MASS TRANSFER KINETICS OF OSMODEHYDRATED GUAVAS: EVALUATION OF VACUUM PULSE J. L.G. CORRÊA1*, L. M. PEREIRA2, G.S. VIEIRA2 and M.D. HUBINGER2 1* Depart. Food Science, Federal University of Lavras, 37200-000, Lavras, MG, Brazil, [email protected] 2 Depart. Food Engineering, Faculty of Food Engineering, State University of Campinas, 13083-862, Campinas, SP, Brazil, [email protected] Abstract: The influence of vacuum pulse and solution concentration on mass transfer of osmotically dehydrated guavas (Psidium guajava L) were studied. Kinetics of water loss (WL) and solid gain (SG) were obtained using sucrose solutions at 40; 50 and 60 ºBrix and vacuum pulse of 100 mbar for 0; 10 and 15 min at the beginning of the process. Kinetic data were obtained until 300 min for all process condition studied. The experimental data were fit with Fito’s hydrodynamics model in order to obtain diffusivity coefficients. An effective influence of concentration and vacuum pulse on the WL and SG was observed. Fito’s model carried out to good agreements. Keywords:.PVOD, sucrose concentration, dehydrated fruits, HDM 1. INTRODUCTION Osmotic dehydration of fruits is a process that carries out to small differences of sensorial properties with respect to the product in natura. It can be performed at atmospheric pressure (OD) or with vacuum pulse (PVOD). PVOD process consists on immersion of the product in a hypertonic osmotic solution (OS) with the application of sub-atmospheric pressure for a small period at the beginning of the process. After this, the osmotic process is developed at atmospheric pressure. Several works were published considering PVOD of fruits (Fito, 1994; Giraldo et al., 2003; Chafer et al., 2003; Panadés et al., 2006; Ito et al., 2007; Deng et al., 2008; Moraga et al., 2009) and most of them reported the improvement on product quality in a PVOD with respect to OD products. Among the available mathematical models to describe osmotic dehydration, the most used approach is based on the Fick diffusion law (Shi and Maguer, 2002). In PVOD process, it was demonstrated that the consideration of hydrodynamics process coupled with Fick’s diffusion law results in best agreements (Fito, 1994; Fito and Chiralt, 1997). In the present work, kinetics of WL and SG on mass transfer of guavas were studied at OD and PVOD conditions. Different sugar concentrations (40; 50 and 60 °Brix) and pulse vacuum time (0; 10 and 15 min) were analyzed and the experimental data obtained were fit with Fito’s hydrodynamics model. 2. MATERIAL AND METHODS 2.1 Material and samples preparation Red guava (Psidium guava L.) fruits were purchased in a local market (CEASA-Campinas, SP, Brazil) and selected based on a similar ripening grade (80% of skin yellowness) and soluble solids content of fruits (around 8 ºBrix) to minimize raw material differences. The fruits were washed with tap water and peeled manually. They were cut into halves and had the seeds removed. From each half, two slices of 0.05 m x 0.025 m was obtained, preserving the original guavas thickness (around 0.005 m). 2.2 Osmotic dehydration Osmotic dehydration tests were carried out on a jacketed stainless steel chamber designed to work at atmospheric pressure and/or under vacuum (Ito et al., 2007). The bath temperature was maintained at 40 ºC with a controlled thermostatic bath. The OS was stirred by a controlled flow recirculation system, performed by a turbine-type measurement device. Vacuum was obtained with a vacuum pump. The equipment (Figure 1) used was a pilot scale device with a minimum solution volume of 22 L. The ratio of weight product-to-weight solution was about 1:45 (w:w). Fig. 1. Pulsed vacuum osmotic dehydration equipment. For OD and PVOD treatments, guava slices were placed in a single layer on perforated metallic trays and immersed in the sucrose solutions at 40; 50 and 60°Brix, at 40°C. For treatments under vacuum, pressure of 100 mbar was applied to the system for the first 10 or 15 min of the osmotic process, afterwards restoring the atmospheric pressure. At predetermined times (15; 30; 60; 120; 180; and 300 min), samples were removed, rinsed with water, and placed on absorbent paper to remove excess solution. The samples were then weighed and analyzed in terms of water loss (WL) and solids gain (SG), according to Equations 1 and 2. The samples moisture content was determined according to AOAC (2007). WL(%) x 0w Mo0 x fw Mof Mo0 (1) 100 SG(%) o xST f Mf o xST 0 M0 Mo0 (2) 100 where Mo0 = initial sample weight (kg), Mof = final sample weight (kg), x 0w = initial moisture content (%), x fw = ST final moisture content (%), x ST 0 = initial solids content (%), and x f = final solids content (%). 3. MATHEMATICAL MODELING—DIFFUSION COEFFICIENTS The diffusion coefficients were estimated using the Fito Hidrodynamics model (Fito and Chiralt, 1997). This mathematical model considers an equilibrium approach (Equation 3): zSS ySS (3) SS where z is the mass fraction of soluble solids in the food and ySS is the mass fraction of soluble solids in the OS, both at equilibrium state. The variation on the Food Liquid Phase (FLP) composition is related to the hydrodynamic mechanism (HDM) at the very beginning of the process (t=0) and the dependency of the activity gradients, correspondent to the pseudo-diffusion mechanism (PDM) are modeled with Fick’s equation for semi-infinite slab and short time (Crank, 1975). These two effects were coupled by Fito and Chiralt (1997) to consider the effect of HDM at t = 0 (Equation 4), where Ytw PD, t 0 , the reduced driving force, is defined by equation 5, where Deff is the effective diffusivity, k would reflect the effect of mechanisms that are neither diffusional nor hydrodynamic, PD is pseudo-diffusion.and t is the time. 1 Ytw PD, t 0 2 Deff t t2 0.5 0.5 k (4) Ytw Ytw PD, t 0 Ytw HDM, t 0 zw t zw t yw zw t HDM yw y w / z0w yw (5) The effect of HDM on the FLP concentration was calculated by equation 6, where z w t is the calculated HDM, t 0 initial FLP concentration when the pseudo-diffusion mechanism (PDM) acts. zw t M o0 x 0w HDM, t 0 M o0 x 0w (1 )VX M o0 x ST 0 (1 It is supposed that z w t os y w )VX (6) os ≈ z 0w in the case of OD. In the case of PVOD, z w t HDM, t 0 HDM, t 0 ≠ z 0w due to the massive flux of OS because of the HDM action (Fito, 1994). V is the sample volume, X is the food volume fraction occupied by impregnating solution, γ is the relative volume deformation, os is the OS density, yw is the mass fraction of water in the OS, Mo0 is the overall mass sample, x 0w is the initial mass fraction of water, x ST 0 is the initial mass fraction of total solutes and The Deff and K parameters were obtained for each experiment from the linear fitting of the experimental 1 Ytw versus t0.5 PD, t 0 4. RESULTS AND DISCUSSION Figures 2 to 4 show the kinetics of WL with respect to solution concentration and pressure. It is possible to evaluate from such Figures that WL increased with solution concentration and vacuum pulse application. However, the solution concentration was more influent than vacuum pulse on guavas water loss. 60,0 Water loss [%] 50,0 40,0 30,0 20,0 10,0 0,0 0 100 200 300 Time [min] Atm 10 min vacuum 15 min vacuum Atm 10 min vacuum 15 min vacuum Fig. 2. Kinetics of water loss of guava slices osmotically dehydrated in sucrose solution at 40ºBrix. Atm: osmotic process at atmospheric pressure; 10 min and 15 mim vaccum: osmotic process with vacuum pulse application during 10 and 15 minutes, respectivelly. Water loss [%] 60,0 50,0 40,0 30,0 20,0 10,0 0,0 0 100 200 300 Time [min] Atm Atm 10 min vacuum 10 min vacuum 15 min vacuum 15 min vacuum Fig. 3. Kinetics of water loss of guava slices osmotically dehydrated in sucrose solution at 50ºBrix. Atm: osmotic process at atmospheric pressure; 10 min and 15 mim vaccum: osmotic process with vacuum pulse application during 10 and 15 minutes, respectivelly. 60,0 Water loss [%] 50,0 40,0 30,0 20,0 10,0 0,0 0 100 Time [min] 200 300 Atm 10 min vacuum 15 min vacuum Atm 10 min vacuum 15 min vacuum Fig. 4. Kinetics of water loss of guava slices osmotically dehydrated in sucrose solution at 60ºBrix. Atm: osmotic process at atmospheric pressure; 10 min and 15 mim vaccum: osmotic process with vacuum pulse application during 10 and 15 minutes, respectivelly. WL was favored by higher solution concentrations, due to the increase in the osmotic gradient. These results corroborates with the ones obtained by Ito et al. (2007) on PVOD of mango slices; Madamba and Lopez (2002) in OD of mango and Mastrantonio et al. (2005) in OD of guavas. WL was positively influenced by vacuum pulse application. This effect of vacuum pulse is due to the greater occupation of the internal spaces of the pores with the OS that occurs with application of vacuum. The use of vacuum pulse creates a larger interface surface available to mass transfer (Fito, 1994). Such trends were also observed in other works (Fito, 1994, Panadés et al., 2006; Deng and Zhao, 2008). Moreover, the influence of vacuum pulse was more evident in the higher solution concentrations, suggesting an interaction between these two variables. In most treatments, SG was negatively affected by OS concentration (Figures 5 to 7). The negative influence of solution concentration on SG is a consequence of a dense layer of sucrose at the surface, which acts as a barrier against solutes penetration and makes mass transfer more difficult (Mastrantonio et al., 2005). The results obtained are also similar to the ones of Barat et al. (2001), Madamba and Lopez (2002), Mastrantonio et al. (2005) and Ito et al. (2007). It is important to note that a negative influence on SG is highly desirable in an osmotic dehydration process. It results in a smaller change on the fruit composition. With respect to the influence of vacuum pulse, it was directly proportional to solid gain (Panadés et al., 2006; Ito et al., 2007; Deng and Zhao, 2008) and was more evident at lower solution concentrations, showing again a possible interaction between these two variables. This behavior can be explained by two different factors: the occupation of the internal spaces of the guavas pores with the osmotic solution due to the application of vacuum favoring the SG and the formation of a dense layer of sucrose at the surface with the increase of solution concentration, acting as a barrier against solutes penetration. Solid gain [%] 25,0 20,0 15,0 10,0 5,0 0,0 0 100 200 300 Time [min] Atm Atm 10 min vacuum 10 min vacuum 15 min vacuum 15 min vacuum Fig. 5. Kinetics of solid gain of guava slices osmotically dehydrated in sucrose solution at 40ºBrix. Atm: osmotic process at atmospheric pressure; 10 min and 15 mim vaccum: osmotic process with vacuum pulse application during 10 and 15 minutes, respectivelly. Solid gain [%] 25,0 20,0 15,0 10,0 5,0 0,0 0 100 200 300 Time [min] Atm Atm 10 min vacuum 10 min vacuum 15 min vacuum 15 min vacuum Fig. 6. Kinetics of solid gain of guava slices osmotically dehydrated in sucrose solution at 50ºBrix. Atm: osmotic process at atmospheric pressure; 10 min and 15 mim vaccum: osmotic process with vacuum pulse application during 10 and 15 minutes, respectivelly. Solid gain [%] 25,0 20,0 15,0 10,0 5,0 0,0 0 100 200 300 Time [min] Atm 10 min vacuum 15 min vacuum Atm 10 min vacuum 15 min vacuum Fig. 7. Kinetics of solid gain of guava slices osmotically dehydrated in sucrose solution at 60ºBrix. Atm: osmotic process at atmospheric pressure; 10 min and 15 mim vaccum: osmotic process with vacuum pulse application during 10 and 15 minutes, respectivelly. In a general way (Figures 2 to 7), could be observed that the behavior of WL and SG of guavas osmotically dehydrated with the application of vacuum pulse during 10 minutes at the beginning of the process were very similar to the ones processed at atmospheric pressure conditions. Moreover, the main differences between OD and PVOD treatments occurred only after 120 min of treatment, as also observed by Ito et al. (2007). For the process conditions studied, it was also observed that the sucrose solution concentration is a more influent variable on kinetics of osmotically dehydrated guavas than vacuum pulse. Table 1 shows that the values obtained with Fito’s hidrodynamics model for Deff ranged from 0.64 to 2.20 x10-10 m2s-1. An increase on effective diffusivity could be observed with the decrease of OS concentration and the increase of vacuum pulse time, although of some divergences observed with treatments at 50 °Brix. This tendency was also observed by Fito et al., 2001; Barat et a., 2001; Chafer et al., 2003 and Giraldo et al., 2003. Table 1. Effective diffusivities for water and solids Condition Deff x1010 [m2s-1] r2 40 ºBrix, atm 1.18 0.9414 40 ºBrix, 10min vacuum pulse 2.20 0.9526 40 ºBrix, 15min vacuum pulse 2.20 0.9354 50 ºBrix, atm 1.23 0.9459 50 ºBrix, 10min vacuum pulse 1.08 0.9937 50 ºBrix, 15min vacuum pulse 1.54 0.9662 60 ºBrix, atm 0.64 0.9637 60 ºBrix, 10min vacuum pulse 0.71 0.9538 60 ºBrix, 15min vacuum pulse 1.38 0.9894 Higher Deff with vacuum pulse application is promoted due to the substitution of gas volume in the intercellular spaces by liquid phase, where solutes and water can be transferred (Giraldo et al., 2003). The reduction of Deff with increase of OS concentration may be explained by the different induced viscosity in the free liquid phase occupying intercellular spaces after the vacuum pulse (Giraldo et al., 2003) and due to the formation of a dense layer of sucrose at the surface, which will affect the diffusion. 5. CONCLUSIONS An effective influence of OS concentration and vacuum pulse on WL and SG of osmotically dehydrated guavas was observed. Diffusivity values, obtained by Fito’s hydrodynamics model, varied from 0.64x10-10 m2s-1 to 2.20 x10-10 m2s-1, and good agreements was obtained using the mathematical model with r2 higher than 0.93 for all the studied treatments. A tendency to increase the effective diffusivity was observed with the decrease of OS concentration and increase of vacuum pulse time. 6. ACKNOWLEDGEMENTS The authors are grateful to FAPEMIG (Process 548/08), FAPESP (Process 2001/13809-5 and Process 06/598901) and CNPq for the financial support. 7. REFERENCES A.O.A.C. (Association of Official Analytical Chemists). Official methods of analysis (18th ed.). AOAC International, 2007. Barat, J.M., Chiralt, A., and Fito, P. (2001). Effect of osmotic solution concentration, temperature and vacuum impregnation pretreatment on osmotic dehydration kinetics of apple slices. 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