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Flavoring Beverages:
Opportunities and Challenges
October
Andrew G. Lynch, Ph.D.
Quest International
Global Citrus Applications Manager
2005
andrew.lynch@questintl.com
What is Food Science ?
Food Science deals with the physical, chemical and biological
properties of food. Food Scientists are concerned with:
Nutrition and Safety
Stability
Processing and Packaging
Cost and Quality
There are very few things as personal as food!
flavoring beverages
•background
•opportunities
•challenges
•citrus flavor stability
•orange juice processing
•clouds
•milk & coffee drinks
Quest for creative difference
key facts
• creative leader in the industry
• corporate headquarters in Naarden, the
Netherlands
• two businesses: Flavours and Fragrances
• total sales US$ 1.1 billion (2003)
• creative and application centres and production
facilities across Europe, the Americas and Asia
Pacific
• approx. 3,500 employees
Quest for creative difference
sales 2003: US$ 1.1 billion
60% flavours
40% fragrances
flavoring beverages
•background
•opportunities
•challenges
•citrus flavor stability
•orange juice processing
•clouds
•milk & coffee drinks
opportunities - North American beverage market
Projected
Sales 2003 ($ billion) CAGR (04-07)
22.5
38
20.0
34
17.5
30
15.0
26
12.5
24
10.0
20
7.5
16
5.0
12
2.5
8 0.0
4 - 2.5
0 - 5.0
Carbonates Still Flavored Flavored Juices RtD Tea, Powder Sports &
Drinks Alcoholic Bottled & Nectars & RtD Beverages Energy
Beverages Water Coffee Drinks
opportunities
market trends
diet (low carbohydrate, low calorie)
healthy fats (shift from trans and hydrogenated fats)
shift from fanciful to more exotic natural flavor
e.g. Blood orange instead of orange
masking, suppressing & smoothing
innovative beverages
opportunities
non-alcoholic beverage segment new launch top flavors 2004
citrus flavors top the list, moving strawberry from #1 2003 to #3
in 2004. cranberry and chocolate are new to the list.
1. lemon
2. orange
3. strawberry
4. chocolate
5. apple
6. peach
7. mango
8. raspberry
9. vanilla
10. cranberry
Source: Global New Products Database (Mintel)
opportunities
obesity
Obesity in the US is truly an
epidemic. In the last 10 years,
obesity rates have increased by
more than 60% among adults.
percent
Source: World Health Organization 2003
opportunities
masking and suppressing
• bitterness
(soy, grapefruit, protein drinks, coffee)
• sourness
(coffee, fermented and acid products)
• saltiness
(iso-tonic applications)
• artificial sweetener
(low cal products, lingering aftertaste, lack of body)
opportunities
enhancement
• sweetness
sugar flavors
• aromatics beyond drinking
odor release prior to consumption, instant
teas & coffees
• visual
• taste modification
opportunities
innovation in beverages
• dairy-based beverages
• soy and juice combination drinks
• meal replacement (juice/cereal/yogurt)
flavoring beverages
•background
•opportunities
•challenges
•citrus flavor stability
•orange juice processing
•clouds
•milk & coffee drinks
challenges
• packaging
• regulatory
• consistent quality of natural ingredients
• stability
• processing
• flavor stability
• physico-chemical stability
challenges
regulatory
• GMO
• natural & artificial
• kosher
• nature identical
• global customers
• globalization of flavors
• Halal
• TTB (formerly BATF)
challenges
consistent quality of natural ingredients
• natural products have natural variation
• focused quality assurance program is critical
• catastrophe in one part of the world? Example: 2004 Florida
hurricanes significantly damage grapefruit crop
challenges
processing
• consistency in scale-up & transfer to other regions
• processing impact on flavor/cloud
hot fill vs. cold fill
oxygen control
challenges
flavor degeneration
• fading
• light induced degradation
• acid hydrolysis
• oxidation
flavoring beverages
•background
•opportunities
•challenges
•citrus flavor stability
•orange juice processing
•clouds
•milk & coffee drinks
challenges
citrus flavor stability
• oxidation of terpenes
• citral in aqueous low pH
• acid catalyzed hydrations
Source: Rouseff, R. and Naim, M. 2000. Citrus Flavor Stability. In: Flavor
Chemistry, ed. By Risch, S.J and Ho, C.T. American Chemical Society. Pages
101-121.
challenges
citrus stability demonstration
soda base
pH 2.7
Brix 10.6
Carbonation 7 g/L
Good oxygen control
storage conditions
2 weeks at 4°C and 2 weeks at 45 °C
challenges
typical off flavor formation in acidic aqueous solution
challenges
off flavor formation in lemonade stored at high ambient temperatures
challenges
sensory analysis of aged lemonades
bitter deteriorated
3.5
3
2.5
2
1.5
1 0.5
barny 0 moldy
Control 4°C
Control 45°C
metallic oxidized
challenges
lemon flavors
less off flavors
increased shelf life
traditional citrus favorites
citrus flavors that deliver
with authentic taste profiles
flavoring beverages
•background
•opportunities
•challenges
•citrus flavor stability
•orange juice processing
•clouds
•milk & coffee drinks
Orange Juice Processing
• Oranges are processed to make not from concentrate
(NFC) or frozen concentrated orange juice (FCOJ)
• Quality must be controlled (variety, growing conditions, etc)
• Processing must be closely controlled to:
• Deactivate enzymes
• Limit oxygen levels
• Destroy pathogenic and spoilage microorganisms
• Minimize chemical and flavor changes
• Correct packaging and storage conditions must be used to
deliver safe and stable product to consumers.
Cross section of Orange
Juice vesicles
Flavedo
Albedo
Oil glands
Citrus Materials: Basic Processing
Overview of Production of Orange Juice Concentrate
Main Products By-Products
Fruit Reception Juice Extraction Peel Oil Recovery
Clarification
Peel Oil
Pasteurization Past/Evaporat
NFC OJFC
Bulk Transportation
Essence Recovery
Reprocessing
Oil Phase
Packaging Water-Phase Aroma
Distribution
Pulp, Limonene,
Citrus Pulp Pellets
Why does juice need to be pasteurized ?
(1) Enzyme deactivation
• Deactivation of pectin methyl esterase (PME)
• PME cleaves methyl groups from pectin causing cloud loss and gelation
• Calcium (from the juice) interacts with the demethylated pectin
• Calcium pectate is insoluble and settles at the base of the container
• For Florida-grown Valencia oranges, a heat load of 2-3 D values is
generally sufficient for total enzyme destruction.
• Typically pasteurization conditions employed are 95-98C for 10-30 secs.
Why does juice need to be pasteurized ?
(2) Ensure a microbiologically stable product
• Main micro-organisms of interest in OJ are:
• Acid-tolerant bacteria, yeasts and moulds
• Acid-tolerant bacteria, e.g., Lactobacillus plantarum (grow best at 20-37C)
• Spoilage characterized by diacetyl (buttery) off-notes and CO2
• Saccharomyces cerevisiae is the most common spoilage microorganism
• Spoilage characterized by alcoholic fermentation, off-flavors and CO2
• Spore-forming microorganisms (thermo-resistant acidophilic bacteria)
• In 1992, Alicyclobacillus classified as new genus
• Spoilage characterized by an off-flavor like “disinfectant” or guaicol
Thermal processing of OJ
• Thermal resistance of microorganisms is traditionally expressed in terms
of D values and Z values.
• D value is the time at a specified temperature for the microbial population
to decrease by 90% or one log cycle (also called the decimal reduction time)
• Z value is the change in temperature needed to alter the D value by
one log cycle
• For example, if an organism has a z = 10C and a D80C = 1 min,
then the D90C = 0.1 min and the D70C = 10 min.
Thermal processing of OJ
• Pasteurization destroys most vegetative microorganisms but has little effect
on bacterial spores (Most spores do not grow < pH 4.5).
• long term survival of some pathogens in unpasteurized refrigerated juice is
possible, therefore pasteurization is recommended
• For microorganisms usually found in fruit juices, z values are typically 5-7.
• Typical pasteurization temperatures are 75-95C for 15 to 30 secs
• For a given increase in temperature, the rate of destruction of microorganisms and
enzymes increases faster than the rate of destruction of sensory and nutrient
components.
• Summary……Deactivate enzymes, Ensure microbiological safety and
minimize heat damage to nutrient and flavor components.
Theoretical thermal destruction curves of pectin methyl esterase,
ascospores and vegetative cells of Saccharomyces cerevisae in
orange juice (The Orange Book, Tetra Pak)
challenges
packaging
• trend towards less glass and increased use of
polypropylene and PET (polyEthyleneTerephthalate)
• scalping
(loss of flavor into the packaging material)
• permeation
(movement of compounds through packaging materials)
• migration
(movement of components of the packaging material into
food product)
Source: Risch, S. 2000. Flavor and packaging interactions. In: Flavor Chemistry, ed. By
Risch, S.J and Ho, C.T. American Chemical Society. Pages 94-100.
Barrier properties
Off-flavor formation
Oxygen oxidation
Flavor
Flavor fading (scalping, permeation)
Permeation rate = Diffusion x Solubility
P=DxS
Vitamin C stability in different package types
(The Orange Book, Tetra Pak)
AA + ½ O2 = DHA + H20
AA = ascorbic acid (vitamin C), DHA = dehydroascorbic acid
Properties of different polymers: P = D x S
Polar polymers: PET, ethylene vinyl alcohol (EVOH) and polyamide (PA)
show very slow diffusion coefficients with polar and non-polar aroma
compounds.
Non-polar polymers: low density polyethylene (LDPE), high density
polyethylene (HDPE) and polypropylene (PP)
Limonene (non-polar aroma compound) has a high solubility in all the non-
polar polymers and diffusion and consequent permeation rates differ by
orders of magnitude in the different polymers – in decreasing order
LDPE > HDPE > PP
Ethyl butyrate (polar aroma compound) has low solubility in non-polar
polymers. Losses of polar molecules are negligible with this type of barrier.
Terpenes: the largest single chemical class within citrus volatiles
*Three month study of orange juice in Tetra-Pak laminated containers showed:
(a) Significant loss of limonene due to absorption/scalping by polymer barrier
(b) a-terpineol (formed from degradation of limonene) increased more rapidly
at higher storage temperatures
*Duerr et al., Alimenta 1981, 20, 91-93
Volatile contribution to orange juice aroma
Contribution to typical aromas Contribution to off-notes
Important Desirable Precursors Detrimental
ethyl butyrate linalool linalool a-terpineol
neral limonene limonene carvone
geranial a-pinene valencene t-carveol
valencene 4-vinyl guaiacol
acetaldehyde 2,5-demethyl-4-
hydroxy-3-(2H) furanone
octanal
nonanal
a-sinensal
b-sinensal
flavoring beverages
•background
•opportunities
•challenges
•citrus flavor stability
•orange juice processing
•clouds
•milk & coffee drinks
challenges
clouds
• provides turbidity to a beverage; visual enhancement that gives
finished beverage more value
• many different types of cloud systems
• weighting agents in clouds are regulated
• sucrose acetate isobutyrate (SAIB)
• brominated vegetable oil (BVO)
• ester gum
• blended systems
challenges
clouds
Neutral cloud
Goal: cloud with minimal taste impact
Most made from orange terpenes
Vegetable oil as an alternative
• typically less stability
• cleaner taste
challenges
cloud ringing
emulsion in beverage product breaks down giving rise to creaming
perform tests to predict stability
• make assumptions for predictions
• microscope, particle size analyzer, shelf-life studies etc.
challenges
cloud ringing
Stokes Law:
V = 2gr2 (po-p)
9no
v = velocity
r = droplet radius
g = gravity
po - p = difference in density
no = viscosity
v = negative creaming
v=0 stable cloud
v = positive sedimentation
challenges
cloud ringing
ringing
stable
phase separation,
shrinkage of cloud layer
flavoring beverages
•background
•opportunities
•challenges
•citrus flavor stability
•orange juice processing
•clouds
•milk & coffee drinks
milk-coffee RTD challenges
matrix complexity
milk-coffee drinks contain coffee, milk,
sweeteners, flavors, salts, hydrocolloids, proteins,
emulsifiers amongst other components
complex mixture of ingredients
physico-chemical and flavor stability issues
(processing and storage)
Milk coffee RTD matrix
Milk coffee RTD matrix
Coffee
Black Fresh whole milk Specialty proteins Alternative systems
Coffee Fresh skimmed milk
Skim/whole milk powders
Caseinate
Clouds
Whey proteins
Others Others
Dairy/non-dairy fat with milk flavour
Effect of heating, antioxidants, pH, O 2 content, stabilizing salts,
Processing
homogenization etc.
R&D Application, Sensory & Flavour expertise Emulsifiers, Proteins
Hydrocolloids
Beverages with improved stability & fresher coffee flavour
milk-coffee RTD opportunities
consumption
coffee consumption is growing
2.5 billion liters of canned coffee are
consumed annually in Japan alone!
served hot during winter & cold in summer
beverage manufacturers are adopting coffee
house trends into RTD‟s
milk-coffee RTD challenges
flavor complexity
• coffee contains over 830 volatile components!
• some of the key flavor components responsible for fresh
roast coffee character are:
• 2-furfurylthiol
• coffee aroma and taste is dependent on the type of coffee used
• species: Arabica or Robusta
• origin
• degree of roasting
milk-coffee RTD challenges
flavor complexity
at temperatures > 60°C, acidity increases, sourness increases and
volatiles are lost resulting in an unpleasant drinking experience
milk is added to coffee for:
appearance
taste
mouthfeel
LC Fractionation of Arabica Coffee (filtered brew)
milk-coffee RTD challenges
flavor complexity
• coffee flavors are needed to compensate for the damage to the coffee
volatiles during the extraction and beverage processing stages
• fruity (eg. acetaldehyde)
• phenolic (eg. guaiacol)
• earthy (eg. 2-ethyl-3,5-dimethylpyrazine)
• roast (eg. 2-furfurylthiol)
• sweet (eg. methylpropanal)
• opportunities for flavored coffees include;
• vanilla • amaretto and almond
• Irish Cream
• chocolate and caramel
• coconut
• macadamia Nut and Hazelnut • fruit flavors eg.
orange & raspberry
The composition of milk
CONSTITUENT RANGE % MEAN VALUE %
Water 85.5 – 89.5 87.0
Total solids 10.5 – 14.5 13.0
Fat 2.5 – 6.0 4.0
Protein 2.9 – 5.0 3.4
Lactose 3.6 – 5.5 4.8
Minerals 0.6 – 0.9 0.8
Main fatty acids of milk fat
% OF TOTAL FATTY MELTING
CONSTITUENT
ACID CONTENT POINT °C
Butyric 3.0 – 4.5 –7.9
85.5 – 89.5
Caproic 1.3 – 2.2 –1.5
Caprylic 0.8 – 2.5 16.5
Capric 1.8 – 3.8 31.4
Lauric 2.0 – 5.0 43.6
Myristic 7.0 – 11.0 53.8
Palmitic 25.0 – 29.0 62.6
Stearic 7.0 – 13.0 69.3
Oleic 30.0 – 40.0 14.0
Linoleic 2.9 – 3.1 –5.0
Distribution of the major constituents of the casein micelle
between the serum and micellar phases of bovine milk at pH
6.7 at 20°C
MICELLAR PHASE SERUM PHASE
COMPONENT
(g/l) (g/l)
as1-Casein 10.9 0.7
85.5 – 89.5
as2-Casein 3.0 0.1
b-Casein 9.0 1.3
k-Casein 2.9 0.5
Calcium 0.8 0.4
Phosphate 0.9 1.1
Citrate 0.1 1.8
Some physico-chemical characteristics of casein micelles
CHARACTERISTIC AVERAGE VALUE
Diameter 130-160 nm
Surface area 8.0 x 10-6 cm2
Volume 2.1 x 10-5 cm3
Mass 2.2 x 10-15 g
Density (hydrated) 1.0632 g/cm3
Water content (hydrated) 63%
Hydration 3.7 g H2O/g protein
Voluminosity 4.4 cm3/g
Zeta potential (at 25°C) –18.7 0.3 mV
Particle weight (hydrated) 1.3 x 109 Da
Particle weight (dehydrated) 5 x 108 Da
No. of monomers (av MW 25,000) 5 x 103
Schematic representation of a sub-micelle (A) and a
casein micelle (B) composed of sub-micelles (from
Schmidt, 1982)
Possible reactions of side-chain residues
of proteins at high temperatures – 1
1. -CH2-CONH2 + H2O -CH2COOH + NH3
Asparagine Aspartic acid
2. -(CH2)2-CONH2 + H2O -(CH2)2-COOH + NH
Glutamine Glutamic acid
3. -CH2-O-PO32- + H2O -CH2-OH + HPO42-
Phosphoserine Serine
4. -CH2-O-PO32- =CH2 + HPO42-
Phosphoserine Dehydroalanine
5. -CH2-SH + OH- -CH2-S- + H2O
Cysteine
6. R1-CH2-S-S-CH2-R2 R1/R2-CH2-S-
R3-CH2-S- R3-CH2-S-S-CH2-R1/R2
Possible reactions of side-chain residues
of proteins at high temperatures – 2
7. -CH-S- + -S- -CH2-S-S-CH2
CH2- Cystine
Cysteine
8. -CH -S-
2
=CH2 + HS-
Cysteine Dehydroalanine
9. =CH2 + HS-CH2- -CH2-S-CH2
Lanthionine
10. -(CH ) -NH + + H C + OH- -(CH2)4- +NH-CH2- + H2O
24 3 2 Lysinoalanine
Lysine
11. -(CH ) -NH + + -O C-CH -(CH2)4-NH-CO-CH2 +
24 3 2 2 H2O + e-N-(B-aspartyl)lysine
Lysine Aspartic acid
12. -(CH ) -NH + + -O C-(CH ) - -(CH2)4-NH-CO-(CH2)2- +
2 4 3 2 22
Lysine Glutamic acid H2O + e-N-(g-glutamtyl)lysine
Browning (Maillard) reactions in milk
in milk the main Maillard reactants are lactose and lysine
the rate of Maillard reaction in milk is dependent on pH, time,
temperature and water activity
some of the compounds identified from „dry‟ extracts of milk
systsems incubated at pH 6 or 7 and water activity 0.75 to
0.80 included: 5-hydroxymethyl-furfural, furfuryl alcohol,
furfural, maltol, acetol, 2-oxo-proponal, acetaldehyde, and
formic, acetic, propionic, butyric and lactic acids
Heat stability versus pH curves
for normal skim milk heated at 140°C
HEAT COAGULATION TIME (HCT) (min.)
50
40
maximum
30
milk A milk B
20
minimum
10
0
6.2 6.4 6.6 6.8 7 7.2
pH
Changes which can occur to milk constituents on heating – 1
calcium and phosphate are converted from soluble to
colloidal state
formic acid and lactulose are formed from lactose at
temperatures > 100°C
hydrolysis of the phosphoserine residues at high
temperatures
the titratable acidity of the milk increases and pH
decreases
solubility of the whey proteins decreases significantly at
temperatures > 75°C
Changes which can occur to milk constituents on heating – 2
enzymes are inactivated by heating at > 50°C, but varies
with enzyme
there is a decrease in redox potential probably due to the
formation of free sulphydryl groups and hydrogen sulphide
formation at temperatures > 60°C
Maillard reactions increase as temperature of heating
increases
casein micelles may start to aggregate above 110°C
lactones and methyl ketones are formed from the fat
Alkaline urea-PAGE of solutions of sodium caseinate
heated at different pH values and temperatures.
as1-casein
as2-caseins
Alkaline urea-PAGE of
unheated sodium
b-casein caseinate (1); sodium
caseinate, pH 7, heated
at 110°C (2), 120°C (4),
k-casein of 130°C (6) for 5 min.
and sodium caseinate,
g-casein pH 10.0, heated at
110°C (3), 120°C (5)
or 130°C (7) for 5 min.
Lynch, Andrew, Ph.D thesis,
NUI, Cork, Ireland, 1995.
1 2 3 4 5 6 7
milk-coffee RTD challenges
preparation of milk-coffee beverages
Coffee-milk mixtures usually have near neutral pH values and careful
processing is required to ensure a stable product with good organoleptic
properties
• controlled temperature & duration of heating during coffee extraction
• homogenization is required if milk fat or other fat is used
• sufficient amount of surface active material must be present
• check coffee-milk/ingredient and flavor compatibility
• pH of the mixture needs careful control
• sterilization/UHT processing is required for long shelf-life products
milk-coffee RTD challenges
why homogenize?
under homogenization optimum homogenization
milk-coffee RTD challenges
emulsion stability
OIL
Creaming Aggregation Coalescence
creaming separation
Reversible Irreversible
STABLE UNSTABLE
milk-coffee RTD challenges
droplet stabilitly
close approach of
droplets
steric stabilization
coalescence interfacial film
rupture
interfacial rheology
no interfacial film
rupture
flocculation
Emulsifiers
Surface active molecules
Contain water-loving hydrophilic part and oil-loving
lipophilic part
Reduce surface tension
Orientate at oil / water or air / water interface
Interact with other ingredients (e.g. protein, starch)
Emulsifiers : Chemical Characteristics
Iodine value unsaturated fatty acids
gram iodine absorbed per 100 g emulsifier
Peroxidase value oxidation level
meq. oxygen bound as peroxide per kg emulsifier
Acid value free fatty acids
mg KOH needed to neutralise 1 g emulsifier
Saponification value free + bound fatty
acids
mg KOH needed to saponify 1 g emulsifier
Composition of emulsifiers
Hydrophilic / Lipophilic Balance of Emulsifiers
Monoglyceride : Saturated
-o-
E
CO
- Fatty
OH acid
-
OH
GMP
(glyceromonopalmitate)
Sodium stearoyl-2-Lactylate
CH3
|
CH3 CHO CO
| |
CHO--CO Fatty
acid
| - +
COO (Na )
milk-coffee RTD challenges
effect of homogenization pressure on particle size distribution
flavoring beverages
•background
•opportunities
•challenges
•citrus flavor stability
•orange juice processing
•clouds
•milk & coffee drinks
Flavoring Beverages:
Opportunities and Challenges
A.G. Lynch
