E. T. Contis et al.

(Editors)
Food Flavors: Formation, Analysis and Packaging Influences
© 1998 Elsevier Science B.V. All rights reserved 369

Effect of processing conditions on volatile composition of apple jellies and jams

M. Moldao-Martins, N. Moreira, I. Sousa, and M.L. Beirao da Costa,

Instuto Superior de Agronomia, Tapada da Ajuda, 1399 Lisboa Codex PORTUGAL

Abstract
When producing fruit jellies and jams it is intended to preserve as far as possible the
presence of the aromatic characteristics of the fresh fruit. In the present work, the influences of
sugar content - 6 to 55°Brix - and type of pectin - low methoxyl and medium methoxyl pectin -
on the volatile composition of apple jellies and jams is studied. Volatile compounds were
extracted by Clevenger distillation for 180 min and collected in w-hexane. All extracts were
analysed by Gas Chromatography (GC) and Gas Chromatography-Mass Spectrometry (GC-
MS). The influence of jelly structure on flavor release was evaluated by measurement of
objective texture. It was observed that the studied parameters quantitatively affected the
chromatographic profile, keeping the composition similar. Main compounds identified were 3-
methylbutanol, 2-methylbutanol, 1-hexanal, 2-hexanal, hexyl propionate and estragole. The
decrease observed in volatile release from jellies and jams seemed to be related to the retention
of volatiles in the gel matrix and to sugar bonding.

1. INTRODUCTION

The quality of apple fruit and related products depends, among other things, on the
flavor characteristics of the raw material, which is linked to the cultivar and affected by
cUmate, harvesting time, and storage conditions [1]. With regard to the harvesting date, the
lack of volatiles in the immature apple fruit is probably due to the low level of volatile
precursors and enzyme forming systems [2]. This is very important for apples intended to be
stored in controlled atmosphere (CA), since the fruits in this case are usually picked earlier
than those for immediate consumption or refrigerated storage.
Studies of volatiles in apples have shown that between 20 to 40 volatiles are
responsible for apple aroma. These compounds fall into three classes: the "apple-peel smelling"
esters like ethyl 2-methylbutanoate, the lipid oxidation products like (E)-2-hexenal and the
terpenoids like P- damascenone [3].
In the processed fruit products changes in flavor may also occur. Changes in the
contents of the volatile compounds of fresh apple juice afl;er heat pasteurisation have been
reported [4]. The perception of flavor is related not only to the chemical interaction between
the flavors and the matrix, but also to the physical properties of each kind of food. For
instance, flavor perception is lower in gels than in viscous solutions [5]. Many studies have
reported that hydrocolloids not only modify viscosity, but also reduce intensities of odor, taste
and flavor [5].
370

Pectin is the gelling agent generally used in the fmit preserves industry to produce
jellies and jams. Traditionally, high methoxyl (HM) pectin are used. This type of pectin needs
boiling temperatures and high contents of sugar to produce acceptable products. Low
methoxyl pectins (LM) are used in products of lower sugar content; in this case the strength of
gels varies essentially with concentration of calcium ions.
The present work is a study of the influence of processing conditions, namely the type
of pectin and the sugar content (which also influences the texture) on the volatile composition
of apple jellies and jams produced from Golden Delicious apples stored at controlled
atmosphere.

2. MATERIAL AND METHODS

2.1. Materials
Golden Delicious apples stored for six months at controlled atmosphere (% CO2 - 1,5
%; O2 - 2 %; Temperature - 0.5°C) were used.
Low methoxyl pectin, SBI Unipectine LM325 - LM
Medium methoxyl pectin, LM 325 and H&F AF 602 - MM
Sugar 01 commercial grade.
All other reagents are analytical grade and standards are GC grade.

2.2. Jellies and jams preparation

Jellies were produced from apple peels and seeds and jams prepared with apple pulp,
based on the recipe Diese (Portuguese Company) NS/047 with different additions of sugar and
type of pectin (Table 1). In the case of LM pectins an extra supply of Ca++ ions of 0.5 g / g
pectin was added and for the MM pectins the pH was adjusted to 3.0. The sugar content
quoted in this work is the total sugar (apple natural sugar + added sugar) as determined by
refractometry (°Brix).

Table 1. Jellies and jams main differences in compositic n

l Jfmm 3?<!^0i!» ...Itttj \:mm' F^^o :ism:.\
ji LM, 0.5 % (w/w) 30 Gl LM, 0.5 % (w/w) 35
J2 LM, 0.5 % (w/w) 9 G2 LM, 0.5 % (w/w) 6
J3 MM, 0.5 % (w/w) 50 03 MM, 0.5 % (w/w) 55
1 J4 MM, 0.5 % (w/w) 9 04 MM, 0.5 % (w/w) 7 1
J - Jam, G - jelly, LM - low methoxyl pectin, MM - medium methoxyl pectin

2.3. Aroma extraction methods

Distillation on a modified Clevenger apparatus (CLEV) was conducted for 180 min at
atmospheric pressure. Aroma compounds were collected in 2 mL of w-hexane. w-Hexane
solutions were concentrated to 50 |aL by gently blowing nitrogen gas over the «-hexane
surface.

2.4. Analytical methods

Analyses were conducted both on raw material (apple pulp and peel) and prepared
jellies and jams.
 371

The essential oil was analysed by Gas Chromatography (GC) and Gas
Chromatography-Mass Spectrometry (GC-MS).
GC analysis was performed on a Hewlett-Packard 5890 gas chromatograph equipped
with an FID and an HP-5 column (cross-linked 5% biphenyl, 95% dimethylsiloxane) 50 m x
0.32 mm i.d., film thickness 0.17 |im.
GC conditions. Oven temperature: programmed 60°C for 10 min, followed by a slope of
2°C/min to 180°C; 10°C/min to 200°C and a plateau at 200°C/30 min. Injector and detector
temperatures were 200 and 250°C, respectively. Carrier gas, N2 was adjusted to a linear
velocity of 1 mL/min. The samples were injected using the split mode (split ratio 1:8) using a
0.2 |iL injection volume. The quantification of the components was made by internal standard
methodology.
The GC-MS unit consisted of a Hewlett-Packard 5970 mass selective detector
operating in the electron impact mode (70 eV) coupled to a Hewlett-Packard 5890 gas
chromatograph. A capillary column Supelco Wax 10; 30 m x 0.25 mm i.d., film thickness 0.25
|j,m was used. Analytical conditions. Oven temperature: programmed at 80°C for 10 min,
followed by a slope of 2°C/min to 180°C ; lOX/min to 200 °C and a plateau at 200°C/30 min.
Injector temperature was 200°C. Samples were injected using the split mode (split ratio 1:19)
using a 0.2 |LIL injection volume. Carrier gas, He, was adjusted to a linear velocity of 0.89
mL/min.

2.5. Texture analysis

Textural parameters were calculated from a penetration test [6] using a TA-TX2
(Stable Microsystems) texturometer with a 38 mm diameter cylinder probe. The probe was set
to penetrate the gel 10 mm deep, at a speed of 2 mm s"V The jellies and jams were contained
in 100 mL cylindrical glass flasks with 60 mm diameter at 35 mm height.

3. RESULTS AND DISCUSSION

Table 2 shows the main volatile compounds identified in fresh apple peel and pulp. The
compounds of each class included 7 esters, 3 aldehydes, 3 alcohols and 2 terpenoids. The
solvent stripping procedure outlined removed some volatile compounds such as acetaldehyde.
It is interesting to note that the same compounds were identified in the peel and in the
pulp although at different amounts. The largest volatile constituents of fresh fruit are aldehydes
and esters. The most abundant volatile compounds in the peel are C13 aldehyde (20.196 ppm)
and hexyl hexanoate (3.963 ppm). The latter compound is absent in the pulp. Estragole, an
important terpenoid in apple flavor, was found to be present both in pulp (1.423 ppm) and in
peel (1.137 ppm).
The volatile compounds of fresh peel and jellies are shown in Figure 1. It can be seen
that most of the flavor changes in jellies reflect a substantial decrease in the content of
aldehydes and esters. The most dramatic change is the decrease in aldehydes content (from
around 20 ppm to 0.3-0.4 ppm). On the other hand, alcohols show a much smaller decrease
(from 0.7 ppm to 0.3 ppm).
372

Table 2. Volatile compounds of fresh Golden Delicious fractions (ppm).

FIIIJ^ PEElc 1
Batyliasrelate 0.597 0.252
J-lli9Eeft?l*eef««cC^^V i 0.606 0.850
Eesi^l fe»(js|rte„, , , , ^ - 1.285
ESTERS Metier! d«ci^»Mi^e 0.155 1.113
B[e3^|iHES»B€»^ - 3.963
i Z^ Wi^^ h^t^H^fv^^ i - 0.747
i Iie9i^lp^l0ot»te 0.202 0.565
i Mk^i^m^ 0.432 0.368
ALDEHYDES \2-Bs3mas&tia:am&^ 0.376 0.248
Cj^Aid^^e 0.775 20.196 1
i^Besiai^ 0.357 0.278
ALCOHOLS i 2<Mi!^i^iiil3insd 0.277 0.194
i 3rS»i^l^1tabm(]i 0.323 0.210
[ISstri^e 1.423 1.137
[ TERPENOroS \ M^m^^hflk0t^w^ - 0.333 1

The volatile compounds of fresh pulp and jams are shown in Figure 2. Most of the
flavor changes in jams is due to a decrease in the aldehyde content.

Table 3
Texture parameters
Gel Strength (g) Brittleness (mm)
Average value S.E. Average value S.E.
Gl 81.1 2.5 9.811 0.001
G2 nm - nm -
G3 42.9 0.5 9.976 0.024
G4 nm - nm -
Jl 88.1 3.7 9.811 0.001
J2 109.8 11.4 10.000 0.000
J3 79.5 3.7 9.975 0.025
J4 73.4 3.3 9.976 0.024
nm - not measurable

For jams the gel strength results can be grouped into two classes: Jl, J2 and J3, J4 as a
function of the pectin degree of esterification [9]. Brittleness was considered to be related with
the flavor release [7] of the gel materials. From Table 3 the results allow for two classes of
brittle values Jl and J2, J3, J4. These two classes can also be clearly identified on figure 2 for
the content of volatile compounds with the exception of the esters class of compounds, where
this tendency is not so clear. This is in agreement with the reported [7] direct relation of
brittleness with flavor release.
 373

1,8

1,6
20.812
8.77 2.0200

V
a,2

0,6826

o
H,4
0,2

Figure 1. Volatile compounds of fresh peel and jellies (ppm).

Figure 2 - Contents of volatile compounds of fresh pulp and jams (ppm).

The values for gel strength (force at rupture) and brittleness (deformation at rupture)
for jellies and jams can be seen in Table 3. The jellies produced with no extra addition of sugar
did not reached measurable gelification and these jellies showed a higher release of flavor as it
374

is shown in Figure 1. It is known L^^^J that the building up of the gel matrix will reduce the
release of flavor. As expected, L^J the gel strength is determined by the nature of the gelling
agent. The jellies produced with LM pectin showed values of gel strength of the order of 80g
and with MM pectin the value was about 40g. There was no significant difference (P<0.05) in
the brittleness values for jellies.

ACKNOWLEDGMENTS

We acknowledge the kind supply of apples by FRUTUS, S.A..

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