Desalination 148 (2002) 93–98

Cold sterilization and clarification of pineapple juice

by tangential microfiltration

Lucia Carneiroa, Iralla dos Santos Saa, Flávia dos Santos Gomesb, Virginia Martins
Mattab, Lourdes Maria Corrêa Cabralb*
a
Food Technology Department, UFRRJ, Rodovia BR465 Km7, Seropédica, Brazil
Tel./Fax +55 (21) 26821220; emails: lucia_carneiro@hotmail.com, iralla@zipmail.com
b
Brazilian Agricultural Research Corporation, Av. das Américas, 29501, Guaratiba, 23020-470 Rio de Janeiro, Brazil
Tel. +55 (21) 24107435; Fax +55 (21) 24101090; emails: fgomes@ctaa.embrapa.br, vmatta@ctaa.embrapa.br,
lcabral@ctaa.embrapa.br

Received 5 February 2002; accepted 25 March 2002

Abstract

Pineapple is a very appreciated tropical fruit due to its unique aroma and flavour. Pineapple juice was cold
sterilised and clarified by crossflow microfiltration associated with an enzymatic treatment. A tubular polyethersulfone
0.3 µm pore size membrane with effective filtration area of 0.05 m2 was used in the pilot system. Ten experiments
were carried out under the same operational conditions, 25ºC and 100 kPa, in order to evaluate the cold sterilisation
and clarification of pineapple juice by microfiltration. It was observed that the permeate flux did not change
significantly after fifteen minutes of processing time. It was stabilised around 100 L/hm2. The clarification process
was considered very efficient due to the great reduction of haze and viscosity, and by showing no significant changes
in pH, acidity, sugar and soluble solid content of the juice. The permeate of the process was collected in sterile
bottles inside a laminar flow station and kept under refrigeration (8ºC) for a period of 28 d. The samples were
submitted to microbiological evaluations in intervals of seven days. The microbiological analysis of the microfiltered
pineapple juice showed that it was in agreement with the requirements by the Brazilian Legislation for juices and
drinks.

Keywords: Pineapple; Microfiltration; Sterilization; Clarification; Enzymatic treatment

*Corresponding author.

Presented at the International Congress on Membranes and Membrane Processes (ICOM), Toulouse, France,
July 7–12, 2002.

0011-9164/02/$– See front matter © 2002 Elsevier Science B.V. All rights reserved
94 L. Carneiro et al. / Desalination 148 (2002) 93–98

1. Introduction be pasteurised and added to the permeate sterile

juice in order to obtain the reconstituted juice [3].
Pineapple is one of the most appreciated
Microfiltration is already applied in industrial
tropical fruit due to its very attractive aroma and
scale for fruits like apple, pear, grape, orange and
very nice flavour. The Smooth Cayenne variety is
lemon [4]. In Brazil, there are few industries
known as one of the best for juice production. Its
applying microfiltration to clarify apple, acerola,
chemical composition shows a good equilibrium
lemon and orange juices [5].
between acid and sugar: 4.50; 2.21; 1.45; 0.80 wt.%
In previous works, it was studied the influence
sucrose, fructose, glucose, citric acid, respectively
of membrane pore size and transmembrane
[1].
pressure on the clarification of pineapple juice
Fruit juices world market is about US$ 5.0
[3,6,7]. It was verified that juice quality (Brix,
billions/y, in which Brazil is responsible for 33%.
pH, acidy, total sugar, colour, haze) was independent
Brazil is the most important of exporter in the
of the applied transmembrane pressure and the
world, and exports 50% of the total orange juice,
process used, microfiltration or ultrafiltration. The
besides of passion fruit, pineapple, banana and
investigated microfiltration membrane presented
acerola products [2].
the best permeate flux. So, the present work aimed
There is, indeed, a crescent demand for fruit
to study the use of the microfiltration for the
juices with the original characteristics of the fresh
stabilisation and clarification of pineapple juice.
fruits and free from chemical additives. This
results in the search of new technologies that are
able to improve the sensorial, nutritional and
microbiological quality of the fruit juices.
2. Material and methods
Since thermal processes largely affect the
characteristics of fruit juices, microfiltration can 2.1. Material
be an alternative to fruit juice preservation and
Pineapple from the variety Smooth Cayenne
conservation, because it does not involve the use
was used as raw material. The juice was obtained
of heat treatment. The advantages of micro-
from the pressing of the fresh fruits in a depulping
filtration in relation to the thermal processes are
machine with a sieve of 0.8 mm and it was kept
the use of mild temperature and pressure conditions,
in a freezing chamber at –18ºC until its processing.
which maintain the nutritional quality and the
sensorial attributes of the products.
One of the disadvantages of microfiltration is
2.2. Enzymatic treatment
the decline of the permeate flux along the pro-
cessing (fouling), caused by the retention of some Before the microfiltration process, the pineapple
feed components on the membrane surface or in juice was submitted to an enzymatic treatment
membrane pores. During microfiltration of pulpy with 0.03% (v/v) of two enzymatic preparations
juices the fouling is caused by pectins, tannins, (Pectinex SP-L and Celuclast 1.5 L, from Novo
proteins, starch, hemicellulose and cellulose. Nordisk), at 30°C for 60 min. The enzymatic
Therefore, it is important to introduce actions to treatment reduces the viscosity and the suspended
minimise fouling, such as enzymatic hydrolysis solids (pulp) content of the juice, and, consequently,
prior to membrane filtration. decreases the fouling in the microfiltration process.
The application of microfiltration process to The hydrolysis was carried out in a stainless steel
fruit juices produces two fractions: a clarified and mixture tank with controlled temperature and
sterile juice (permeate) and a fibrous concentrated agitation. The hydrolysis condition was defined
pulp one (retentate). The concentrated pulp can in a previous work [3].
 L. Carneiro et al. / Desalination 148 (2002) 93–98
2.3. Microfiltration
A tubular polyethersulfone membrane from
Koch Membrane Systems with an effective
filtration area of 0.05 m2 and 0.3 µm pore size was
used in the pilot system. The process conditions
were feed velocity of 6 m/s, temperature of 25ºC
and applied transmembrane pressure of 100kPa.
During the process, the permeate was continu-
ously collected and the retentate stream was re-
circulated. The process performance was evaluated
by permeate flux behaviour. The experimental
design consisted of a set of ten microfiltration experi-
ments in the pilot unit under the same operational
conditions. After each process alkaline/acid/alkaline
cleaning steps were used to recover the water
permeability of the membrane (1800 L/hm2bar).
The volumetric concentration factor (VCF) is
defined as the initial volume divided by the
retentate volume at any time. The retentate volume
was determined by the difference between the
initial feed and permeate volumes. All the processes
were finished when the concentration factor was
equal to 2.
2.4. Analytical procedures
Samples from the feed, retentate and permeate
were analysed in relation to pH, titrable acidity,
soluble and total solids content [8]. Instrumental
colour and haze evaluations were carried out in a
Hunter system [9]. Glucose, fructose and sucrose
concentrations were measured by HPLC [10].
The permeated juice was collected in sterile
bottles inside a laminar flow station and kept
under refrigeration for a period of 28 d. They were
submitted to microbiological evaluations in inter-
vals of 7 d (total count, mould and yeast count,
fecal and total coliforms counts). The microbio-
logical analyses were performed in clarified juices
following the methodology described in American
Public Health Association [11].
3. Results
An enzymatic treatment was associated with
95
microfiltration of pineapple juice to improve the
filtration. The treatment consisted of hydrolysing
soluble polysaccharides, which are responsible for
the high viscosity of the juice, as well as liquefying
the non soluble polysaccharides such as non soluble
pectins, cellulose, hemicellulose and lignin from
cell [12].
The enzymatic treatment did not result in
significant differences on the physical and
chemical characteristics of the single strength and
hydrolysed juices. As it was expected, the excep-
tions were the viscosity and pulp content values.
The average reduction of the viscosity from the
single strength juice to the hydrolysed one was
29.6% and for the pulp content was 22.0%.
Table 1 shows the main physical and chemical
characteristics of the pineapple juice along all the
steps of the processing: single strength (juice),
hydrolysed (feed), clarified (permeate) and
retentate.
Acidity, pH and soluble solids did not change
during the processing and presented average
values of 0,80 w/w % citric acid, 3.7 and 10.0ºBrix,
respectively. Glucose, fructose and sucrose con-
centrations were maintained constant along the
process steps, presenting average values of
5.4 w/w %, 2.4 w/w % and 2.2 w/w %, respectively.
As the sugar and acid concentrations remained
unchanged the microfiltered juice maintained the
same flavour characteristics of the single strength
one.
It was verified an increase in the luminosity
and a decrease in the haze of the permeate juice
when compared to the single strength one (Table
1). The pineapple juice became clearer and brighter.
It was also observed a reduction of the pulp
content in the hydrolysed juice (5.7 g/100 g) and
the permeate (0.0 g/100 g) when compared to the
single strength juice (7.4 g/100 g). The clarification
process completely removed the suspended pulp
in the permeated juice, as it was already observed
by Matta et al. [2].
Fig. 1 shows the behaviour of the permeate
flux during one of the microfiltration processes.
It could be separated in two steps. First there was
96 L. Carneiro et al. / Desalination 148 (2002) 93–98

Table 1
Average physical-and chemical characteristics of single strength (juice), hydrolysed (feed), clarified (permeate) and retentate
pineapple juice during all the steps of microfiltration processes

Parameters Juice Feed Permeate Retentate

a a a,c
Total solids content, w/w% 10.1 10.2 9.1 10.6a
pH 3.6a 3.6a 3.6a 3.6a
Acidity, w/w % citric acid 0.8a 0.8a 0.8a 0.8a
Soluble solids, °Brix 10.0a 10.1a 9.9a 10.0a
Viscosity, mPa.s 6.3a 4.4b 1.1c 10.4d
Sucrose, w/w % 5.7a 5.4a 5.3a 5.1a
Glucose, w/w % 2.1a 2.3a 2.6a 2.7a
Fructose, w/w % 2.0a 2.1a 2.3a 2.5a
Pulp content, w/w % 7.4a 5.7b 0.0c 10.3d
LHUNTER1 16.8a 17.2a 97.9b 9.9c
aHUNTER2 –0.6a –0.6a –3.8b 1.4c
bHUNTER3 6.8a 6.6a 12.4b 6.2a
Haze 97.2a 97.3a 3.3b 98.7c
Averages at the same line with different letters are different (p< 0,05, Tukey test)
1
LHUNTER – luminosity (0 = black and 100 = white)
2
aHUNTER – (from –80 to zero = green, from zero to +100 = red); 3bHUNTER – (from –100 to zero = blue, from zero to +70 = yellow)

250
15 min of process, and it was equal to 100 L/hm2.
Permeate flux (L/hm2)

200
150
100
50
0 results in the flux decline [12].
0 30 60
Processing time (min)
Fig. 1. Permeate flux during a microfiltration process of
pineapple juice.
an acute decay of the permeate flux followed by
a period when the flux decay was less pronounced
tending to stabilisation. Other authors like Itoua
Gassaye et al. [13] who also studied the clarification
process of pineapple juice have described the
same behaviour.
In the beginning of the microfiltration process
the permeate flux was around 232 L/hm2. After
five minutes of processing, this parameter reduced
52%. The average permeate flux stabilised after
The main factors that contribute to the flux
decay are the concentration polarisation, the pore
blocking and the juice viscosity increase due to
the increase of the concentration factor. The main
disadvantage of microfiltration of pulpy juice is
the fouling on the membrane surface, which
90 The clarified juice presented a great reduction
in the viscosity value due to the removal of pulp
and macromolecules from the single strength
juice. As observed in Table 1, the apparent viscosity
value of the microfiltered juice was 1.1 mPa.s.
The clarified juice presented the rheological
characteristics of a Newtonian fluid (Fig. 2). The
same behaviour was verified by Hernandes et al.
[14], who studied orange juice ultrafiltration, and
by Matta et al. [2] during the investigation of
acerola juice by microfiltration.
The characteristics of the permeated juice
showed that microfiltration was effective for the
“commercial” sterilisation of the juice. The micro-
filtered pineapple juice presented microbiological
 L. Carneiro et al. / Desalination 148 (2002) 93–98 97

2500 enzymatic hydrolysis with microfiltration can be

Shear stress (mPa)

2000 an attractive alternative to sterilise tropical pulpy

1500
1000
500
0
0 500 1000 1500
-1
Velocity gradient (s )
Fig. 2. Rheological behaviour of the clarified pineapple
juice.
characteristics in agreement with the established
patterns of the Brazilian legislation for juices and
drinks. It presented the counting of moulds and yeast
and of mesophilic bacteria less than 10 CFU/g, total
coliforms less than 0.3 per g and absence of
Salmonella in 25 g (Table 2). These parameters
were maintained during the storage period. These
results indicate that microfiltration can be used
as an alternative process for fruit juice conservation
in substitution to the thermal pasteurisation.
4. Conclusions
Pineapple juice was successfully clarified. Its
haze changed from 97.2 to 3.4 and the luminosity
from 16.8 to 97.9. The clarified product presented
also “commercial” sterilisation grade, which fulfils
the requirements of microbiological safety. The
obtained results showed that the association of
fruit juices. The use of this proposal technology
can improve new trends for fruit juices market.
Acknowledgements
2000 The authors wish to tank CNPq and FAPERJ
for the financial support of this project.
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Table 2
Microbiological characteristics of the pineapple juice pasteurised by microfiltration storage at 8°C for 28 d

Sample Total count Moulds and yeasts Fecal coliforms Total coliforms
(CFU/mL) (CFU/mL) (MPN/mL) (MPN/mL)
0d <1.0×101 <1.0×101 <3×10–1 <3×10–1
7d <1.0×101 <1.0×101 <3×10–1 <3×10–1
15 d <1.0×101 <1.0×101 <3×10–1 <3×10–1
28 d <1.0×101 <1.0×101 <3×10–1 <3×10–1
Standard1 * 102 1 *
1
As required from Brazilian Legislation for fruit juices quality, *no standard value
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