334 FOOD AND NUTRITIONAL ANALYSIS / Fruits and Fruit Products
For chocolate fats in particular, it is often neces-
sary to know the composition of the TAGs based
simply upon the level and position of unsaturation.
The SOS (1-saturated, 2-monounsaturated, 3-satu-
rated) type TAGs are responsible for the particular
physical properties of cocoa butter and its equiva-
lents. The information can be obtained from the
reversed-phase method mentioned above, but a sim-
pler profile is obtained by using 5% silver nitrate-
impregnated silica as a 25 cm column.
Tocopherols are analyzed in their unesterified form
and separations are very easy by HPLC. The use of
fluorescence detection provides very accurate results.
The oil is diluted with eluent (3% tetrahydrofuran in
isooctane) to B10 mg ml
1. Pure standards are analy-
zed (2 mg ml
1) to obtain retention data, while pure
a-tocopherol is used as an external standard for every
two samples. A 15 cm column of 5 mm Chromega-
sphere is equilibrated with the isocratic solvent at
1.5 ml min
1. Injection volume is 50 ml. The spectro-
fluorimeter excitation is 290 nm and emission is
330 nm. Full separation should be readily achieved,
but the column will require conditioning by pumping
chloroform–methanol (2:1; v/v) for 10 min every 30
samples. After this conditioning, the column activity
must be regenerated by pumping normal eluent for
at least 20 min.
Fruits and Fruit Products
R J Pither, Campden and Chorleywood Food Research
Association, Chipping Campden, UK
& 2005, Elsevier Ltd. All Rights Reserved.
This article is reproduced from the previous edition, pp. 1525–
1531, & 1995, Elsevier Ltd.
Introduction
Fruits have long been valued as a foodstuff owing to
their pleasant flavor and aroma, and attractive ap-
pearance; however, the use of fruits as a staple in the
diet has only become possible in the past century
through the development of canning and other bulk
preservation techniques, and improvements in trans-
portation and storage systems. The increased aware-
ness of the importance of a nutritionally balanced
diet has also contributed to the increased consump-
tion of fruit and fruit products.
Fruits are an important low-fat energy source con-
taining varying proportions of sugars and starches as
See also: Carbohydrates: Starch. Derivatization of
Analytes. Extraction: Solvent Extraction Principles. Flu-
orescence: Food Applications. Gas Chromatography:
High-Temperature Techniques. Lipids: Fatty Acids; Polar
Lipids. Liquid Chromatography: Food Applications.
Mass Spectrometry: Food Applications. Quality Assur-
ance: Quality Control; Internal Standards. Sample Hand-
ling: Comminution of Samples. Sampling: Theory.
Further Reading
Firestone D (Associate Chapter Editor) (1997) AOAC
Official Methods of Analysis chapter 28, Oils and Fats,
p. 507. Washington: AOAC.
Duchateau GSMJE, van Oosten HJ, and Vasconcellos MA
(1996) Analysis of cis- and trans-fatty acid isomers in
hydrogenated and refined vegetable oils by capillary gas–
liquid chromatography. JAOCS 73(3): 275–282.
Gurr MI and James AT (1980) Lipid Biochemistry: An In-
troduction, 3rd edn. London: Chapman & Hall.
Hammond EW (1993) Chromatography for the Analysis of
Lipids. Boca Raton, FL: CRC Press.
Hamilton RJ and Hamilton S (eds.) (1992) Lipid Analysis,
A Practical Approach. New York: IRL Press, Oxford
University Press.
Standard Methods for the Analysis of Oils, Fats and
Derivatives (1987) 7th Revised and Enlarged Edition,
International Union Pure and Applied Chemistry.
Oxford: Blackwell Scientific Publications.
well as being good sources of dietary fiber, mineral
salts, and vitamins, especially vitamin C. The organic
acids found in fruits essentially balance with the
sugars to give them their characteristic flavors and
are therefore also a vital component.
Major Components
The major component of fresh fruit is water, with
levels ranging from 65% (in avocado) to 93% (e.g.,
in melons, strawberries). Dried fruit products can
contain up to 25% water while fruit juices can vary
between 85% and 93%. The second most important
component in terms of percentage content is carbo-
hydrate, with reducing sugars, primarily a mixture of
glucose and fructose, being the main soluble carbo-
hydrate. Most fruits contain relatively low levels of
sucrose; however, it is the primary sugar in peaches,
apricots, bananas, pineapple, and certain citrus
fruits. Starch, cellulose, hemicellulose, and pectin
are also found in varying proportions in fruit.
 FOOD AND NUTRITIONAL ANALYSIS / Fruits and Fruit Products 335
In general, fruits are poor sources of protein and
lipid, the major exceptions to this being avocado and
olives, which can contain B11% and between 10%
and 40% lipid, respectively.
Most fruits are particularly rich in organic acids,
the principal ones being citric, tartaric, and malic
acids; however, the range is extensive.
By far the most important acid present in fruits is
L-ascorbic acid, vitamin C. Fruits, together with
vegetables, are the main sources of this vitamin in the
human diet. Its importance was first reported by a
Hungarian physician in 1732, who documented the
relationship between citrus fruit and antiscorbutic
activity. The concentration of L-ascorbic acid can
vary between only 2 and 30 mg per 100 g in apples
and pears, to over 1000 mg per 100 g in rose hips and
certain cherry varieties. The majority of fruits,
however, including citrus, have values in the region
of 30–100 mg per 100 g. Today, orange juice alone
provides 60% of the US Recommended Daily
Allowance (RDA) for vitamin C in the American diet.
Several fruits are good sources of b-carotene, for
example, apricots, peaches, melons, and cherries,
while a range of B vitamins (pantothenic acid, folic
acid, biotin, thiamine, and riboflavin) can also be
found. In general, however, the concentrations of the
latter vitamins are low when compared with other
animal and vegetable sources.
Fruits and fruit products contain a wide range of
mineral salts including potassium, calcium, magne-
sium, phosphorus, and the trace elements, copper,
zinc, iron, and manganese, with potassium being the
most abundant of these in a majority of fruits.
Whereas a serving of a fruit or fruit product may
provide only a small percentage of the RDA of many
of these mineral nutrients, they are still good sources
when calculated in terms of their calorific contribution.
Sampling and Preparation for Analysis
Sampling and preparation techniques are the first,
and some of the most important, steps toward
achieving an accurate analytical result. There are
many sources of error in any analytical technique,
e.g., analyst’s error, contaminated reagents or equip-
ment, inappropriate methodology, and calculation or
data handling error. Most of these can be controlled
or detected by the use of standards, blanks, reference
samples, and other quality control procedures.
An unrepresentative sample, however, may not be
so easily detected. Foodstuffs are naturally he-
terogeneous materials and, therefore, obtaining a
homogeneous and representative sample is a major
problem. For most fruits and fruit products sampling
will be carried out from bulk materials. For such
sampling it is important, first, to identify the size of
the population or batch, then to select and remove
gross samples from this population, and finally to
reduce these samples to a suitable laboratory sample
size, all whilst maintaining as far as possible the re-
presentative nature of the sample. This is generally
achieved by selecting several samples from the bulk,
either randomly or according to a plan, and
thoroughly mixing these to form a composite sam-
ple from which a subsample for laboratory analysis
can be taken.
There is much information available on sampling
plans for foodstuffs. The Codex Alimentarius Com-
mission (document CAC/RM 42-1969) deals with
sampling plans for prepackaged foods, and there are
standards available from the International Standards
Organization (ISO) for sampling of various food-
stuffs including fresh fruits and vegetables (ISO
874:1980). Details of the mathematical principles
involved are dealt with in many books on statistics.
Due both to the economic aspects of statistical
sampling plans and the difficulties encountered
owing to the natural variation in foodstuffs, most
analyses, however, are carried out on randomly se-
lected samples.
The method of preparation used to produce a
homogeneous laboratory sample varies considerably
with food type. Examples of laboratory sampling
and preparation procedures for fresh fruit products
can be seen in Table 1.
There is a wide range of fine-slicing devices avail-
able that are suitable for homogenization of fruit and
fruit products: liquidizers, domestic-type food proc-
essors, Waring blenders. Care must be taken to en-
sure that excessive heat generation does not occur
during the homogenization process that can lead to
loss of moisture, and that the sample is transferred
immediately to a suitable storage vessel. These
should be of glass or rigid plastic, have a tightly fit-
ting lid and be easily labeled.
Stabilization of the product after preparation is
also an important consideration, with the sample
susceptible to change due to enzymatic, oxidative, or
microbial action. In most cases for fruit and fruit
products the most practical way of achieving this is
by rapid freezing and storage at
201C. Inactivation
of enzymes can also be achieved by treatment with
80% methanol or ethanol, or ice-cold 10% perch-
loric or trichloroacetic acid, while oxidation may be
reduced if reducing agents such as hydrogensulfite or
dithiothreitol are added during the homogenization
process. The most appropriate method will depend
on the analyses to be performed and the exact nature
of the sample.
336 FOOD AND NUTRITIONAL ANALYSIS / Fruits and Fruit Products
Table 1 Preparation procedures for fresh fruit products
Fruit type Preparation technique
Apples, pears, Select 10–15 fruits
etc. Remove extraneous matter: leaves, stalks,
etc.
Cut into quarters along the longitudinal axis
Take a selection of the quarters and
mechanically finely chop and mix
Plums, peaches, Select 15–20 fruits
apricots, etc. Remove extraneous matter and destone
Proceed as for apples, pears, taking care to
collect any released juices
Berries, cherries, Remove a random selection of individual
olives, etc. berries from the sample (minimum of
100 g)
Remove stones (preferably using a cherry
stoner) while carefully avoiding loss of
juice and fruit flesh
Mechanically finely chop and mix
Exotic fruits: Remove inedible portions: skin, peel, stones,
bananas, etc., and extraneous matter
avocados, Cut into quarters
kiwi, etc. Take a selection of these quarters and
mechanically chop and mix
Citrus fruits:
oranges,
grapefruit,
lemon, lime,
etc.
Analytical Methods
Moisture/Total Solids
Water is present in foods as both bound and available
free water, the quantification of which is dependent
on the methodology used.
The standard procedure for measuring moisture in
fruits and fruit products is by weight loss on drying.
References to this methodology can be found in
many books; however, they all follow the same basic
technique, i.e., Association of Official Analytical
Chemists (AOAC) methodology:
Accurately weigh a sample into a large flat-
bottomed dish and dry at 701C under vacuum
(pressure p100 mmHg) until consecutive weigh-
ings vary by less than 3 mg.
This method has the disadvantage of a consider-
able drying time (usually 4–6 h) and many rapid
techniques are now available. Infrared drying ovens
and microwave ovens have been shown to produce
comparable results to vacuum oven drying methods
for various fruit products. Nondestructive techniques
such as low-resolution nuclear magnetic resonance
(NMR) and near-infrared (NIR) spectroscopy can
also be used for moisture determination and are of
particular use for online checking during food man-
ufacture and processing.
Carbohydrates
Sugars A wide range of methods is available for the
determination of sugars in fruit and fruit products.
These include relatively simple refractometry and
hydrometry techniques, polarimetry, copper(II) reduc-
tion, enzymatic/color detection, and various chromato-
graphic techniques. These vary greatly in their
sensitivity, specificity, and in the level of equipment
and expertise required, and these considerations
generally dictate the method chosen.
Refractometry This allows for the rapid, reasona-
bly accurate estimation of sugar levels based on the
measurement of soluble solids. Correction tables
exist allowing for other dissolved substances, e.g.,
acids, and for changes in temperature; however,
many modern refractometers make automatic allow-
ance for this.
Hydrometry This technique relies on the measure-
ment of relative density but is generally less accurate
than refractometry.
Polarimetry The determination of sucrose and red-
ucing sugars in fruit and fruit products by polarime-
try is an AOAC recommended method. The
polarimeter measures the rotation of plane polarized
light caused by a solution containing an optically
active compound. Separate measurements for the
quantification of sucrose and reducing sugars can be
made with the Clerget–Hertzfeld double-polarization
method.
Copper(II) reduction These methods rely on the
ability of certain sugars, i.e., all monosaccharides
and the disaccharides maltose and lactose, to act as
reducing agents, owing to the presence of free alde-
hyde or ketone groups in their structure. Fehling’s
solution consists of alkaline copper(II) tartrate and it
is the ability of reducing sugars to convert this to
insoluble copper(I) oxide that forms the basis of a
number of analytical procedures. The most widely
accepted of these are the Lane and Eynon method,
which has a titrimetric endpoint using a redox indi-
cator and the Munson and Walker method (AOAC)
where the copper(I) oxide is filtered off and weighed.
The Luff–Schoorl method uses alkaline carbonate
solution and sodium citrate and employs an iodi-
metric determination of the excess copper(II) with
 FOOD AND NUTRITIONAL ANALYSIS / Fruits and Fruit Products 337
thiosulfate. This method is recommended by the
Codex Alimentarius Commission for the analysis of
fruit juices.
All of the copper reduction methods can be used to
determine sucrose, after inversion (conversion to
glucose and fructose), as well as reducing sugars.
These methods are therefore particularly suitable for
fruits and fruit products.
Liquid chromatography (LC) LC is now a popular
and useful analytical technique that has the advan-
tage that different sugars can be determined simul-
taneously. The separation technique can be carried
out using strong cation-exchange chromatography,
or a modified silica gel–amino column, with detec-
tion by refractometry. This method does have certain
disadvantages in that initial equipment costs are high
and, owing to the sensitivity of the detectors, they are
best when used exclusively and continuously for the
same analysis. The latest development in LC analysis
of carbohydrates uses improved anion-exchange
techniques combined with pulsed amperometric de-
tection, which is both more sensitive and specific
than the traditional LC methodology.
Gas chromatography (GC) This technique has the
advantage of allowing food sugars to be determined
with very high sensitivity and provides an AOAC
recommended method. The sample sugars have to be
converted to volatile and heat-stable derivatives be-
fore analysis and this technique is not widely used in
routine analysis because of the accuracy and relative
simplicity of alternative methods.
Enzymatic reactions Enzymatic reactions have the
advantage of being specific; for example, hydrolysis
of sucrose is more accurate using invertase than an
acid. A wide range of sugar analysis kits is available
commercially; for example, sucrose/glucose/fructose
kits are particularly suitable for fruit and fruit prod-
ucts. They, in common with the copper reduction
methods, have the advantage of simple sample prep-
aration techniques. The enzymatic reactions involved
cause the reduction of NADP þ, the concentration of
which is determined by spectrophotometry at 340 or
366 nm. Great care is needed in their use because of
the very precise quantities involved; however, the re-
sults obtained compare favorably with more tradi-
tional methods and the methods are now widely
accepted.
Starch The determination of starch in fruits and
fruit juices is normally achieved by the hydrolysis of
the starch to glucose and the subsequent analysis of
glucose levels. Acid hydrolysis methods can be
subject to error because of the possibility of hydro-
lysis of nonstarch polysaccharides or the destruction
of glucose. Enzymatic hydrolysis of the starch can
also be employed using amyloglucosidase, and com-
mercial kits are available that allow for concurrent
analysis of the prepared sample for glucose content,
with and without the addition of the amylo-
glucosidase.
Dietary fiber The determination of dietary fiber has
increased greatly in importance in recent years;
however, due partly to lack of a clear definition for
dietary fiber, several standard methodologies exist.
AOAC enzymatic gravimetric method The samples
are dried, with fat extracted if necessary, gelatinized
with heat-stable a-amylase, and enzymatically digest-
ed with protease and amyloglucosidase to remove
protein and starch. The soluble dietary fiber is then
precipitated using ethanol, the residue filtered and
washed, and corrections are made for indigestible
protein and ash. This method is widely used in the
EC and the USA.
Englyst method Samples are defatted if required
and any starch present is gelatinized and removed by
enzymatic digestion. The remaining polysaccharides
are hydrolyzed by sulfuric acid and the resulting
sugars can be measured either colorimetrically or by
using gas chromatography. This method can be used
to determine both total nonstarch polysaccharides
and resistant starch, and is a recognized method in
the UK and Canada.
Pectin There are many methods for the estimation
of pectic substances. The most commonly used for
fruit products are those based on aqueous extraction,
saponification with cold alkali, acidification and the
precipitation of the pectin as the calcium salt; alter-
natively, precipitation using acetone or alcohol can
be utilized.
Minerals: Sodium and Potassium
The AOAC and Codex recommended methods for
determination of potassium and sodium are by flame
atomic emission spectrometry. These methods have
the advantage of quick and simple sample prepara-
tion, aqueous dilution of sample and filtration, with
rapid, reasonably accurate detection. The samples
can be aspirated directly into the flame and the
readings quantified by comparison with a range of
known standards. Atomic absorption spectrometry
can also be used, giving increased accuracy and low-
level sensitivity and a far wider range of detectable
338 FOOD AND NUTRITIONAL ANALYSIS / Fruits and Fruit Products
minerals. It has the disadvantage of higher
equipment costs and requires a dry-ashing sample
preparation technique, which, though simple, can
take a relatively long time; however, if trace metals or
other minerals are also being determined the ashed
sample can be used for all analyses.
Vitamin C
There are two standard (AOAC) procedures for vita-
min C (ascorbic acid) determination in fruits and
fruit products. The sample preparation is common to
both and involves maceration/dilution of the sample
in a stabilizing solution such as 5% metaphosphoric
acid or trichloroacetic acid followed by filtration.
The ascorbic acid can then be determined by titration
with 2,6-dichloroindophenol, where the ascorbic ac-
id reduces the redox indicator dye to a colorless so-
lution, or by fluorimetric detection, in which the
ascorbic acid is oxidized to dehydroascorbic acid,
which then reacts with o-phenylenediamine to
produce a fluorophore. The latter method has the
advantages that it is suitable for colored solutions
and can also be used to measure levels of naturally
occurring dehydroascorbic acid as well as ascorbic
acid. Many other methods are available for determi-
nation of vitamin C, with the use of LC techniques
currently the subject of much interest. Reversed-
phase LC techniques can be used to determine both
dehydroascorbic acid, ascorbic acid and their iso-
mers.
Phosphate
The sample is first ashed and dissolved in hydrochlo-
ric acid; the phosphate can then be determined titri-
metrically or colorimetrically. The most widely
accepted method is a colorimetric method using Mis-
sion’s reagent, which is based on the reaction between
the acidified sample solution and an acid reagent
containing molybdic acid and vanadic acid, to
produce the stable orange–yellow vanadomolybdo-
phosphoric acid.
Organic Acids/Acidity
For routine analysis a measurement of titratable
acidity is usually sufficient, with the acidity of the
fruit/fruit product calculated as the predominant
acid, e.g., as citric acid in citrus fruits, as malic acid
in apples. The sample is diluted in distilled water and
titrated against dilute sodium hydroxide to either a
phenolphthalein endpoint or to pH 8.10. Volatile
acidity, generally expressed as acetic acid, can be
measured by distilling the sample using a steam dis-
tillation apparatus, with titration of the distillate as
above. Individual acids can be determined using a
range of techniques including chromatographic and
titrimetric methods fully described by the AOAC,
and enzymatic methodologies with commercial en-
zyme-based test kits now available for many fruit
acids. LC techniques are also available facilitating
identification and quantification of a range of
organic acids.
Quality Assurance of Fruits and
Fruit Products
Many analyses and tests are carried out on fruits and
fruit products as a means of quality assurance and
many regulations and specifications exist in relation
to this. These include the Joint Food and Agriculture
Organisation of the United Nations/World Health
Organization (FAO/WHO), Food Standards Pro-
gramme–Codex Alimentarius, the US Department
of Agriculture (USDA) standards for grades of proc-
essed fruit products, the UK Fruit Juices and Fruit
Nectars Regulations, and EC directives.
The range of chemical analyses carried out to de-
termine compliance with quality and specification
requirements can include: pH, titratable, and volatile
acidity; total solids, soluble solids (1Brix), water-in-
soluble solids, sugars; acid-insoluble ash, alkalinity
of ash, mineral impurities, trace metals (tin, copper,
zinc, iron, aluminum), heavy metals, e.g., lead;
ethanol; preservatives such as sulfur dioxide, sorbic
acid, benzoic acid, and benzoates.
Many specifications also define standards for phys-
ical characteristics, e.g., color, flavor, appearance,
and defects. These are generally assessed by trained
personnel; however, a range of equipment is available
for color measurement.
Many of the chemical analyses used for quality
assurance have already been discussed; however,
there are other important tests worth brief consider-
ation.
Essential Oils
Citrus juices make up the bulk of the retail fruit juice
market, with citrus essential oil being one of the pri-
mary constituents contributing to the flavor of the
juice. Both the Codex and USDA standards legislate
an essential oil content, the official method for de-
termination of the recoverable oil being the Scott Oil
Method.
Ethanol
Low levels of alcohol, which can result from the fer-
mentation of juices, are permitted in the Codex
standards; however, they must be monitored. The
levels can be determined using distillation and
 FOOD AND NUTRITIONAL ANALYSIS / Fruits and Fruit Products 339
dichromate oxidation methodology, enzymatic meth-
ods, and GC, with the last now widely accepted.
Mold Contamination
The Howard mold count is the traditional method
for assessing mold content in tomato products, but
has also been applied to other fruit products. The
samples are studied microscopically using a Howard
cell and the number of positive fields, those where the
aggregate length of not more than three mold fila-
ments exceeds one-sixth of the diameter of the field,
is counted. There are regulations governing the per-
centages of positive fields that are acceptable in the
various products. The Geotrichum mold count
method suitable for citrus juices, canned fruits and
juices, and pureed fruit products is also used.
Preservatives
Many of the standards governing fruit and fruit
products contain guidelines on acceptable levels of
preservatives, e.g., sulfur dioxide, benzoic acid/ben-
zoates, and sorbic acid.
Sulfur dioxide (SO2) is generally measured using
indirect methods. The AOAC describes a modified
Monier Williams method, while the Codex standards
and EC directive recommend the Tanner modified
method. Both are based on similar principles,
involving the distillation of the SO2 from an acidi-
fied aqueous suspension of the food. The evolved gas
is subsequently trapped in hydrogen peroxide where
it reacts to form sulfuric acid which is then titrated
against dilute sodium hydroxide.
Benzoic acid and sorbic acid can both be extracted
using modified Monier Williams distillation methods
and quantified spectrophotometrically, or in the case
of benzoic acid using thin-layer chromatography
(TLC). LC and GC methodologies are now available
and routinely used, having the advantage of simul-
taneous quantification of both benzoic acid/benzo-
ates and sorbic acid.
Trace Metals
Trace metals present in foods can have nutritional or
toxicological significance and in the case of certain
metals, e.g., copper and zinc, both of these. Fruit
products are routinely tested for trace metal con-
tents, e.g., canned fruits for tin, iron, copper, and
zinc; fruit juices for copper, zinc, and lead; tomato
puree for copper and also lead, tin, and arsenic.
Statutory limits exist for many metals, e.g., lead, ar-
senic, zinc, and copper. Atomic emission spectrome-
try is now widely used for trace metal analysis
as multielement determinations can be made on a
single sample; however, other methodologies are
applicable. AOAC details colorimetric methods for
determination of copper as diethyldithiocarbamate,
with colorimetric methods for tin also available.
Chemical Residues
Fresh fruit in particular may also be analyzed for the
presence of chemical residues. These may be present
due to specific horticultural and agricultural practic-
es (pesticides, herbicides, etc.), environmental con-
tamination, or through use of certain permitted
additives. Detection and quantification of these res-
idues is a complex analytical problem. Most methods
used are based on solvent separation coupled with
chromatographic determination using LC, GC, or
GC–mass spectrometry.
Added Colors
Fresh fruits must not contain any added color;
however, certain colors are permitted in processed
products. The range and use of colors are strictly
governed, e.g., by UK and USDA regulations, and EC
directives. Many methods exist for the extraction,
separation, and identification of colors. A standard
method suitable for fruit juices and other products
involves the separation of colors from an acidified
aqueous solution of the food using reversed-phase
C18 cartridge and identification using TLC or UV-
visible spectrophotometry by comparison with stand-
ard color solutions.
Adulteration
By far the largest area of adulteration occurring in
fruit and fruit products is in relation to fruit juices.
The size and value of the fruit juice market has meant
that falsification of juice has become a lucrative
business. The main areas of juice adulteration are the
addition of water, sugar and water, or other fruit-
derived products. Water addition is most effective
when used in single-strength juices, as concentrates
have to be diluted to a certain Brix value to meet
specifications. The addition of sugar and water is
difficult to detect, because of the possibility of adding
appropriate sugar mixes to duplicate natural pro-
portions. The addition of other constituents, e.g.,
organic acids, minerals, amino acids, carotenoids, to
maintain the chemical balance of the fruit juice fur-
ther complicates detection. The most complex form
of adulteration is the use of materials derived from
fruit but which cannot legally be used in the fruit
juice. This can range from the addition of other
fruits, to the use of peel extract, pulp wash, and the
water extract of rag, pulp cell membranes, seeds,
etc., in citrus juices. The wide range of fruit-derived
340 FOOD AND NUTRITIONAL ANALYSIS / Fruits and Fruit Products
materials available with different properties can be
combined in such a way as to make detection ex-
tremely difficult.
The methods available for detecting adulteration
can be divided into two types: those which detect a
specific indicator of the added material and those
which rely on the disturbance of a natural analytical
balance.
Stable Isotope Analysis
The ratios of stable isotopes in biological materials
provide a valuable tool for the analyst in detecting
adulteration.
Carbon isotope ratios The ratio of the carbon iso-
topes (13C/12C) in plant sugars varies according to
whether the plant has a C3 or C4 photosynthetic
carbon cycle. Most fruit juices, including citrus and
apple, are derived from plants with C3 metabolism;
however, cane sugar, corn invert sugar, and high
fructose corn syrup all originate from the less com-
mon C4 plants.
Oxygen isotope ratios The use of oxygen isotope
ratios is largely restricted to the measurement of wa-
ter in fruit juices. Water in fruit is assimilated from
groundwater and reflects the isotope ratios present in
it; variations between juices are therefore naturally
derived from variations in the groundwater. Analysis
for carbon and oxygen isotopes is carried out using
mass spectrometry; however, analysis is not simple.
Hydrogen isotope ratios The ratio of 2H/1H can
provide information on water addition but can also
detect the addition of sugars from other plants.
Measurement is usually carried out by the formation
of sugar derivatives, which eliminates the oxygen-
bound hydrogen from the molecule. This is most
simply achieved by the fermentation of the sugars to
ethanol. Fourier transform NMR spectroscopy has
been used to examine the internal 2H/1H ratios in the
ethanol and has been successful in the detection of
beet sugar in orange juice.
Oligosaccharide analysis The technique is based on
the detection of specific oligosaccharides that are not
normally present in the juice but are introduced by the
addition of sugars that have undergone inversion.
Analysis relies upon liquid chromatographic detection.
Analytical Pattern Methods
There are several analytical systems that rely on au-
thentic juice having a consistent pattern based on its
composition.
Matrix method This method relies primarily on
sugar profiles, UV-visible spectrofluorimetry, metals,
calcium stable isotopes, and flavanoid glycosides to
detect the addition of sugar, other fruits, or pulp
wash.
RSK system This, the best known of the analytical
systems, was developed in Germany in 1977 and is
used to control commercial practice in that country.
RSK stands for Richtwerte und Schwankungsbreiten
Bestimmter Kennsahlem, or guide values and ranges
of specific reference numbers. The juices are analyzed
for a very broad range of analytes for which guide
values, the ranges, and central value are given. Be-
cause of the natural variation in juice composition
the ranges given are necessarily broad, and the de-
tailed interpretation of the analytical data is an
integral part of the system.
Other systems also exist including the French na-
tional system, the AFNOR standards, and on a Eu-
ropean basis, the Association of the Industry of
Juices and Nectars from Fruits and Vegetables of the
European Economic Community has drawn up ac-
cepted analytical characteristics or reference stand-
ards.
Visible and ultraviolet spectra The use of visible
and UV absorption and fluorescent spectral charac-
teristics to detect juice adulteration has also been
developed, with the presence or absence of specific
absorption maxima at selected wavelengths indica-
ting adulteration.
Prospective methods Several new techniques for the
detection of fruit juice adulteration are still under
development. These include pyrolysis mass spec-
trometry, size-exclusion chromatography, NIR
spectrometry, and an expert system for data
interpretation. With the methods of falsifying juices
being so numerous and diverse, however, it is un-
likely that any single method will ever be capable of
detecting all forms of falsification.
See also: Atomic Absorption Spectrometry: Flame.
Atomic Emission Spectrometry: Flame Photometry.
Carbohydrates: Starch; Dietary Fiber Measured as Non-
starch Polysaccharides in Plant Foods. Chiroptical Anal-
ysis. Essential Oils. Ethanol. Food and Nutritional
Analysis: Antioxidants and Preservatives; Contaminants.
Isotope Ratio Measurements. Liquid Chromatogra-
phy: Food Applications. Nuclear Magnetic Resonance
Spectroscopy Applications: Food. Optical Spectro-
scopy: Refractometry and Reflectometry. Pesticides.
Sampling: Theory. Vitamins: Fat-Soluble; Water-Soluble.
Water Determination.
 FOOD AND NUTRITIONAL ANALYSIS / Packaging Materials 341
Further Reading
AOAC (1990) AOAC Official Methods of Analysis, 15th
edn. Arlington, VA: AOAC.
Codex Alimentarius (1969) Codex Alimentarius Sampling
Plan for Prepackaged Foods. Arlington, Virginia CAC/
RM 42-1969.
Hulme AC (1970) The Biochemistry of Fruits and Their
Products. London: Academic Press.
Packaging Materials
A W Lord, Pira International, Leatherhead, UK
& 2005, Elsevier Ltd. All Rights Reserved.
This article is a revision of the previous-edition article by Philip
Tice, pp. 3698–3706, & 1995, Elsevier Ltd.
Introduction
Analytical measurements on food packaging materi-
als are generally carried out for three main purposes:
 To identify the components of the packaging.
 To identify and measure substances present that
could migrate into the packaged foods and cause a
health hazard to the consumer of the food. This work
is often accompanied by measurements of the migra-
tion of particular substances into either the actual
packaged foods, or into food simulants.
 To identify and measure substances present that
could migrate into the packaged foods and result in
adverse effects on the organoleptic properties, such
as taste or odor.
Food Packaging Materials
The main categories of basic materials used for food
packaging are:
* plastics,
* regenerated cellulose films,
* paper and board,
* metal, and
*
glass.
Of these, plastics are the most widely used and with-
in this category there are also the largest numbers of
variants. Many packaging materials are, however,
multilayered with either different layers of plastics or
combinations of plastics with paper/board, metal, or
Kirk RS and Sawyer R (1991) Pearson’s Composition and
Analysis of Foods, 9th edn. London: Longman Scientific
and Technical.
Kratochvil B and Taylor JK (1981) Sampling for chemical
analysis. Analytical Chemistry 53(8): 924A–938A.
Nagy S and Attaway JA (1980) Citrus Nutrition and
Quality. Washington DC: American Chemical Society.
Pomeranz Y and Meloan CE (1987) Food Analysis, Theory
and Practice, 2nd edn. New York: AVI.
glass. The individual properties of the different ma-
terials are used to produce food packaging with the
required characteristics. For example, in a packaging
material with two layers of different plastics, one
layer might provide the basic strength whilst the
other layer enables the packaging to be easily heat-
sealed. Coatings are also often added to the basic
plastic packaging material to provide additional bar-
riers to the permeation of oxygen and water vapor.
These coatings can be polymeric or vacuum depos-
ited aluminum.
With some metal cans used for foods and
beverages there is an inner lacquer (plastics) coating
for the purpose of either preventing corrosion of
the metal by the food/beverage, or preventing con-
tamination of the food/beverage by the can metal.
A combination of a polymer layer with a board is
used to package liquids such as milk, where the
plastic layer provides the barrier to contain the milk
within the package and the board the basic strength.
Where it is necessary to store the beverage for long
periods, such as fruit juices, additional barrier prop-
erties are required to prevent permeation of oxygen
into the food product. To achieve this additional
protection, an aluminum layer is incorporated within
a plastic/board composite.
With many of the multilayer packaging materials
adhesives are used to bind the layers together. The
printing on the outside is a further important com-
ponent of food packaging.
Identifying the Components of
Packaging Materials
It is often necessary to identify or confirm the basic
composition of the packaging materials. This applies
particularly with plastics due to the range of polymer
types that are used. Six major polymer types are used
for packaging and these are shown in Table 1, with