH
Cascade WP Hallertau MF DH
F2 (8.5%)
green/vegetal OHAI
pine/resinous
herbal/spicey citrus
tropical fruit
Huell Melon WP floral Citra WP
Simcoe DH
Nugget DH fruity Mosaic WP
Nugget WP Cascade DH
Hallertau MF WP
Saaz WP Chinook WP
Chinook DH
Saaz DH
Huell Melon DH
F1 (79.5%)
Sharp, 2016
PCA biplot of Descriptive Data
catty/sweaty
F2 (8.5%)
green/vegetal OHAI
pine/resinous
herbal/spicey citrus
tropical fruit
floral
fruity
F1 (79.5%)
Descriptor Group 3
Sharp, 2016
PCA biplot of Descriptive Data
catty/sweaty
F2 (8.5%)
green/vegetal OHAI
pine/resinous
herbal/spicey citrus
tropical fruit
floral
fruity
F1 (79.5%)
Descriptor Group 3
Sharp, 2016
Take-aways
• Normal process variation = minimal effect
• Extraction efficiencies may be very low
• Dry-hopping increases aromatic intensity relative to late hopping
• Aroma character may be significantly difference between the two
19 Farms CAS_26_16
CAS_06_16
WA
ID
12
7
0.9
0.9
• Sample inhomogeneity
• Dissolved oxygen uptake
• Package scalping
Hop Preparation and Dry-Hopping Parameters
Filtration
DH Event 1 DH Event 2
3.8 g/L 3.8 g/L
DO
Dry-hop for 24 hrs
DO
3.8 g/L
Spec. 110 ppb
Carbonated treatment
14.0
12.0 Overall Hop Aroma Intensity
Sensory Score (15pt scale) 10.0
8.0
6.0
4.0
2.0
0.0
0 2 4 6 8 10 12 14 16 18
Dry Hop rate (g/L)
Hop dosage rate – Overall Hop Aroma Intensity
14.0
12.0 c Overall Hop Aroma Intensity
Sensory Score (15pt scale)
c
10.0
b
8.0
a
6.0
4.0
a
2.0
0.0
0 2 4 6 8 10 12 14 16 18
Dry Hop rate (g/L)
14.0
12.0 c Overall Hop Aroma Intensity
Sensory Score (15pt scale)
c
10.0
b
8.0
a
6.0
4.0
a
2.0
0.0
0 2 4 6 8 10 12 14 16 18
Dry Hop rate (g/L)
• Panelists scaled the samples randomly against 28 other samples in the DA panel
• Range of DA OHAI ratings (i.e. ~6- 9.5) for 2015 DA Panels –Same DH rate 3.8/g/L
14.0
12.0 Overall Hop Aroma Intensity
Sensory Score (15pt scale) 10.0 Herbal/ Tea
8.0
6.0
Citrus
4.0
2.0
0.0
0 2 4 6 8 10 12 14 16 18
Dry Hop rate (g/L)
Hop dose response – hoppy quality (citrus and herbal/tea)
14.0
12.0 c Overall Hop Aroma Intensity
Sensory Score (15pt scale)
c Herbal/ Tea
10.0 c
b
8.0 c
a b
6.0 b
a b
b Citrus
4.0 a a
2.0 a
a
0.0
0 2 4 6 8 10 12 14 16 18
Dry Hop rate (g/L)
Linalool (ppb)
80
60
40
20
0
0 2 4 6 8 10 12 14 16 18
Dry hop rate (g/L)
40 2
Geraniol (ppb)
30 1.5
Nerol (ppb)
20 1 #
#
10 0.5
0 0
0 2 4 6 8 10 12 14 16 18 0 2 4 6 8 10 12 14 16 18
Dry hop rate (g/L) Dry hop rate (g/L)
#Estimated values lower than LOQ
*Average of 4 SPME-GC/MS instrumental runs
Hop Compound Concentrations – Terpene Alcohols
120
100
Linalool (ppb)
80
60
40
aKishimotoJ. Agric. Food
20 Detection threshold 1 ppba
Chem Vol 54, no 23. 2006
0
0 2 4 6 8 10 12 14 16 18
Dry hop rate (g/L)
40 2
Geraniol (ppb)
30 1.5
Nerol (ppb)
20 1 #
#
10 0.5
Detection threshold 4 ppba
0 0
0 2 4 6 8 10 12 14 16 18 0 2 4 6 8 10 12 14 16 18
Dry hop rate (g/L) Dry hop rate (g/L)
*Average of 4 SPME-GC/MS instrumental runs #Estimated values lower than LOQ
Hop total oil + compositional analysis
Internal Standard
2-octanol
Target Hop Analytes
Linalool
Terpinen-4-ol
α-terpineol
Nerol
Phenyl Acetate
Geraniol
Geranial-citral
Methyl Geranate
Geraniol Acetate
β-Caryophellyene
α-Humulene
β-Farnesene
Gernyal Isobutyrate
Hop Compound % Extraction – Terpene Alcohols
25
% Linalool extracted
from hop material
20 Dry hop rate
15
10
5
Terpene alcohol
0 extraction (%)
0 2 4 6 8 10 12 14 16 18
Dry hop rate (g/L)
% Geraniol extracted
7 7
from hop material
3.50 4.5
3.40 4.4
pH
4.3
3.30
4.2
3.20 4.1
3.10 4.0
0 2 4 6 8 10 12 14 16 18 0 2 4 6 8 10 12 14 16 18
Dry Hop Rate (g/L) Dry Hop Rate (g/L)
Bitterness?
30.0
*pH and RE measured
25.0
BU using Anton Paar Alcolyzer
20.0
BU
BITTERNESS
OF DRY-HOPPED BEER
How does the nonvolatile fraction influence
dry-hopped beer quality?
Essential oils 3%
Carbohydrates 4%
Minerals 8%
OREGON STATE UNIVERSITY
How does the nonvolatile fraction influence
dry-hopped beer quality?
Protein 15%
Essential oils 3%
Carbohydrates 4%
Minerals 8%
OREGON STATE UNIVERSITY
Hop acids (up to ~20% of hops)
Alpha Acids
Beta Acids
Beta Acids
Hulupones
(oxidized beta acids)
OREGON STATE UNIVERSITY
Hop acids – what you may find in beer
Iso-Alpha Acids
Alpha Acids
Humulinones
(oxidized alpha acids)
Hulupones
(oxidized beta acids)
OREGON STATE UNIVERSITY
Hop acids – what you may find in beer
Iso-Alpha Acids
Alpha Acids
Humulinones
(oxidized alpha acids)
X
Hulupones
(oxidized beta acids)
OREGON STATE UNIVERSITY
Regarding dry-hopped beers…
Does BU work? What drives bitterness?
Beer: 121 unique brands from 42 breweries
• 30 brands multi rep study + 91 brands single rep study
Sensory analysis:
• Bitterness intensity
• Multiple Replication study: data for model building
• Partial Replication study: data for model testing
OREGON STATE UNIVERSITY
4.0
0
4.5
5.0
5 5.5
6.0
10 6.5
7.0
15 7.5
ABV (%)
8.0
Alpha (mg/L)
20 8.5
9.0
9.5
25
10.0
5
2.5
3.0
15
3.5
25 4.0
4.5
35 5.0
5.5
45 6.0
RE (%)
6.5
Iso (mg/L)
55 7.0
7.5
65 8.0
8.5
75
9.0
3.8
0
4.0
10 4.2
20 4.4
30 4.6
4.8
pH
40
5.0
50
5.2
60 5.4
Humulinones (mg/L)
70 5.6
5.8
120
200
Chemistry of beers in commercial survey
280
360
440
OREGON STATE UNIVERSITY
520
TPP (mg/L)
600
Multi rep
Single rep
680
Bitterness comes from Isos & Humulinones
BU predicts bitterness 20 20
18 18
16 16
14 14
12 12
10 10
8 8
6 6
4 4
2 2
0 0
0 20 40 60 80 100 120 0 20 40 60 80 100 120
(Isohumulone + Humulone) (mg/L) Bitterness Unit OREGON STATE UNIVERSITY
Bitterness comes from Isos & Humulinones
BU predicts bitterness 20 20
20 20
18 18
16 16
14 14
12 12
10 10
8 8
6 6
4 4
2 2
0 0
0 20 40 60 80 100 120 0 20 40 60 80 100 120
(Isohumulone + Humulone) (mg/L) Bitterness Unit
OREGON STATE UNIVERSITY
Bitterness comes from Isos & Humulinones
BU predicts bitterness
Hahn, C, Lafontaine, S.R., Pereira, C.B. and Shellhammer, T.H. 2018. Evaluation of the
Nonvolatile Chemistry Affecting the Sensory Bitterness Intensity of Highly Hopped
Beer, Journal of Agricultural and Food Chemistry
OREGON STATE UNIVERSITY
HOP CREEP
Typical fermentation, no dry-hopping
1.050
1.045
1.040
1.035
Density (g/m3)
1.030
1.025
1.020
1.015
1.010
1.005
0 2 4 6 8 10 12
Days after start of fermentation OREGON STATE UNIVERSITY
Dry-hopping can create “Hop Creep”
1.050
1.045
1.040
Dry hop addition
1.035
Density (g/m3)
1.030
1.025
1.020
1.015
1.010
1.005
0 2 4 6 8 10 12
Days after start of fermentation OREGON STATE UNIVERSITY
Cascade hops have broad (low) enzyme activities
Enzyme Hops Malt (130 dp)
α-amylase 0.35 198
β-amylase 0.41 13
Amyloglucosidase 0.02 NA
Beer
Beer + Yeast
3
2.5
2
Beer + Yeast + Hops
1.5
0 10 20 30 40
Days OREGON STATE UNIVERSITY
Hop Creep & Diacetyl issues
1.055 700
1.050
600
1.045
1.040 500
Diacetyl (ppb)
1.035
Density (g/m3)
400
1.030
300
1.025
1.020 200
1.015
100
1.010
1.005 0
0 5 10 15 20 25
Days after start of fermentation OREGON STATE UNIVERSITY
Hop Creep & Diacetyl issues
1.055 700
1.050
600
1.045
1.040 500
Dry hop addition
Diacetyl (ppb)
1.035
Density (g/m3)
400
1.030
300
1.025
1.020 200
1.015
100
1.010
1.005 0
0 5 10 15 20 25
Days after start of fermentation OREGON STATE UNIVERSITY
HOP ENZYMES PERSIST
IN PACKAGED BEER
Enzyme action during production and
post-packaging
• Fresh
Finished beer • Force aged (3 days @ 37°C)
samples
• 3 months 25C (packaged 3 months earlier)
8 0.30
7.63%
7.5
0.25
6.5
0.15
6
0.10
5.5
5.11 °P
5 0.05
8 0.30
7.5
0.25
Maltose
5 0.05
4.5 0.00
Pre- dry hop Pre- second dry 24 Hours after 48 hours after 72 hours after Fresh Force Aged 3 Months
addition hop addition 2nd dry hop 2nd dry hop 2nd dry hop
8 0.30
6.5
0.15
6
0.10
5.5
5 0.05
4.5 0.00
Pre- dry hop Pre- second dry 24 Hours after 48 hours after 72 hours after Fresh Force Aged 3 Months
addition hop addition 2nd dry hop 2nd dry hop 2nd dry hop
8 0.30
7.5
0.25
7
6.5 batch,
stored at 0.15
6 brewery
0.10
5.5
5 0.05
4.5 0.00
Pre- dry hop Pre- second dry 24 Hours after 48 hours after 72 hours after Fresh Force Aged 3 Months
addition hop addition 2nd dry hop 2nd dry hop 2nd dry hop
0.45
8
0.40
7.5
0.35
7
6.5 0.25
0.20
6
0.15
5.5
0.10
5
0.05
4.5 0.00
* Fresh 2 Month (cold) 3 Day Force Aged 7 Day Force Aged