Implementation of Hazard Analysis Critical Control Point HACCP System To The Alcoholic Beverages Industry
Implementation of Hazard Analysis Critical Control Point HACCP System To The Alcoholic Beverages Industry
Implementation of Hazard Analysis Critical Control Point HACCP System To The Alcoholic Beverages Industry
ABSTRACT
Alcoholic beverages (fermented or not) have been consumed for more
than three thousand years and, generally, they have been considered safe because
of their alcohol content. However, in recent years adulteration (i.e., use of lowcost, inappropriate alcohol) has made rapid progress in this field. Food and drink
control and safety can be assured within the frame of strict adherence to quality
and safety systems (ISO 9000 series, HACCP and TQM). The flow diagrams for
the production of several alcohol drinks were shown, and an extensive hazard
analysis critical control point (HACCP) analysis was carried out in order to
reveal the weaknesses of the production line and to suggest the critical limits
in compliance with legislation and the corresponding preventive and corrective
measures.
Key Words: HACCP; Alcoholic beverages; Hazard; CCP; Ouzo; Gin; Vodka;
Brandy; Distilled spirits; Wine; Sake; Beer.
INTRODUCTION
It has taken almost 30 years (since 1971 when it was officially presented for
the first time) for the concept of Hazard Analysis Critical Control Point (HACCP) to
become universally accepted as one of the most rigorous preventive programs whose
strict implementation can assure food safety (1,2). Although HACCP is a system
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aiming at zero defect products, it is well known that this is not feasible and the
real target is the minimization of unacceptable unsafe products. When a company
decides to adopt HACCP it should be able to set controls at each point of the
production line at which safety problems (physical, chemical, and microbiological)
are likely to occur (3).
Prior to initiating a HACCP system, a company must endeavor to put together
a HACCP plan, most often described by the five following steps (1,3,4,5): a) identify
HACCP resources and assemble the team, b) describe the food and its distribution
method, c) state clearly intended use and consumers, and d) develop a process flow
diagram and e) verify the validity of this diagram in practice (operation).
The regulatory requirements for Sanitation Standard Operating Procedures
(SSOPs) in conjunction with Good Manufacturing Practices (GMPs) should also
be considered as a prerequisite to HACCP. The following seven HACCP principles
constituting the major steps to writing an HACCP (6,3,7):
1. Conduct a hazard analysis
2. Identify critical control points (CCPs) by applying the HACCP decision
tree (8, Fig. 1)
3. Establish critical limits (CLs) for each CCP
4. Establish monitoring actions
5. Establish corrective actions
6. Establish record-keeping procedures
7. Establish verification procedures
Today, HACCP is continuously gaining importance and worldwide acceptability, being implemented by most countries all over the world. The implementation of
HACCP in the EU in particular was introduced by the Council Directives 91/43/93
and 92/5/92. HACCPs implementation is considerably facilitated when other complementary quality assurance systems (ISO 9001/2) are already in place (9). The
current tendency is integrating HACCP and ISO 9001 or ISO 9002 (10,11) within
the frame of Total Quality Management.
Since the two most important stages for the drink industry are fermentation
and bottling, where hazards are likely to occur, special care is required (trained
personnel, sanitation, equipment maintenance, GMP).
This review article aims to present an overview of HACCP implementation to
alcoholic beverages through the production and distribution chains and to pinpoint
the current CCPs, CLs and preventive and corrective actions due to be undertaken
in case any deviations are observed.
BEER
Introduction
Beer is an alcoholic beverage produced by the fermentation of wort obtained
from barley malt flavored with hops. The alcoholic content of beer ranges from 4%
for ordinary beer up to 15%. Beers first production in Mesopotamia by the Sumerians in the 5th millennium B.C. classifies it among the most ancient of alcoholic
beverages. Towards the middle of the 3rd millennium B.C. there is documentary evidence of beer drinking by the Egyptians, who probably introduced beer technology
in Europe. Beer drinking in northern Europe dates back to early antiquity contrary
to the Mediterranean countries, in which wine was the commonest drink. A critical
point in its history was the works of Louis Pasteur, which greatly contributed to the
understanding of beer production (12).
Beer Main Production Stages
The main stages for beer production are shown schematically in Figure 2,
together with their critical control point (CCP) numbers.
Incoming Raw Materials (CCP1)
The principal raw materials used to brew beer, are water, malted barley, hops
and yeast. Barley is required to be of sufficiently good malting quality in order to
germinate and to produce a satisfactory product yield. Other factors such as dormancy and losses during malting have also to be considered (13). The malting or
subsequent brewing characteristics are subtly affected by the weather conditions
prevailing over the growing period. Some information regarding the quality of a
batch of barley can be obtained by visual inspection, but usually it is complemented
by analyses including moisture content, total nitrogen, 1000-grain weight and the
portion of nongerminating grain. The National Institute of Agricultural Botany
(UK) provides descriptions of the European malting varieties. Residues of certain
pesticides used on malting barley survive through to the final malt and wort and can
affect the process and quality of the end product (CCP). Fungicides and herbicides
influencing enzyme synthesis during malting process can accumulate in the yeast,
thereby affecting the next fermentation (14). The critical limits of these substances
are prescribed by Codex Alimentarius and are presented in Table 1. Presence of
heavy metals above the specifications of Directive 80/776/EC and mycotoxin production more than 0.04 mg/L, mainly from Fusarium species, such as aflatoxins,
ochratoxine A, zearoleon, deoxyniralenol, constitutes a high risk for human health
(CCP) (15). Temperature and relative humidity are two interacting parameters that
define the germination of spores of different microorganisms (16). Visual inspection and biological plate methods detect the fungal contamination; for mycotoxin
analysis employment of HPLC or ELISA is required (17).
The quality of the water used is a major factor affecting the beer quality
(CCP). The development of strict water control standards was introduced by most
breweries in which water is filtered through activated carbon as well as ion exchange resins to remove impurities (pesticides, herbicides and industrial wastes).
Two ions of particular importance in water are calcium and carbonate/bicarbonate,
which control the pH during brewing. Calcium also protects -amylase from heat
destruction, thereby permitting liquefaction of starch during mashing (18).
Hops not only provide bitter flavor to the beer but impart a hoppy character
as well. These aroma components are derived from the essential oil. The brewing
value of hops depends on the resin fraction which amounts to 15%, and the essential
oil, comprising 0.5%. Total resin is defined as the material soluble in both cold
methanol and diethyl ether; soft resin is that proportion of the total which is
soluble in hexane comprising mainly and -acids, while hard resin is insoluble
in hexane. The -acids that are the most significant bittering precursors can be
distinguished from other soft resins from their ability to form a lead salt which is
insoluble in methanol. The determination of moisture and seed content also provide
useful conclusions about their quality (13). Adjuncts of carbohydrate origin other
Incoming raw
materials
(CCP1)
Process Step
Efficient disease
management
system in use
Certified suppliers
Proper water
decontamination
Use of deioniser
Control of fungi
development,
temperature and
RH regulation
during storage
Certified suppliers,
schedule
inspections
Stricktly following
instructions
ControlPreventive
Measures
Hazards
(P, M, C)a
Waters electrical
conductivity
Heavy metals
presence
Presence of
Enterobacteriaceae
Contamination of
microbial
preparations
Pesticide residues
in barley, hops,
water
Within
specifications
prescribed in
Directive
80/778/EC
<20 ms/cm
By pesticide as
described by
Codex
100% clean
0.004 mg/L
Critical Limit
Mycotoxin
production
CCP Parameter
Continuous
recording of
deioniser
Specific chemical
analyses
Visual inspection
of fungi
development
HPLC, ELISA,
EPS analysis
Microbiological
analysis
Monitoring
Procedures
Automatic
discontinuation
of deioniser,
analysis of water
samples
Rejection of
specific batch
De-metallisation step
Rejection of
specific batch
Change supplier
Change
preparation
method
Rejection of
specific batch
Rejection of
specific batch
Corrective
Actions
Responsible
Personnel
Quality
control
manager
Quality
control
manager
Table 1. Summary of Hazards, CCPs, CLs, Monitoring, Corrective Actions, and Personnel Responsible for Beer Production
6
KOURTIS AND ARVANITOYANNIS
Lautering
(CCP4)
Boiling
(CCP5)
Fermentation
(CCP6)
Schedule
Inspection, under
plate cleaning
Correct use of
boiler treatment
chemicals
Aeration of wort,
use of yeast for
max 6
generations
Control of
temperature, CIP
Proper hadling
operations after
production
Use of indirect
heating systems,
control low-NOx
burners
Control of time,
temperature and
RH
Mashing
(CCP3)
Malting
(CCP2)
Poor yeast
viability, stuck
fermentation
<20 ppb
2.5 ppb
None
0.004 mg/L
Specified by
particular plant
2.5 ppb
Contamination
with detergents
NDMA
production,
detergent
residues
ATNC
Mycotoxin
production
NDMA production
during kilning
Yeast
concentration,
fermentability,
O2 concentration
in the wort
Microbiological
and chemical
analyses
CIP system
Continuous
checking the
area, specific
analyses
Continuous
monitoring of
processing
conditions
Visual inspection
of fungi
development,
HPLC, ELISA,
EPS analysis
Continuous
recording of the
processing
Quality
control
manager
Rejection of
specific batch
Increase
propagation
frequency, wort
aeration
Proper maintain,
re-lautering of
the batch,
Repair CIP, batch
rejection
(continued )
Quality
control
manager
Quality
control
manager
Quality
control
manager
Quality
control
manager
Quality
control
manager
Adjust lautering
program
Quality
control
manager
Rejection or
mixing with
other batches
Bottle/can
sealer
(CCP10)
Bottle/can
pasteurization
(CCP11)
Running
pasteuriser
according to
program
Certified supplier,
proper handling
of bottles
Installation of
controlling
equipment on the
CIP system
Correct installation
of equipment
Bottle/can
inspector
(CCP8)
Bottle/can
filler
(CCP9)
Use CO2 ,
prefilling of filter
with water
GMP
Filtration
(CCP7)
Inspection of CIP
system and
equipment
ControlPreventive
Measures
Fermentation
(CCP6)
Process Step
Hazards
(P, M, C)a
Oxidation caused
of wrong
temperature-time
set
Blow-off effect
Cleaning
performance
O2 uptake
Lactobacilli, acetic
acid bacteria
and wild yeasts
CCP Parameter
Occurrence
reduced to an
acceptable level
Max. 65 C for
20 min, quick
cooling at the
exit
Continuous on-line
time-temperature
checking
Organoleptic
examination of
filled bottles
Complete absence
Cracks/scratches
absence
Elaborate
electronic
recognition
systems after
CIP
On-line visual
control
Plate count
method, or a
rapid detection
method
Measurement of
dissolved O2
Monitoring
Procedures
No solids, no
liquid remnants
>0.2 ppm
dissolved O2
Presence in 1 mL
plate +1 mL
actidione
Critical Limit
Table 1. Continued.
Automatic removal
of destroyed
bottles
Adjust
temperature,
maintain
equipment
Batch rejection
Rejection of faulty
bottles
Proper disinfection
of equipment,
reprocessing of
the batch
Survey of filtration
for increased O2
pick up
Rewashing of
bottles, CIP
system
inspection
Corrective
Actions
Technical
manager
Trained
personnel
Trained
personnel
Trained
personnel
Quality
control
manager
Quality
control
manager
Quality
control
manager
Responsible
Personnel
8
KOURTIS AND ARVANITOYANNIS
Control storage
conditions
Absence of rifts in
the lute, crack or
scratches
Specified by the
particular plant
Bottles condition
during
palletisation
Organoleptic
condition of beer
Misplaced
etiquettes
Occurrence
reduced to an
acceptable level
Reduced to an
acceptable level
Physical damage
Storage (CCP15)
Correct installation
of the equipment
Careful selection
of the etiquettes
Regular inspection
of the machinery
Bottle/can
packaging
(CCP14)
Bottle/can
inspection
(CCP12)
Labeling
(CCP13)
Scheduled controls
of finished
product
Visual checks,
control of the
equipment
On-line visual
control
On-line monitoring
Trained
personnel
Technical
manager
Trained
personnel
Relabeling the
specific batch
Adjust the
equipment
parameters
(speed, pressure)
Adjust the
storehouse
conditions
Technical
manager
Equipment
standardisation
10
11
12
phenol analyses are all essential to avoid chemical contamination and taints development (23).
Clarification
Wort clarification is conducted either through sedimentation or filtration.
When whole hop cones are used, it is necessary to employ either a hop back or
a hop separatorfilter. The drop in hop usage and the widespread acceptance of
preisomerized extracts led to utilization of a vertical cylinder known as whirlpool,
which induces sustainable circulation of the trub collecting as a compact cone in the
base. Whirlpools are more suited to larger worts and can also be used with ale. In
modern breweries, centrifuges constitute a promising alternative to whirlpools (25).
Cooling
To prepare for fermentation, the clear hopped wort is cooled, usually in a
plate heat exchanger. During cooling, it is advisable to aerate or even to oxygenate
the wort, because next processing step involves yeast growth promoted in the presence of dissolved oxygen, despite the low dissolved oxygen concentration in wort
(714 ppm) (22).
Fermentation (CCP6)
Fermentation aims at producing ethanol by fermenting yeasts. Yeasts vary in
their behavior during fermentation; some strains tend to flocculate trap plug CO2 and
rising to the top, whereas others do not flocculate and precipitate. Several lagers are
produced by bottom fermentation, while many types of ales and stouts are produced
by top fermentation. Saccharomyces cerevisiae is usually the top fermenting yeast
in the range of 1822 C, whilst the bottom-fermenting are strains of Saccharomyces
uvarum that function in the range of 715 C (26). Therefore, the temperature at
which fermentation occurs is very crucial for the further stages of beer production.
The modern use of cylindroconical vessels has reduced the fermentation period
for ales and lagers from 7 to 2 or 3 days and from 10 to 7 days, respectively (27).
Fermentation is monitored by taking samples for measuring the specific gravity
and can be controlled by varying the cooling rate (20). Stuck fermentation where
the required ethanol level is not attained and microbial contamination with Lactic
acid bacteria, mainly Lactobacilii and Pediococcus, which cause taints during
maturation or in bottle storage (28) represent microbiological hazards, which are
the only hazard detected at this stage. Common causes for stuck fermentation
include premature yeast flocculation and yeast failure to metabolize maltotriose
due to repression by glucose (25). A minimum of 90% viable yeast cells (CL) can
be applied to ensure the development of the process. During fermentation the pH
13
drops from 5.2 to 4.2 and by its completion the yeast is removed either as a top or
bottom crop and retained to pitch the next fermentation. Apart from the conventional
microbial detection methods with plate count, several rapid detection methods
potentially applied in breweries, such as ATP bioluminescence, flow cytometry,
and polymerase chain reaction, have been developed to reduce the incubation time
from 34 days to 12 (29,30).
Maturation
Maturation includes all those changes occurring between the end of primary
fermentation to beer filtration (31). Ale is matured at relatively warm temperatures,
1220 C, while lagers are held under much cooler conditions. The warmer temperatures allow the rapid metabolism of any residual and priming sugars, as well as
loss of green flavors, within 12 weeks, depending on beer type, yeast strain, wort
composition, and primary fermentation conditions. In case of lager, the beer used to
be held at refrigerated temperatures for up to several months after fermentation, allowing formation of protein/tannin complexes (18). Today, the enzyme addition has
substantially shortened this process to several weeks, during which flavor matures.
Enzymes, such as papain, may be added during transfer between fermentation and
maturation tank. The dosage of the proteolytic enzyme varies depending on type
of beer and process. Enzyme activity decreases progressively during maturation
until its inactivation with pasteurization. Part of the enzyme absorbed in the yeast
surface is removed during filtration (19).
Filtration (CCP7)
Beer produced during fermentation is turbid and should be clarified prior to its
marketing. This turbidity is due to the presence of yeasts and proteinaceous materials associated with carbohydrates and polyphenols. The formation of these protein
precipitates is attributed to cold temperature, low pH and poor solubility in alcoholic
solutions (32). To prevent this from occurring in the final product, the beer may be
subjected to various chill-proofing treatments during its storage. These treatments
generally include the addition of clays to absorb the colloidal materials or proteolytic enzymes used to further solubilize the protein fraction (33). Since oxygen
uptake during this process could severely affect the product organoleptic characteristics, a CCP of dissolved oxygen should be applied with a CL of 0.2 ppm (34).
Packaging and Sealing
The packing section comprises several CCPs including the containers to be
used, their cleaning and disinfection (CCP8), the filler line (CCP9) and the sealer
(CCP10). The bursting pressure of the bottles, as guaranteed by the manufacturer
in his specifications for the new glass, may no longer be valid in case of reusable
14
bottles, due to the considerable physical stress during already exerted upon them
during the filling process. Insufficient cleaning of reusable bottles due to low temperatures and concentrations of the employed cleaning solutions, as well as presence of
extraneous entrapped materials within bottles and improper emptying, consist possible hazards. Moreover, cleaning solution remnants and shards introduced through
the procedure pose problems under working conditions. The beer filler may be contaminated by cleaning and disinfection solutions. Contamination sources may be
due to inadequate pressure or faulty CIP system resulting in cleaning and disinfecting solution remains in the pressure tank or the ring bowl of the filler (35,36). The
crown corker should be correctly installed; the filling pressure of bottle caps on the
mouths of the bottles should be adjusted to ensure a specified blow-off effect to
avoid bottle bursting. After filling, there should be a full bottle inspector detecting
glass particles in bottles or possible leakage (37).
Bottle Pasteurization (CCP11)
Pasteurization is carried out to ensure the beer shelf life over a period of
months. This is accomplished by the development of tunnel pasteurization in which
the beer bottle is subjected to 60 C for 20 min. Over-pasteurization, which causes
oxidation and can adversely affect beer flavor (38) is a potential physical hazard.
Furthermore, it is crucial to check the time-temperature procedure with adequate
corrective actions for assuring the production of a satisfactory product.
Bottle Inspection (CCP12)
Bottle inspection after the pasteurization step is important to ensure that bottles
have not been damaged during the process (39). Should such a situation occur, the
equipment has to be standardized by the production engineer.
Labeling and Standardization (CCP13)
Labeling of the package should comply with the requirements of the Codex
General for the labeling of prepackaged foods (40). This means that the name of the
product shall be clearly declared, there must be a list of ingredients in descending
order of proportion, no other fruit may be represented pictorially except those used,
and the date of minimum durability will be declared by the month and year in
uncoded numerical sequence.
Bottle/Can Packaging (CCP14)
Bottles (cans) are packaged into paperboard boxes of various sizes, according
to the bottle or can dimensions. The encountered hazards can be of physical nature
concerning the bottles (cans) condition during the procedure.
15
Storage (CCP15)
The finished beer undergoes chemical, microbiological and organoleptic analysis to ensure that its properties are within its specification range. A synoptical presentation of the occurring hazards, CCPs, CLs, and preventive corrective measures
is given in Table 1.
SAKE
Introduction
Sake is a fermented liquor made from rice and coming in many varieties
depending on the raw materials, manufacturing process and process after brewing
(41). According to the earliest records, sake was originally brewed from rice that
had been chewed to reach saccharification, followed by natural fermentation. Sake
brewed this way was used as a sacred wine in the worship of the Shinto gods. This
association with religion, Shintoism and Buddhism, has caused a deep intertwining
of sake with the traditions and social customs of Japan. Thus, today sake is served
at ceremonies and celebrations of all kinds (42). Sake has the highest alcohol
percentage by volume of any fermented beverage. In its natural, undiluted state, it
may contain a potent 20% ethanol compared to 35 % for beer or 912% for wine,
which may reach higher values for fortified wines (43,44). The central brewers
union divides sake into four basic flavor types, on four axes of sweet, sour, bitter
and umai. The latter is another translators nightmare, which generally ends up
translated as delicious. According to position established along these axes, sake
is considered to be of mature type, fragrant type, light and smooth type, or
full-bodied type (Fig. 3). However, no set of criteria can adequately express the
multiplicity of sensations that together create the flavor unique to any individual
sake, but there is a perceived need for terms which quickly and simply give the
general idea.
16
17
the bubble removal step, thus shortening the brewing period and reducing the cost.
Should the factory wish to employ a specific yeast, an adequate disinfection of
the building interior is required, otherwise undesirable bacteria may be introduced
which could prove hazardous to human health (CCP, microbiological hazard) (46).
Rice Polishing (CCP2)
The brown rice used for sake production must be first polished to remove the
outer portion of the grain, which contains fats, proteins, minerals and amino acids
that can cause unpleasant flavors, leaving the starch residues that are located in the
center of the grain. Nowadays, machines are programmed to automatically remove
whatever portion of the rice is required for the specific sake (47). The rice polishing
ratio (7335%) is expressed by the following formula (43):
Rice polishing ratio=(weight of white rice/weight of brown rice)100 (1)
The polishing process should be gently carried out, because friction results in
heat generation, thereby greatly affecting water absorption and rice grain structure.
Broken grains are unlikely to satisfactorily ferment (47). Maybe the most important
stage in sake production consists of yeast starter mash production, which can take
place either with the classical Kimoto or slightly revised Yamahai process, or with
the new high speed methods (48).
Washing (CCP3)
After the rice has been polished, rice powder clinging to the grain surface is
removed by washing. Washing can be carried out either mechanically or manually
(laborious hand washing) and should result in removing most of the organic and
inorganic impurities, reaching the CLs set by Codex Alimentarius of 1.5% and
0.1% m/m respectively.
Soaking (Steeping)
Soaking allows rice to absorb the desired amount of water that is crucial to
establishing the rice consistency. For sake produced en masse, simply dumping
into a vat overnight for as long as 14 h is a usual case (47). However, high polished
rice may be soaked within minutes. In such a case an error of a minute might prove
to have dire consequences for the end product (43).
Steaming (CCP4)
Steaming aims at softening the rice grains and breaking down the starch
molecules, thus encouraging the growth of Aspergillus oryzae and eliminating all
18
19
Table 2. Quantities of Ingredients at Each Stage of Mixing the Main Mash (Moromi)
Yeast
Starter (Moto)
1st
Addition
2nd
Addition
3rd
Addition
4th
Additiona
210
140
70
470
850
330
200
1470
650
240
1230
230
140
420
1010
2030
Total
1200
3000
2350
650
1200
360
405
Traditional brewers mix the final mash in three stages. The fourth addition of alcohol and water
is a controversial postwar development (Kondo, 1984).
20
set CLs. However, in recent years, refrigerated storage and transport have made
unpasteurized sake, with characteristic aroma, available to the consumer (43).
Dilution
The produced sake in its raw state (Genchu) contains more than 20% alcohol
by volume, but it is generally diluted to about 1516 vol.-%.
Bottling/Storage/Distribution
The applied procedures are similar to those mentioned for the beer production.
A summary of the occurring hazards, CCPs, CLs, and preventive and corrective measures is given in Table 3.
WINE
Introduction
Wines are made from the fruit of Vitis vinifera, of which there are a great
number of varieties growing in many parts of the world. The history of wine is
inextricably interwoven with human history. It might be as true to say that it was
with wine that civilization began, for the vine takes longer to mature than any other
crop, and does not produce grapes for wine making until its fourth year. It is not
exactly known when men first had wine, but it was accepted as a gift from the gods:
the Egyptians attributed it to Osiris and the Greeks to Dionysos. Mesopotamia and
the Caucasian slopes were no doubt early sources of wine from where it was spread
to Egypt and Greece and then to the rest of the world (52).
Wine Main Production Stages
The main stages for wine production are schematically presented in Figure 5.
Harvesting (CCP1)
Grape harvesting is a CCP comprising both physical and chemical hazards.
Physically, the grapes should be sound without rotten parts; otherwise oxidative
and microbial contamination can rapidly develop. Therefore, harvesting should
be conducted with the greatest possible care and an efficient disease management
system should be applied (53,54). Pesticides play an important role in pest management, but they should be handled with care because they constitute chemical
hazards (55). At the time of harvest, the grapes must have also reached the correct
maturity when Brix and Total Acidity (TA) levels indicate maturity of wine. Since
pesticide and fungicide residues on the surface of the berries constitute chemical
21
hazards, Oliva et al. (56) proposed a rapid and simple gas chromatographic method
for their determination. The maximum residue limits for pesticides in grapes and
wines are provided by Codex Alimentarius (45) and Organisation International du
Vin (57). Finally, the bulk bins used for grapes transportation, should be effectively
decontaminated to avoid any microbial infection.
Stemming
Stemming includes the removal of stem, leaves, and grape stalks before crushing. This procedure has several advantages because the total volume of processed
product drops by 30%, thus resulting in smaller tanks, and eventually increasing
the products alcoholic content (58). However, the end of fermentation and the alcohol content of finished product depend mostly on the Brix level of initial grapes.
Stemmers usually contain a perforated cylinder allowing berries to pass through
but prevent the passage of stems, stalks and leaves.
Crushing
Crushing typically immediately follows stemming, since some crushing of
the fruit occurs during stemming. The released juice is highly susceptible to oxidative browning and microbial contamination. The most common crushing processes
involve pressing the fruit against a perforated wall or passing the fruit through a set
of rollers. It is very important to avoid crushing the seeds to preclude contaminating the must with seed oils, the oxidation of which could produce rancid odors and
constitute an undesirable source of bitter tannins. Equally important is the proper
handling of product, because inappropriate timing might lead to a sudden start
of alcoholic fermentation and consequently to higher fermentation temperatures,
while a delay might cause microbial contamination and oxidative browning (59).
Maceration
Maceration is the breakdown of grape solids after crushing of grapes. While
maceration is always involved in the initial stage of red wine fermentation, the longstanding trend has been to limit maceration in white wine production. Temperature
and duration of maceration depend on grape and wine variety. Usually for white and
rose wines the maceration time is less than 24 h, red destined for early consumption
is macerated for 35 days and red for aging is macerated from 5 days to 3 weeks.
Fermentation usually occurs during this or at the end of maceration. The amount of
the antimicrobial to be used, usually added to white musts that are most sensitive to
oxidation, depends on the crop health and maceration temperature. Sulfur dioxide
has a distinct advantage over other antimicrobial agents, because of the relative
insensitivity of the wine yeasts to its action. However, it is also toxic, or inhibitory,
to most bacteria and yeasts (i.e., Candida, Pichia, Hansenula) at low concentrations
(60) and has a rather low retention capability after the clarification step (61).
Washing
(CCP3)
Steaming (for
unpasteurised
sake) (CCP4)
CCP Parameter
ControlPreventive
Measures
Rice polishing
(CCP2)
Incoming raw
materials
(CCP1)
Process Stepa
Hazards
(M, C, P)b
Set by the
specific plant
MRLs as
described by
Codex
Alimentarius
0.1% m/m
1.5% m/m
0.1% m/m
Absence of
pathogens
Specific batch
reprocessing,
CIP standardisation
Rewashing of
specific batch,
change supplier
Specific
examination
Microbiological
analysis
Rejection of
specific batch
Change supplier
Inspection of the
equipment
Rejection of
specific batch
Specific chemical
analysis
Microbiological
analysis
Evaluation of the
decontaminating
methods
Within
specifications
prescribed in
Directive
80/778/EC
100% clean
Corrective
Actions
Rejection of
specific batch
Change supplier
Monitoring
Procedures
Critical Limits
(CLs)
Quality
control
manager,
Trainned
personnel
Quality
control
manager
Quality
control
manager
Quality
control
manager
Quality
control
manager
Responsible
Personnel
Table 3. Summary of Hazards, CCPs, CLs, Monitoring, Corrective Actions, and Personnel Responsible for Sake Production
22
KOURTIS AND ARVANITOYANNIS
Running of
pasteuriser
according to
program
Certified supplier
Alcohol
addition
(CCP6)
Pasteurization
(CCP7 &
CCP8)
Heavy metal
presence
Pesticide residues
Microbiological
analysis
Detection of
yeasts, LAB
% enzymatic
activity
Quality
Demetallisation
control
Change supplier
manager
Rejection of
specific batch
Dilution with large
quantities,
machinery
modification
Quality
Rejection of
specific batch
control
manager
Quality
Temperature
control
adjustment,
manager
batch
Technical
reprocessing,
manager
proper
machinery
disinfection
Regarding the procedures of bottling, storage and distribution, the CCPs are similar to those mentioned in Table 1 for beer production.
M, C, P stand for microbiological, chemical and physical hazards, respectively.
GC examination
<0.5 g/L
Specific chemical
analysis
Specific chemical
analysis
Methanol content
GMP, use of
Residues of
0
nontoxic glycole
ehtylene glycole
& detergents
Material control,
GMP corrosion
checks
Fermentation
(CCP5)
24
Pressing
The must is allowed to remain in the press for several minutes, during which
juice runs out under its own weight. Depending on the press type (horizontal,
pneumatic, continuous screw presses), the produced juice and wine fractions vary
in terms of their physicochemical properties. Combining different wine fractions,
the winemaker can influence the character of the wine. However, a potential hazard
might be the occurrence of oxidation reactions if there is a delay in the process
(52).
25
26
Malolactic Fermentation
Early onset and completion of malolactic fermentation allows the prompt addition of sulfur dioxide, storage at cool temperatures, and clarification. It is conducted
by lactic acid bacteria (Oennococcus oenos), which directly decarboxylate L-malic
acid (dicarboxylic acid) to L-lactic acid (monocarboxylic acid). This metabolism
results in acidity reduction and pH increase, which are in turn related to an increased smoothness and drinkability of red wines but might also generate a flat
taste (68,69). The initial pH, the sulfite concentration (70), the phenolics and the
anthocyanin content (71) of juice/wine strongly affect whether, when, and how
(with what species) malolactic fermentation will occur. Bacterial viruses (phages)
can severely disrupt malolactic fermentation by attacking the Oennococcus oenos
cells, thus causing microbial destabilization of wine (72). Therefore, to assure the
development of malolactic fermentation, winemakers inoculate the wine with one
or more strains of Oennococcus oenos (CCP3) (73,74). After fermentation, the
wines desirable total acidity is generally considered to vary within the range of
0.550.85% (white and red wines toward the upper and lower end, respectively).
Whenever, the total acidity surpasses those limits, acidification and deacidification
techniques should be in place (35).
Maturation (CCP4)
The maturation step often lasts 624 months and takes place in oak barrels.
During maturation a range of physical and chemical interactions occurs among the
barrel, the surrounding atmosphere, and the maturing wine, leading to transformation of flavor and composition of wine (75). Here there is a CCP concerning the oak
barrel, which should be fault-free and should have undergone a decontamination
treatment. The wood also must be free of pronounced or undesirable odors, which
could taint the wine (76). During the maturation period, several components of the
wood (most of them phenolics) are extracted to the wine tannin (77,78). Since oak
tannins can significantly add to the bitter taste of wine, white wines are usually matured in oak for shorter periods than red wines, and in conditioned barrels to release
less extractable (79,80). Another CCP is related to the inhibition of the oxygen penetration through wood or during racking and sampling of wine. Although a slight
oxidation is desirable, a more extensive one can cause various sensory changes, such
as oxidized odor, browning, loss of color in red wines, activation of spoilage bacteria and yeasts, development of ferric casse, and precipitation of tannins (81). Limits
on free and total SO2 levels in finished wine are variable from country to country.
Clarification
Clarification involves only physical means of removing the suspended particulate matter. Juice clarification by racking, centrifugation or filtration often
27
improves the flavor development in white wine, and helps the prevention of microbial spoilage. If sufficient time is provided, racking and fining can produce stable,
crystal clear wines, but now that early bottling in a few weeks or months after fermentation is employed, centrifugation and filtration are used to obtain the required
clarity level (82). Microbial contamination of wine during the above mentioned
procedures constitutes a potential problem for its stability (83). Racking is also
effective on pesticide residue reduction of wine (84).
Stabilization (CCP5)
The reason for stabilization is production of a permanently clear and flavor
fault-free wine. The most important procedures include a) tartrate stabilization
by chilling the wine to near its freezing point and then filtering or centrifuging
to remove the crystals, b) protein stabilization with absorption, denaturation, or
neutralization by fining agents (bentonite) (85), c) polysaccharide removal with
pectinases that hydrolyze the polymer, disturbing its protective colloidal action
and filter plugging properties (82), and d) metal casse (Fe, Cu) stabilization. Ferric casse is controlled by the addition of agents (bentonites, proteins) controlling
the flocculation of insoluble ferric complexes, whereas wines with copper content
greater than 0.5 mg/L are particularly susceptible to copper casse formation (86).
Legal residual copper levels in finished wines are variable and not all methods for
copper removal are approved in all countries. In particular, all wine industry federal
regulations for the US industry can be accessed via the Bureau of Alcohol, Tobacco
and Firearms (BATF) (available at http://www.atf.treas.gov).
Bottling (CCP6)
Wine is bottled in glass bottles sealed with cork. The bottles must pass a
decontaminating step and an inspection control to assure the absence of any defects and the stability of the product until its consumption (87). The cork should
be correctly sized, 67 mm bigger than the inner neck diameter, to avoid any possible leaks. In bottling all three hazards may be encountered. In particular, cork
microflora, residues of heavy metals, SO2 , pesticides and detergents, and absence
of cracks, scratches and rifts in the lute represent microbiological, chemical and
physical hazards. Although cork is noted for its chemical inertness in contact with
wine, it might cause off-flavors when contaminated (88,89) or when the producers are not applying effective quality control (90). The CL for cork is absence of
LAB and yeast, which can be assured with microbiological analysis. When long
storage of wine is anticipated, longer and denser corks are preferred, because prolonged exposure slowly affects the cork integrity. Since on compression a plunger
forces the cork down into the neck of the bottle, precaution must be taken against the
buildup of microbes within the equipment (91,83), the lead transfer to wine through
28
the wine-cork-capsule system (92), and the oxidation during filling by flushing the
bottles with carbon dioxide. Cork insertion may also occur under vacuum. The
headspace oxygen might affect the product quality by causing the disease of
the bottle. The CL for SO2 is 175 and 225 mg/L for red and white wine, respectively, for As < 0.2 mg/L, Cd < 0.01 mg/L, Cu < 1 mg/L, Pb < 0.3 mg/L, the
residues of pesticides and insecticides in the final product are provided by Office
International de la Vigne et du Vin (57).
Storage (CCP7)
Shipping and storage of wines at elevated temperatures can initiate rapid
changes in color and flavor of wine. Direct exposure to sunlight corresponds to the
effect of warm storage temperatures. Temperature affects reaction rates involved
in the maturation, such as the acceleration of hydrolysis of aromatic esters and
the loss of terpene fragrances (93). Temperature can also affect the wine volume
and eventually loosen the cork seal, leading to leakage, oxidation, and possibly
microbial formation resulting in spoilage of bottled wine.
The occurring hazards, CCPs, CLs, preventive and corrective measures are
given synoptically in Table 4.
DISTILLED SPIRITS
Introduction
Distillation is one of the earliest examples of implementation of chemical
technology. The process was known in China many hundred years before the birth
of Christ and the first distilled beverage is believed to have been made from rice
about 800 B.C. The first few years A.D., the Arabs learned the technology and from
them, distillation was introduced to Western Europe (25). The spirit distillation industry comprises a heterogeneous assortment of manufacturing processes linked by
yeasts as a common function. Distillery spirits are available in many forms, varying
from pure alcohol to complex potable spirits. Nevertheless, they are all based on the
same biochemical and physical principles and similar manufacturing stages (18).
Gin and vodka typify non-cogeneric spirits. In the case of gin, the spirit is flavored
with juniper and other botanicals, while with vodka, the flavor is modified by
filtration through charcoal. Both distillates can be produced from the several grains
or potatoes, fermentation depending essentially on consistency and reliability of
supply and quality and on economics and on the plant available (13). Ouzo, the
most popular distilled spirit consumed in Greece, is traditionally manufactured
from wine distillation. Its characteristic aroma and flavor are attributed to anethol,
the main constituent of anise seed (94). Brandy is a spirit distilled from wine and
is produced in all viticultural regions. In terms of quality the best-known brandies
are Cognac and Armagnac. Both of these brandies are produced by distillation of
white wine from geographically defined regions of France.
Bacterial
preparations
(CCP3)
Fermentation
(CCP2)
Harvesting
(CCP1)
Process Step
Hazards
(C, M, P)a
Avoid intensive
fertilization
Avoid high
temperatures
Use proper yeast
cultures
Employ urease
Certified suppliers,
strictly following
instructions
Careful handling
of grapes
Specify the last day
of applying
pesticides
Material without
heavy metals,
corrosion checks
Certified suppliers,
control of the
product
Careful maintain the
equipment, use of
non-toxic glucole
GMP
ControlPreventive
Measures
Microbiological
contamination
100% clean
Ethyl carbamate
formation
Residues of
ethylene glycole
& detergents
Methanol
content
Pesticide residues
Heavy metals
presence
Reduced to
acceptable level
Per pesticide
according to
Codex Alim.
As < 0.2, Cd <
0.01, Cu < 1,
Pb < 0.3 (mg/L)
Per pesticide
according to
Codex Alim
Absence
300 mg/L (red),
150 mg/L (white
& rose)
Critical Limits
(CLs)
CCP Parameter
Microbiological
analyses
Gas
chromatography
Specific chemical
analyses
Inspection during
harvesting
Specific chemical
analyses
Monitoring
Procedures
Trained
personnel
Quality
control
manager
Quality
control
manager
Responsible
Personnel
(continued )
Rejection of
specific batch,
dilution with
large quantities,
machinery
modification
Rejection of
specific batch,
dilution with
large quantities
Instruct
personnel
Delay of
harvesting
date
Rejection of
specific batch,
demetallisation
Rejection of
specific batch
Corrective
Actions
Table 4. Summary of Hazards, CCPs, CLs, Monitoring, Corrective Actions, and Personnel Responsible for Wine Production
GMP, materials
without heavy
metals
Certified suppliers,
control of the
product
GMP, avoidance of
high doses
Inspection and
screening of the
bottling area
Stabilization
(CCP5)
Bottling
(CCP6)
Certified suppliers,
proper barrel
decontamination
GMP, materials
without heavy
metals,
calculation of
ferrocyonide
needed according
to Fe present
ControlPreventive
Measures
Maturation
(CCP4)
Process Step
Hazards
(C, M, P)a
Insect
presence in the
full
bottles
Detergent and
SO2 residues
Pesticide residues
Heavy metals
presence
Residual
ferrocyonide
Heavy metals
presence
Microbiological
contamination
CCP Parameter
Fe: 5 mg/L
Absence of yeasts,
molds and lactic
acid bacteria
As < 0.2, Cd <
0.01, Cu < 1,
Pb < 0.3 (mg/L)
Critical Limits
(CLs)
Table 4. Continued.
Visual inspection
Specific chemical
analyses
Specific chemical
analyses
Microbiological
analyses
Monitoring
Procedures
Quality
control
manager
Quality
control
manager
Quality
control
manager
Quality
control
manager
Responsible
Personnel
Modification of the
CIP, rejection of
batch
Trained
Disinfect the
personnel
area, rejection
of specific
batch
Filtration or
dilution with
larger quantities
Rejection of
specific batch,
demetallisation
Rejection of
specific batch
Rejection of
specific batch,
demetallisation
Rewash the
barrel
Corrective
Actions
30
KOURTIS AND ARVANITOYANNIS
Certified supplier,
establishment of
decontamination
processes
Control storage
conditions and
retail stores
Wine quality
Cork microflora
Cork sizing
Bottle condition
Absence of rifts in
the lute, cracks,
scratches,
Proportional to the
bottle
Yeast, LAB
absence
Storage
(CCP7)
Certified supplier,
continuous
inspection
Certified supplier
Organoleptic
controls
Sample
measurements
Microbiological
analyses
On-line visual
inspection
Trained
personnel
Quality
Rejection of
control
faulty corks,
manager
decontamination
process
Rejection of
Trained
faulty batches
personnel
Rejection of faulty
bottles
32
33
34
Fermentation (CCP2)
Yeasts are selected in terms of their satisfactory performance in the particular type of mash used. The main criteria are fast fermentation rate, high ethanol
yield, high ethanol tolerance and ability to ferment carbohydrates at relatively
high temperatures. Overheating can be a serious problem and temperatures in the
fermentation vessels must be carefully controlled. An infection-free yeast is also
required for this stage (CCP). For this particular stage the CCPs are similar to those
mentioned for wine production in Table 4.
Distillation (CCP3)
Alcohol of 96 vol.-%, deionized water, and flavorful seeds (anise, gum, etc.),
wine or fermented grains are fed into the boilers at concentrations prescribed by
the formulation for large-scale ouzo production, traditional production of ouzo and
brandy, gin and vodka, respectively. Distillation is carried out within the range 63
80 C for 10 to 12 h. The percent alcohol volume of the final distillate amounts to
about 5% v/v At this step a potential chemical hazard is the formation of ethyl carbamate, as mentioned in wine production. The CL for ethyl carbamate is different
per product (i.e., 150 ppb for wine distillates, 400 ppb for fruit brandies, 60 ppm for
rum, 70 ppm for sherry). Since inadequate thermal process might result in a possible microbiological hazard, on-line inspection of the thermal processing conditions
and microbiological examination of the distillate are indispensable. Moreover, the
distillate must satisfy the prescribed standards for the incoming alcohol (97). Were
considerable deviations to be observed, the responsible person would need to order
the redistillation or the rejection of the batch. Chocolate used for brandy production undergoes both physical control (microscopy, naked eye observation) for the
inspection of presence of foreign materials and microbiological examination for
E. coli (less than 103 cfu/g) and B. cereus (CCL = 104 cfu/g) (98,99).
Dilution of Distillate with Alcohol Addition
The produced distillate has a high concentration of flavorful compounds and is
diluted by adding alcohol of 96 vol.-%, thus resulting in a minimum concentration
of distilled alcohol of 40% in the final product, in agreement with current legislation
for ouzo production (95).
Storage of Spirit Distillate (CCP4)
The diluted distillate is transferred into stainless steel tanks, where it is stored
for about 1015 days stirred continuously so that all components are adequately
dissolved. The concentration of cis-anethol should be accurately controlled by
Storage of distillate
(CCP4)
Distillation (CCP3)
Incoming raw
materials
(CCP1)
Process Step
Urea determination
Use proper yeast
cultures
GMP, control of
distillation
procedure,
frequent cleaning
Certified suppliers
Control of storage
conditions,
Certified suppliers
ControlPreventive
Measures
Hazards
(M, C, P)a
Time-temperature
on-line
monitoring
Gas
Rejection of
chromatography
specific batch,
dilution with
large quantities
6380 C for
1012 h
Temperature and
distillation time
Content of total
anethol in
cis-anetol
Ethyl carbamate
formation
150 ppb,wine
distillate
400 ppb,fruit
brandies 60 ppm,
rum 70 ppm,
sherry
<1%
HPLC analysis
Microbiological
control
Toxic metals
presence (Greek
Food codex)
Methanol content in
wine, alcohol,
fermented grains
E. coli, B. cereus,
Cl. perfrigens
Recall of specific
distillate batch
Change supplier,
Dilution with
large quantities
Rejection/
redistillation of
specific batch
Change supplier
Rejection of batch
Change storage
conditions
E. coli, B. cereus,
Cl. perfrigens
Corrective
Actions
Monitoring
Procedures
Critical Limits
(CLs)
CCP Parameter
Quality
control
manager
Production
manager
Quality
control
manager
Responsible
Personnel
Table 5. Summary of Hazards, CCPs, CLs, Monitoring, Corrective Actions, and Personnel Responsible for Distilled Spirits Production
Bottle packaging
(CCP8)
Proper storage
conditions
GMP, Testing of
the machinery
Alteration of
organoleptic
properties
Detergent remains
Appearance of
bottles
2.Electrical
conductivity
Use of deionizer
Supplier certificate
1.Water quality
Frequent control on
the system in use
GMP
Complete absence
Absence of
undesirable
foreign materials
& particles, rifts
in the lute, cracks
or scratches
Absence of defects
& correct
labeling
Within
specifications
prescribed in
Directive
80/778/EC
<20 ms/cm
Storage (CCP9)
Bottling (CCP7)
Addition of
deionized
water (CCP5)
Organoleptic
analysis
Chemical analysis
Trained
personnel
2.Automatic
discontinuation
of the deionizer
Rejection of
faulty bottles
Quality
1.Pause of water
control
flow and
manager
analysis of one
or more samples
Continuous
recording of
deionizer
On-line visual
control empty
and full bottle
Chemical and
toxicological
analysis with
AAS
36
KOURTIS AND ARVANITOYANNIS
37
HPLC. The CCL for cis-anethol is 1% of total anethol. In case of deviation, the
specific batch distillate should be recalled.
Addition of Deionized Water (CCP5)
The stirred product is transferred into tanks, where the final product is prepared. Deionized water, aromatic substances (anethol or juniper) and sucrose are
added in ratios, according to formulation, and the mixture is continuously stirred.
The deionized water must comply with the standards as defined by Directive 80/778,
where the CCL for electrical conductivity is 20 ms/cm and water conductivity values
are monitored on-line.
Maturation (CCP6)
Unlike the other spirits mentioned, several brandies are aged for certain period
in wood barrels. Aging involves several processes: complex phenolic substances
as tannins are extracted from wood, structural molecules are depolymerised and
extracted to the distillate, and reactions may occur between components of wood
and distillate (100). These chemical reactions are very important for the organoleptic quality of the final products, which depends on composition of wood, different
treatments in the manufacture of oak barrels and history of the oak barrel (76,101).
Especially for brandy, the presence of scopoletin (determined with HPLC) is considered as a proof of maturation in oak barrels (101). The CL for this step is the
same as mentioned for wine in Table 4.
Bottling (CCP7)
The end product is filtered and then pumped into filler machines. The bottles to be used must be supplied by certified suppliers and undergo a washing step
(sterilization) and on-line visual control for the detection of undesirable foreign
materials, particles, rifts in the lute, cracks or scratches. If any physical defects
are detected, the bottles are rejected (CCP). Once the bottles are filled they are
transferred to the sealing machine, which functions by exerting air pressure onto
the heading of the bottle. The sealed bottles move to the standardization machine
where a code number is printed, containing information about production time and
the serial number of the tank where the final product was prepared. The code number is very important and useful for traceability reasons, such as possible recall of
a certain batch of bottles, external audits and company internal control.
Labeling
Bottle labeling is carried out with a machine that heats and spreads the adhesive
upon each label. Another automatic machine presses labels on the surface of bottles.
38
The label of the beverage should be in accordance with the principles of the Codex
Stan 11985 (Rev. 11991) of the Codex Alimentarius (102).
Bottle Packaging (CCP8)
Bottles are packaged into paperboard boxes of various sizes, according to the
dimensions of the bottles. The encountered hazards can be of physical, chemical,
and microbiological origin (CCP). Visual control before packaging can assure that
no defective bottles leave the plant. Chemical and microbiological control must be
carried out to assure the efficiency of cleaning in place system (CIP) and to check
the possibility of cross-contamination due to the remains of washing solutions.
Storage Distribution (CCP9)
During their storage and distribution the bottles of ouzo/brandy should be
kept away from sunlight, that might affect their organoleptic properties (103). The
occurring hazards, CCPs, CLs, control (preventive) and corrective measures and
responsible personnel are summarized in Table 5.
CONCLUSIONS
The implementation of HACCP system to the drinks industry has been of a
tremendous help in terms of providing the required assurance for worldwide trade
expansion. Although the alcoholic beverages are comparatively safer than other
foods and drinks because of their high alcohol content, identification of potential
hazards and resumption of preventive and corrective actions (whenever required)
is of primary importance. Establishment of critical control limits in conjunction
with appropriate and effective monitoring procedures carried out by responsible
personnel have managed to minimize the outbreaks of incidents that are hazardous
and pernicious for human health.
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