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LWT 40 (2007) 759765 www.elsevier.com/locate/lwt

Technological aspects for restructuring concentrated pineapple pulp

Maur cio De Aguirrea, Regina Kitagawa Grizottoa,, Roy Edward Brunsb, Jose Hilary Castle De Menezesc
Fruit and Vegetable Technology Center, Food Technology Institute, Ital, Box Number 139, 13070-178, Campinas, SP, Brazil b Institute of Chemistry, State University of campinas, PO 6154, 13083-970, Campinas, SP, Brazil c Department of Food Technology, Faculty of Food Engineering, University of Campinas, Unicamp, Box Number 6121, 13083-970, Campinas, SP, Brazil Received 13 February 2006; received in revised form 24 April 2006; accepted 3 May 2006
a

Abstract This study investigated how different concentrations of alginate, low methoxy pectin and glycerol could be used to obtain restructured concentrated pineapple pulp, with the aid of response surface methodology. The results of a central composite design show that changes in pectin and alginate levels have statistically signicant effects on the rmness of restructured pineapple fruit. Products with the highest values for rmness resulted from using 16 g/kg of both alginate and pectin independent of the concentration of glycerol used. Glycerol, used at the concentration of 100 g/kg, reduced the water activity of the restructured product to an intermediate moisture level (0.880), besides substituting part of the sucrose incorporated into the fruit pulp. A mixture of low methoxy pectin and alginate made it possible to obtain very rm structured fruits using acid pulps. The restructured fruit formulated with a high content of concentrated pineapple pulp (735 g/kg), low sugar content (210 g/kg) and a combination of alginate (20 g/kg), pectin (10 g/kg) and glycerol (100 g/kg), partially dehydrated to 20% moisture content (w.b.), was evaluated by a group of panelists and received a mean score of 5.45, between liked slightly and liked moderately on the seven-point hedonic scale. r 2006 Swiss Society of Food Science and Technology. Published by Elsevier Ltd. All rights reserved.
Keywords: Restructured fruit; Pineapple pulp; Hydrocolloids; Response surface; Optimization

1. Introduction The technology for the production of restructured fruit with high contents of fruit pulp using hydrocolloids as binding agents has not been totally established. Nussinovitch and Peleg (1990) veried that the addition of fruit pulp provoked a decrease in gel strength that was less accentuated at low pulp concentrations. The extent of this effect depended on the type of pulp employed and its interactions with the other components, especially the sugar and the hydrocolloid used (Kalentuc, Nussinovitch, & Peleg, 1990; Mancini & McHugh, 2000). A mixture of alginate and pectin has several advantages over the pure hydrocolloids, since the synergism established between them frequently results in higher quality products in terms of physical structure, sensory quality and thermal stability
Corresponding author. Tel.: +55 19 37431825; fax: +55 19 32423104.

E-mail address: regina@ital.sp.gov.br (R.K. Grizotto).

during processing (Mancini & McHugh, 2000). The gels formed, even at low pH, are rm, support cutting and can be obtained without the addition of calcium, required for structuring with pure alginate (Mancini & McHugh, 2000). The addition of sucrose also improves gel texture when the concentration is between 300 and 400 g/kg (Fizman & Duran, 1992; Mouquet, Aymard, Guilbert, Cuvelier, & Launay, 1997; Nussinovitch, Kopelman, & Mizrahi, 1991), probably due to the enhancement of polymerpolymer bonding. Sugar is capable of reducing solventpolymer interaction and thus increases polymerpolymer attraction, but seems to cause a decrease in gel homogeneity at high concentrations (Nussinovitch et al., 1991). Glycerol is a short chain, low molecular weight (94.04 g/mol) polyol used in food systems with the objective of removing or immobilizing free water so as to lower the water activity (aw) to intermediate levels (Boyle, Sofos, & Schmidt, 1993). ment, and Cheftel (1981), studying different Guilbert, Cle types of solutes as aw suppressors, observed that glycerol

0023-6438/$30.00 r 2006 Swiss Society of Food Science and Technology. Published by Elsevier Ltd. All rights reserved. doi:10.1016/j.lwt.2006.05.002

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showed the additional advantage of making a positive contribution to the organoleptic quality (texture) of pectin gel, and conferring plasticity to the product. Response surface methodology (RSM) (Barros Neto, Scarminio, & Bruns, 2002; Box, Hunter, & Hunter, 1978) is a tool frequently used in the optimization of food processing parameters. It is based on the simultaneous variation of several factors (independent variables), previously selected for their suspected inuences on a determined parameter (dependent variables or response). Using mathematical and statistical techniques, the experimental results indicate the combination of levels of the variables, which would optimize the response in a given situation. The objective of this work was to investigate the process parameters for the structuring of concentrated pineapple pulp, evaluating the effects of mixtures of alginate, pectin and glycerol on the characteristics of fruit gels containing between 770 and 830 g/kg of concentrated pineapple pulp with an elevated solids level (501Brix). The formulation and processing to prepare restructured fruits with high solids contents used experimental statistical designs to obtain response surfaces optimizing the nal product properties: rmness, pH and water activity. A taste panel evaluated the sensory acceptance of a restructured fruit produced according to the formulation optimized by RSM. 2. Material and methods

sugar are shown in Table 1. The proportions of alginate, pectin and glycerol along with their codied and real values and following a central composite statistical design are shown in the same table. Initially glycerol was added to the CPP at a rate of 40200 g/kg and, based on the soluble solids content, the amount of sugar required to reach 501Brix, was calculated. This mixture, previously heated to 60 1C, was placed in a mixer-deaerater (Cunnington and Cooper Ltd., England) and the dry mixture of hydrocolloids (alginate+pectin) and sugar was added with mixing (390 rpm) under vacuum (88 kPa). After 10 min of mixing, 4 g of CaHPO4 was added per kg CPP, suspended in a minimal amount of distilled water (7 ml H2O), and mixed for a further 5 min. With the aid of 5 cm diameter Petri dishes (depth 1 cm) with a capacity for approximately 25 g sample, the restructured fruits were molded into the form of a solid cylinder with a volume of approx. 20 cm3, and maintained under refrigeration at 10 1C for 24 h to complete the gelling process. Cylindrical samples with a diameter of 1.5 cm were withdrawn from the restructured fruits using a 1.5 cm diameter stainless steel cork borer, and cut into 1 cm long pieces, giving them an appearance similar to that of wine gums. The gums were nally dried at 60 1C for 6 h with the objective of reducing the free water content and minimizing surface stickiness. The last two stages were only applied to those samples destined for the sensory evaluation. 2.3. Firmness measurements

2.1. Preparation of the concentrated pineapple pulp Pineapple pulp (pH 3.55, 12.51Brix), acquired on the local market, was vacuum concentrated (88 kPa) in a 30 l jacketed vat (Groen MGF Co., EUA) operating at 4045 1C. A low temperature was used in order to preserve the pigments, aromatic components and vitamins present in the pulps. The concentration level was monitored by periodic measurements of the soluble solids (1Brix) using a refractometer (Atago, Japan). The concentrated pineapple pulps (CPPs) obtained (pH 3.68, 391Brix) were used as the raw material in this work. 2.2. Restructuring process The procedure used to prepare the restructured pineapple fruit, as described by Grizotto, Aguirre, and Castle (2005), is shown in Fig. 1. The technological co-adjutants used to prepare the restructured pineapple fruit were commercial rened sugar (Unia o, Brazil), sodium alginate (Danisco Ingredients, Landerneau, France) and low methoxy pectin (3337% esterication) (Danisco Cultor Mexico, Mexico) as the food grade hydrocolloids, glycerol (C3H5(OH)3) (Synth, Brazil) as the solute used to suppress the water activity and anhydrous calcium hydrogen phosphate (CaHPO4) (Synth, Brazil, analytical grade) as the source of calcium. The 19 formulations tested using different proportions of CPP and Firmness of the restructured fruit was measured using a TA.XT2 texturometer (Stable Micro Systems, Godalming, EUA) with the 35 mm diameter cylindrical probe and 25 kg load cell, according to the methodology described in the TA.XT2 application manual SWTI/P35 (Stable Micro Systems, 1997). The TA.XT2 settings were: mode and operation force in compression, time 60 s, option hold until time, 1 mm/s test speed and 20 mm of distance from the sample. Once the trigger force of 5 g was attained, the maximum force was registered and the probe proceeded to compress the sample to 20% of its original height. It was held at this distance for 60 s and then withdrawn from the sample to its starting position. The rmness values, expressed in grams, represented the mean of three peaks of maximum force with their respective standard deviations (SD) expressed as percentages. The rmness measurements were carried out on three distinct samples, maintained in Petri dishes at room temperature. 2.4. Water activity, pH and soluble solids The experimental water activity was determined with a model CX-12 hygrometer (Aqualab, Decagon Devices Inc., USA) coupled to a constant temperature (2570.3 1C) water bath. The value obtained for the experimental water activity was corrected using the equation obtained by calibrating the instrument with solutions of known water

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Fresh Pineapple pulp (12,5Brix; pH 3,55)

Concentration (40 - 45C; 88kPa)

Glycerol (40 to 200g/kg)

Concentrated pineapple pulp (39Brix; pH 3,68)

Formulation Hydrocolloids + Sucrose + CaHPO4 (4g/kg) Heating in water bath to 60C

Mixture/Deaeration (390rpm; 81kPa)

Formulated pulp with appr. 50Brix

Molding in pieces (volume 20cm3) Optional

Cutting in pieces (volume 20cm3)

Drying the pieces (60C/6h)

Restructured fruit

Fig. 1. Process ow sheet for the production of intermediate moisture content restructured fruits. The stages of cutting and drying of the pieces are optional and were only used to prepare material for the sensory acceptance test.

activity. The pH was determined using a potentiometer according to AOAC method no. 42.1.04 and soluble solids using the AOAC refractometric method no. 42.1.10 (Cunniff, 1998). 2.5. Date analysis of the experimental designs The restructuring process for the pineapple pulp was optimized by RSM as described by Box et al. (1978) and Barros Neto et al. (2002). The results obtained from the central composite design, composed of a 23 factorial design with a central point and the corresponding star

design, were modeled using multivariate linear regression techniques. The centre point trial was repeated ve times to provide an estimate of the experimental error. A total of 19 trials were performed, allowing for the evaluation of three factor linear and quadratic models. The lack of t of the model was investigated by performing F tests of the standard analysis of variance (ANOVA) results, and t-tests of the model co-efcients relative to their standard errors were made to determine statistically signicant model parameters. The calculations were done using the Statistic 6.0 commercial package (Statsoft, Inc.).

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762 R.K. Grizotto et al. / LWT 40 (2007) 759765 Table 1 Results of the central composite design trials for rmness, pH and water activity of the restructured pineapple fruit prepared with different concentrations of concentrated pineapple pulp (391Brix) and sugar Trial CPPa Sugarb Variables in laboratory units (g/kg of CPP) Pectin [P] 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19
a b

Codied variablesc X1 X2 X3

Responses Firmness (g) 95.27 451.80 753.77 1611.83 58.60 306.93 669.37 1723.07 148.7 1076.2 45.3 1529.3 655.1 585.9 565.8 515.1 745.53 790.60 688.37 pH Water activity 0.895 0.896 0.908 0.826 0.835 0.890 0.895 0.869 0.898 0.893 0.897 0.895 0.922 0.858 0.894 0.890 0.892 0.893 0.895

Alginate [A] 4 4 16 16 4 4 16 16 10 10 0 20 10 10 10 10 10 10 10

Glycerol [G] 40 40 40 40 160 160 160 160 100 100 100 100 0 200 100 100 100 100 100

830 830 830 822 792 785 785 778 808 795 808 795 835 771 802 810 810 810 810

140 140 140 140 90 90 90 90 123 123 123 123 173 73 123 123 123 123 123

4 16 4 16 4 16 4 16 0 20 10 10 10 10 10 10 10 10 10

1 1 1 1 1 1 1 1 1.68 1.68 0 0 0 0 0 0 0 0 0

1 1 1 1 1 1 1 1 0 0 1.68 1.68 0 0 0 0 0 0 0

1 1 1 1 1 1 1 1 0 0 0 0 1.68 1.68 0 0 0 0 0

3.71 3.72 3.72 3.92 3.70 3.67 3.94 3.93 3.37 3.36 3.24 3.42 3.28 3.39 3.33 3.31 3.89 3.93 3.88

CPP concentrated pineapple pulp with 39oBrix, in grams per kilogram of restructured fruit. % Sugar in grams per kilogram of CPP. c x1 P 10=6; x2 A 10=6; x3 G 100=60.

Table 2 Restructured pineapple fruit used in the sensory evaluationformulation Ingredient Concentrated pineapple pulp Sugar Alginate Low methoxy pectin Glycerol CaHPO4 Water CPP concentrated pineapple pulp with 351Brix. Amount (g/kg) 735 210 20 10 100 4 7 (wt (wt (wt (wt (wt (wt (wt of of of of of of of product) CPP) CPP) CPP) CPP) CPP) CPP)

analysed using a frequency histogram, that is, scores for acceptance against percentage of panelists. 3. Results and discussion The restructuring procedure proposed here allowed for the simultaneous use of a high level of pineapple pulp (770830 g/kg) and a minimal quantity of sucrose (7317 g/ kg) as established for the nineteen trials according to the RSM (Table 1). The quantity of sucrose used in this work was well below the quantity (300400 g/kg) needed to restructure mango pulp (Mouquet, Duma, & Guilbert, 1992), grape and apple pulp (Kalentuc et al., 1990) and orange, banana and apricot pulps (Nussinovitch et al., 1991). The high concentration of pineapple pulp attained (391Brix) and the addition of glycerol permitted the addition of only a small amount of sucrose in order to raise the soluble solids level to 501Brix. The addition of the minimum amount of glycerol (40 g/kg of CPP) resulted in an increase of about 8% in the soluble solids level of the CPP, requiring the addition of 140 g of sucrose per kg of CPP to reach 501Brix. On the other hand the addition of the maximum amount of glycerol (200 g/kg CCP) resulted in an increase of 20% in the soluble solids level of the concentrated pulp, requiring an even smaller amount of sucrose (73 g sucrose/kg CPP) to reach 501Brix. The glycerol acted as a water activity suppressor independent of the amount added, lowering the aw from 0.922 (without glycerol) to approximately 0.87, within the intermediate

2.6. Sensory acceptance evaluation Thirty potential consumers of the product evaluated the acceptance of the partially dehydrated structured fruit showing a moisture content of about 20% (w.b.), and the formulation is presented in Table 2. The formulation was based on the trial 12 of the experimental design (Table 1), that resulted gels with good rmness (1.5 kg) using the smallest total amount of hydrocolloids (10 g pectin+20 g alginate) per kilo of product. The amounts of sugar and concentrated pulp had to be adjusted to the specic concentration of the pulp (351Brix) used to prepare the samples. The panel members registered how much they liked or disliked the sample on a seven-point hedonic scale, with seven representing liked very much and one representing disliked very much. The scores were

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moisture range. This fact, together with the possibility of high levels of glycerol (200300 g/kg) negatively affecting the avour of the product (Boyle et al., 1993), led to the choice of an intermediate level of glycerol, that is, 100 g/kg (based on the concentrated pulp), to prepare the intermediate moisture structured fruit destined for the acceptance evaluation. A reduction in the level of exuded liquid due to syneresis, probably due to the high pulp concentration (371Brix) and presence of glycerol, was observed visually, facilitating the reduction in free water. Before drying, the structured fruits before showed a moisture content of about 30% and mean water activity of 0.884, a value within the range of 0.650.90 established by Chirife and Buera (1994) for intermediate moisture foods. After drying the moisture was 20% (w.b.) and favoured the external pellicle, contributing to the formation of a kind of skin and dening the nal texture of the structured fruits. Table 1 presents the results for rmness, pH and water activity of the restructured pineapple fruits obtained from the central composite design trials. The real levels and their corresponding codied levels are also given. The modeling and statistical analyses of each of these response values are presented below. 3.1. Firmness Linear and quadratic models were tted to the rmness data in Table 1. The quadratic model, ^ 659:7 298:5x1 464:3x2 19:8x3 y
52:4 31:7 31:7 31:7

2 9:8x2 1 52:0x2 31:7 31:7 41:5

7:0x2 3 163:4x1 x2 41:5 31:7 R2 0:98 1

resulted in an interval of 38.77173.8 g. Since this interval contained the zero value, the null hypothesis that the glycerol level does not affect rmness was accepted. Furthermore the results for trials 13 and 14 (656.1 and 585.9) are similar to the rmness values obtained for the centre point ve-fold replicate results (565.8, 515.1, 745.5, 790.6 and 688.4). The rmness of restructured pineapple fruit varies with the alginate and pectin concentrations. As their concentrations are increased, so the rmness values increase. This is to be expected, since the signicant terms, x1 and x2, in the model had positive signs and indicate that increasing the alginate and pectin levels could increase the rmness of the restructured fruit. The x1x2 interaction conrms the existence of a synergic effect between these hydrocolloids, as pointed out by Mancini and McHugh (2000). The glycerol concentration was not included in the nal model, since all the terms containing x3 in Eq. (1) are not statistically signicant at the 99% condence level. In general, the rmness of the restructured pineapple increased 2.6 times when the pectin concentration was increased from 4 to 16 g/kg. Alginate, on the other hand, was even more effective, increasing rmness values 5.7 times for the same increase in concentration. The observed rmness values were randomly distributed close to the line of the values predicted by the quadratic model in Eq. (1). This distribution represents complete agreement, showing that the experimental designs and process modeling were adequate to optimize the structuring process of CPP under the conditions established in this study. 3.2. pH Both the linear and quadratic models showed a good t with the pH values that ranged from 3.24 to 3.93, as shown in Table 1. Both the standard error calculation and ANOVA showed there were no signicant terms in either model, implying that the hydrocolloids and glycerol concentrations have no inuence on the pH of the structured fruit. This is understandable since the mean and SD for trials 114, which had varying factor levels, were 3.6070.25, whereas the same values for the ve-fold replicate centre point were 3.6770.32. The SD for the replicate points is about the same as that for trials 114 for which the factor levels varied extensively, hence the SD for the factorial and star designs can simply be explained by the experimental error. Furthermore, the difference in average values is much smaller than either SD, indicating that all the trials in the central composite design belonged to the same statistical population. The results obtained in experiments 4 and 8 (Table 1) show that those structured fruits with the highest rmness values (1.7 kg) presented pH values around 3.9 and were obtained using maximum quantities of alginate and low methoxy pectin (16 g/kg). Thus the 3.9 pH

10:9x1 x3 26:0x2 x3
41:5

proved to be superior to the linear one since the x1, x2 cross term was signicant. All the quadratic terms and the other cross terms in x1, x3 and x2, x3 were not signicant at the 95% condence level. The ANOVA results conrmed the statistical signicance of the terms x1, x2 and x1x2 in Eq. (1). Since no terms in x3 were signicant, a simplied model for x1 and x2 can be used to represent the experimental data, ^ 659:7 298:5x1 464:3x2 163:4x1 x2 y R2 0:97. (2)

The validity of this two-factor model can be veried using the data in Table 1. If the different levels of factor 3, the glycerol concentration, did not affect the rmness values, one would expect similar values, within the experimental error, for the 15, 26, 37 and 48 pairs of trials. The rmness results for these pairs, (95.3, 58.8), (451.8, 306.9), (753.8, 669.4) and (1611.8, 1723.1) conrm this interpretation. Each pair has identical alginate and pectin levels, but the glycerol levels are 40 and 160 g/kg. A paired comparison calculation at the 95% condence level

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value can be taken as a minimum value for structuring acid pulps when mixtures of low methoxy pectin and alginate are used. 3.3. Water activity In contrast to the pH data the water activity values were very sensitive to changes in the factor levels. The linear and quadratic models showed very signicant lack of t indicating that these simple models were not capable of describing the variations in water activity. The average and SDs, 0.88470.027, for trials 114 and 0.89370.002 for the ve-fold replicate centre point, showed much larger variations in water activity when the factor levels were varied than for the replicate trials. The 0:02732 = 0:00202 186:3 calculated F ratio is much larger than that of the 95% condence level value of 5.87 for 14 and 4 degrees of freedom, indicating different populational variances for these two groups of experiment. However the functional dependence of water activity on the pectin, alginate and glycerol concentrations is too complex for the simple models usually employed in RSM. Optimization of the restructuring process for CPP using Surface Response Methodology allowed for the denition of the process parameters, considering the concentrations of the hydrocolloids (alginate+pectin) and the glycerol. The use of a combination of hydrocolloids shows that rmness of restructured fruits can be achieved even without previous neutralization of the acid pulp with a NaOH solution, as required when alginate is used as gelling agent as proposed by Kalentuc et al. (1990) and Mouquet et al. (1992). These results provide a promising perspective for the production of restructured fruit from pineapple pulp. Restructured fruits with greater rmness can be obtained using maximum levels of alginate (16 g/kg) and pectin (16 g/kg) independent of the glycerol level. 3.4. Sensory acceptance The results of the sensory test indicated acceptance of the partially dried restructured pineapple fruit by the panel members. The product obtained mean acceptance scores of 5.5, between the terms liked slightly and liked moderately on the hedonic scale. In addition, more than 80% of the panelists preferred the product by giving it a score of 5 (liked slightly) or higher. Some panelists made the following negative comments: product too soft and sticky, too little pineapple aroma and acidic taste. No comments were made about undesirable or offavors, specically those that could be related to the presence of glycerol, such as bitterness or a slight burning sensation. Drying of the restructured pineapple fruit probably resulted in evaporation of the glycerol, as reported by Favetto, Chirife, and Bartholomai (1979).

4. Conclusions The results of the central composite design show the viability of restructured fruit production with a high level of CPP (735 g/kg) and low quantity of sucrose (210 g/kg). Glycerol was the solute used to suppress the water activity of the restructured products during the optimization process using the central composite design, in addition to substituting part of the sucrose incorporated into the fruit pulp. The use of mixtures of hydrocolloids minimized the effect of pH, considered to be an important factor in the restructuring process of acidic fruits. A pH of around 3.9 can be taken as a minimum value for structuring acid pulps when mixtures of low methoxy pectin and alginate are used. From the central composite design, the alginate (x1) and pectin (x2) variables were shown to be statistically signicant for the objective of increasing product rmness. Restructured fruits with greater rmness were obtained employing maximum levels of alginate (16 g/kg) and pectin (16 g/kg), independent of the glycerol level. There were no signicant terms in either the linear or quadratic models tted to the pH values determined in the restructured pineapple fruit. The difference in average values could only be explained by experimental error. The water activity values were very sensitive to changes in factor levels, but the functional dependence of water activity on pectin, alginate and glycerol concentration was too complex for the simple models employed in RSM. The partially dried restructured pineapple fruit obtained good sensory acceptance, although some panelists considered the texture too soft and sticky and commented on the lack of pineapple aroma and the acidic taste.

Acknowledgments RKG and JMA thank FAPESPFundac -a o de Amparo ` Pesquisa do Estado de Sa a o Paulofor a post-doctoral fellowship and research Grant, respectively.

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