Progressive freeze concentration of orange juice in a pilot plant falling film

In the present study the cryoconcentration of orange juice was investigated, using a pilot plant unit for cryconcentration of liquids using a cold surface. The evolution in time of the concentration of solids in the juice and in the ice was analyzed during the process. It was found that the concentration of solids in the juice showed a linear increase in time at a rate of 0.75 °Brix/h until a final concentration of 28.8 °Brix. The concentration of solutes in the ice showed an exponential increase.Industrial relevanceThe freeze concentration allows dewatering orange juice at temperatures below the water's freezing point, which allows obtaining products of better quality. The freeze concentration is a technology that allows eliminating water from the juices at temperatures below the water's freezing point, which allows obtaining products of better quality. This work has applied this technology to concentrate orange juice, obtaining promissory results.     

Calculation process for the recovery of solutes retained in the ice in a multi-plate freeze concentrator: Time and concentration

Fractionated thawing was studied as a method to recover solutes incorporated in the ice obtained in a cryoconcentrator. Thawing times and solute concentration in the ice were determined at several thawing temperatures.Ice sheets used for the thawing studies were obtained by cryoconcentrated solutions of sugars and simulated juice at initial concentrations of 5 to 20 °Brix. The ice sheets produced contained levels of solutes between 1.0 and 9.0 °Brix.Fractionated thawing was performed at temperatures of 20 to 30 °C while maintaining geometrical similarity for the test samples. By fractionated thawing more than 60% of the solutes retained in the ice was recovered in 34%, of the total thawing time.The procedure presented allows the determination of the solute concentration achieved in the various thawing fractions and predicts the thawing time required for a given form factor, melting temperature and the solute mass fraction in the ice.Industrial relevanceThe freeze concentration is a technology that allows eliminating water from liquid foods at temperatures below the water's freezing point, which allows obtaining products of better quality. Fractionated thawing was studied as a method to recover solutes incorporated in the ice, improving the global efficiency of a freeze concentration process by optimal recovery of the solutes retained in the ice. It also provides estimations of the energy used for thawing. This work continues the research in falling film freeze concentration technology which we have submitted and published in this journal. This work contributes to increase the global process efficiency.     

Dynamics of the loss and emergence of volatile compounds during the concentration of cashew apple juice (Anacardium occidentale L.) and the impact on juice sensory quality

Concentrating cashew apple juice alters the beverage aroma and flavor, compromising consumer acceptability of the concentrated beverage. To understand the mechanisms involved in these changes, this research characterized the dynamics of the loss and emergence of volatile compounds during cashew apple juice concentration, reporting their impact on beverage sensory quality. Fresh cashew apple juice (10.3°Brix) was concentrated in a thermal-siphon type evaporator operating in a closed system. Five samples were taken throughout the concentration process with the following soluble solids contents: 11.8°Brix, 14.9°Brix, 20.2°Brix, 29.6°Brix and 42.1°Brix. Trained judges rated the aroma note intensities, described as “fresh cashew apple” and “cooked” as perceived in the fresh and concentrated beverages. The headspace volatiles of the six samples were identified and quantified by GC–MS. The results indicated the esters as the major component in the fresh juice (226.46 μg kg^− 1) representing 45.0% of the total mass of volatiles, followed by the terpenes (118.98 μg kg^− 1), acids (45.23 μg kg^− 1), aldehydes (39.10 μg kg^− 1), alcohols (18.91 μg kg^− 1), lactones (19.15 μg kg^− 1), hydrocarbons (18.02 μg kg^− 1) and ketones (11.05 μg kg^− 1). Predictive statistical models (R² > 0.956, p ≤ 0.002) revealed that on reaching 14.9°Brix, the ester concentration declined more than 90%, the terpene content almost 100%, alcohols 85%, aldehydes 80% and hydrocarbons 90%. At 14.9°Brix, the intensity of “fresh cashew apple” aroma still predominated in the juice, but the panelists detected the presence of a weak “cooked” aroma. Concentration of the beverage to 20.2°Brix or above expressively increased the cooked aroma intensity and the concentration of hydrocarbons, alcohols and some aldehydes usually associated with off-flavors such as pentanal and decanal. This raises the possibility that some of these compounds might have been formed during juice processing. Juice with better sensory quality could possibly be obtained by concentrating the beverage to levels below 20.2°Brix, recovering the esters that evaporated off the juice until ~ 15°Brix is reached, and re-adding them to the juice concentrated.     

Processing of clear and turbid grape juice by a continuous flow UV system

The inactivation of inoculated (S. cerevisiae) and spoilage microorganisms, i.e. yeasts and lactic acid bacteria (LAB), in clear and turbid grape juice was investigated using a pilot scale UV system. The biodosimetry method was used for UV dose prediction in a continuous flow UV reactor. Weibull model was applied for fitting the inactivation data. The flow rates (774, 820 ml/min) in this system were very close to the ones used in fruit juice processing. S. cerevisiae in clear juice was reduced by 3.39 ± 0.04 at 65.50 mJ/cm² of UV dose. 1.54 ± 0.04 and 1.64 ± 0.03 log CFU/ml reductions were obtained for spoilage yeasts and LAB in turbid juice at UV dose of 78.56 and 67.97 mJ/cm², respectively. The soluble solids (°Brix) and pH of grape juice samples were not affected by UV-C treatment (p > 0.05). Although the color parameters slightly were changed after irradiation, the color of PCGJ and FSTGJ did not show visual difference compared to the untreated samples.Industrial relevanceUV light has a potential to reduce the levels of microbial contamination in liquid foods. Although grape juice has many beneficial health effects, it has a fairly short shelf life. Therefore, pasteurization is required. But the thermal pasteurization has some undesired effects on the juice quality. Consumer demands for high quality fruit juice with fresh-like characteristics have markedly expanded in recent years. In the current study, the microbial inactivation efficiency of a pilot scale UV system for non-thermal treatment of clear and turbid grape juice was evaluated under conservative conditions. Most of the physicochemical properties of grape juice samples were not significantly affected from UV-C treatment (p > 0.05). This would be a major advantage in the processing of nutritious juice products.     

Vacuum-assisted block freeze concentration applied to wine

Vacuum is an assisted technique to improve the efficiency of freeze concentration process, and wine is an interesting raw material to be concentrated. In this study reported the vacuum-assisted block freeze concentration to force the separation of solutes from a frozen wine sample. By applying vacuum (40 kPa), the solids content in the concentrated fraction increased significantly compared to the initial value (8°Brix), reaching a value near of 21°Brix after 5 min, although decreasing over time, indicated that the concentrated extract was collected mostly in the first fractions. The efficiency achieved high values near of 90% in a short time (15 min, 45 ml of initial sample), with high values of ice purity over time of suction. The pH, alcohol, acidity and total polyphenol content increased significantly in the concentrated sample (50% of concentrate) compared the fresh wine. The color evaluation indicating that cryoconcentrate (50% of concentrate) was darker than the initial sample, with a ΔE* value > 40 CIELAB units. The vacuum-assisted block freeze concentration applied to wine is an effective technique to obtain a concentrated sample with attractive properties for possible gastronomic use.Industrial relevanceThe vacuum assisted block freeze concentration allows producing wine concentrates with attractive properties, such as a high solid content, darker color and higher alcohol content than the initial sample. In this work has applied vacuum (40 kPa) as an assisted technique to improve the efficiency of block freeze concentration applied to wine, obtaining promissory results.     

Effect of freezing under electrostatic field on selected properties of an agar gel

The objective of this study was to investigate the effects of electrostatic freezing on the quality attributes of freeze-thaw agar gel. Agar gels were frozen under static electric field 0–5.8 × 10⁴ V m^− 1 at − 20 °C. Freezing rate and energy consumption were monitored during the freezing process and microstructures of the formed ice crystals were also analyzed by light microscopy techniques. Agar gel quality changes (syneresis and texture) were evaluated after thawing the frozen samples at + 4 °C. Results showed that the energy used by a DC high voltage generator was negligibly small as compared to the energy consumption by a freezer, and the freezing rate was not significantly influenced by electrostatic freezing (ESF). ESF also reduced the size of ice crystals but did not cause obvious changes in syneresis and texture of the samples.Industrial relevanceThe effects of electrostatic field freezing on the quality attributes of agar gel have been investigated. The results showed that the electrostatic freezing can be used as a potential tool to improve the microstructure of foodstuffs during freezing.     

Effect of static electric field on ice crystal size reduction during freezing of pork meat

The objective of this research was to evaluate the influence of static electric field (SEF) on the freezing of pork meat (pork tenderloin muscle) with respect to the size of ice crystal formulation. The results showed that by increasing the strength of the static electric field, the degree of supercooling was reduced. The measured degree of supercooling varied from 3.93 ± 1.3 °C to 1.92 ± 1.45 °C for the control and the frozen sample under 12 kV SEF, respectively. Meat microstructure was investigated after Carnoy fixation of the frozen tissues. The overall relative surface of the ice crystals was unchanged. The average equivalent circular diameter of the ice crystals was significantly reduced with increasing SEF; values from 32.79 ± 4.04 μm for the control to 14.55 ± 8.20 μm for the sample frozen at the maximum magnitude electric field which was tested were observed respectively. These findings demonstrate clearly the advantage of freezing under SEF which appears as a promising and innovative freezing process for food systems.Industrial relevanceThe reduction of freeze damage exerted to any tissue undergoing freezing remains a challenge. The mechanical and biochemical stress caused by the ice crystals to the cellular membranes results in irreversible tissue damage. Freezing under static electric field (SEF) has been identified as a possible means to reduce the size of ice crystals during freezing of biological tissues. In the present study SEF was applied during freezing of pork meat. Our results indicate that the size of the formed ice crystals was significantly reduced under SEF freezing leading to a lower damage on the microstructure of meat. This paper describes an innovative freezing process that could be used in order for higher quality frozen products to be produced.     

“Ice” juice from apples obtained by pressing at subzero temperatures of apples pretreated by pulsed electric fields

The impact of apple pretreatment by pulsed electric field (PEF) on juice extraction using the freezing-assisted pressing was studied. Apple discs were PEF pretreated at electric field strength of E = 800 V/cm and then air blast frozen inside the freezer (− 40 °C). Then, pressing experiments in a laboratory-pressing chamber (2–5 bars) were started at sub-zero temperature (− 5 °C). Time evolution of juice yield and its nutritional qualities were compared for PEF and untreated apple samples. High improvements of juice yield were obtained for freeze-thawed (FT) and PEF + FT samples. The combination of PEF + pressing (5 bar) at sub-zero temperature gave optimum results for juice extraction with high levels of carbohydrates, and antioxidant bioactive compounds. At fixed value of extraction yield, Y, PEF pretreatment improved nutritional parameters. E.g., at Y = 0.6, an increase in °Brix (by ≈ 1.27), carbohydrates (by ≈ 1.42), total phenolic compounds (by ≈ 1.16), flavonoids (by ≈ 1.09) and antioxidant capacity (by ≈ 1.29) was observed after PEF pretreatment.Industrial relevancePressing constitutes one of the most commonly used technologies at industrial scale to obtain fruit juices. However, during the pressing some undesirable chemical, physical and biological changes may occur in juices, thus reducing their nutritional and sensorial properties. For instance, the use of freezing-assisted pressing is a promising technique for the production of juice concentrates rich in sugars and other solids as the low temperature operation prevents undesirable modifications. But this method is rather expensive and requires strong control of the quality of “ice” juices, their sensory and compositional profiles. Thus, there is an increased search for obtaining new efficient methodologies for producing high quality juices. In this line, PEF-assisted pressing has been shown as a useful technology to increase juice yield. Therefore, the combination of PEF-assisted “ice” juice extraction by pressing of fruits at subzero temperatures may be a useful tool to improve the extraction yield of juices, thus improving their nutritional, physicochemical and sensorial properties.Keywords: “Ice” juice, Apple, Pulsed electric fields, Freezing-assisted pressing     

Effects of freezing treatments on the fermentative activity and gluten network integrity of sweet dough

The effect of freezing treatments on sweet dough was studied. The dough was frozen at ?20 °C, ?30 °C and ?40 °C in air-blast freezer cabinet and by immersion in liquid nitrogen. The yeast viability, gassing power, dough volume and dough network integrity from fresh and thawed sweet doughs were assessed. The results showed that both parameters depend on the freezing rate, which controls ice crystals size and location. Dough volume loss after freezing was attributed to reduced yeast fermentative activity and gluten network alteration in frozen dough. Fermentative activity reduced significantly in frozen dough using liquid nitrogen, causing 70% decrease on yeast population. Gluten integrity seemed to be affected by slow freezing treatment, i.e. ?20 °C and ?30 °C. Gas loss was also evaluated as a decrease of 25% ± 2 in dough volume. A correlation was observed between the freezing rate and osmotic pressure effects which influence strongly the yeast viability.     

Influence of freezing and dehydration of olive leaves (var. Serrana) on extract composition and antioxidant potential

In this work, the effect of the methods used for the freezing and drying of olive leaves on the polyphenol content and antioxidant capacity of the extracts was addressed. Thus, different methods were used to dry olive leaves (fresh or frozen by conventional (? 28 °C) or N₂ freezing): hot air drying at 70 or 120 °C and freeze drying. The extracts were characterized by determining the phenolic content, antioxidant capacity and HPLC-DAD/MS–MS profile.Drying had a significant (p < 0.05) influence on the antioxidant potential of olive leaf extracts. Both the drying and freezing methods significantly (p < 0.05) influenced the concentration of the main polyphenols identified. Hot air drying provided a higher phenolic content, especially in oleuropein, than freeze drying. Thus, drying at 120 °C was the best processing condition. Freezing reduced the antioxidant potential as compared to fresh leaves, probably due to oxidase activation, although its influence was not dependent on the freezing method.     

Investigation on the effects of microwave and conventional heating methods on the phytochemicals of pomegranate (Punica granatum L.) and black mulberry juices

Black mulberry and pomegranate juices were concentrated by conventional and microwave heating at different operational pressures (7.3, 12, 38.5, and 100 kPa). The effects of each heating method on the phytochemical changes (total anthocyanin content and antioxidant activity) of juices were investigated. The effect of various heating methods on the profile of the pomegranate anthocyanins were conducted using high-performance liquid chromatography–mass spectrometry (HPLC–MS). The main anthocyanins of pomegranate quantified by HPLC–MS were cyanidin, delphidin, pelargonidin, 3-glucoside, and 3, 5-diglucoside. In black mulberry juice, the final juice concentration of 42° Brix was achieved in 140, 120, and 95 min at 100, 38.5, and 7.3 kPa respectively and the final pomegranate juice concentration of 40° Brix was achieved in 140, 127, and 109 min at 100, 38.5, and 12 kPa respectively by using a rotary evaporator. Applying microwave energy decreased the required times to 115, 95, and 60 min for black mulberry juice and to 118, 95, and 75 min for pomegranate juice. Results showed that anthocyanin degradation and consequently decrease in antioxidant activity were more pronounced in rotary evaporation compared to microwave heating method.     

Flavanone glycosides in Brazilian orange juice

Authentic samples of oranges, frozen concentrated orange juice and pulp-wash, and retail samples of freshly squeezed orange juice and frozen concentrated orange juice have been collected in Brazil and analysed for the flavanone glycosides (FG) narirutin and hesperidin by reversed phase HPLC with UV detection at 280 nm. The juice from hand-squeezed fruit gave narirutin and hesperidin concentrations of 16–142 mg l⁻¹ and 104–537 mg l⁻¹, respectively. The ratio of hesperidin to narirutin showed varietal difference with Pera having the highest ratio (mean 8.4) and Baı́a the lowest (3.6). Frozen concentrated orange juice contained higher quantities of FG with narirutin ranging from 62 to 84 mg l⁻¹ and hesperidin from 531 to 690 mg l⁻¹ (after dilution to 12 °Brix). In frozen concentrated orange juice pulp-wash, the narirutin level ranged from 155 to 239 mg l⁻¹ and hesperidin from 1089 to 1200 mg l⁻¹. The analysis of 23 samples of freshly squeezed juice from the Brazilian market place showed that the FG content of most samples (9.1 to 94.8 and 105.8 to 586.6 mg l⁻¹, respectively, for narirutin and hesperidin) was similar to those found for authentic ones, indicating that these orange juices were not adulterated.     

Drying kinetics of grape seeds

Drying of grape seeds representing waste products from white wine processing (Riesling), red wine processing (Cab Franc), and juice processing (Concord) was studied at 40, 50, and 60 °C and constant air velocity of 1.5 m/s. Equilibrium moisture content had a significant effect on the normalized drying curve and was determined for each grape seed at each drying temperature. Effective moisture diffusivity ranged between 1.57 and 3.96 × 10⁻¹⁰ m²/s for Riesling seeds, 2.93–5.91 × 10⁻¹⁰ m²/s for Concord seeds, and 3.89–8.03 × 10⁻¹⁰ m²/s for Cab Franc seeds. The temperature dependence of the effective diffusivity followed an Arrhenius relationship, and the activation energies were 40.14 kJ/mol for Riesling seeds, 30.45 kJ/mol for Concord seeds, and 31.47 kJ/mol for Cab Franc seeds. Three thin-layer models were used to predict the drying curves: Page model, Lewis model, and the Henderson–Pabis model. All three models were found to produce accurate predictions compared to the mass average moisture loss for each grape seed variety (percent error less than 10%), and the Lewis model was shown to be an excellent model for predicting all three grape seed varieties (percent error less than 5%).     

Quality and filtration characteristics of sugar beet juice obtained by “cold” extraction assisted by pulsed electric field

Detailed comparison of various properties (concentration of soluble solids, purity, nature of impurities, coloration and filterability) of sugar beet juices obtained by pulsed electric field (PEF) assisted “cold” extraction (T = 30 and 50 °C) and classical “hot” extraction (T = 70 °C) was done. It was shown that application of PEF-assisted “cold” extraction results in lower concentration of colloidal impurities (especially, pectins), lower coloration and better filterability of juice. Concentration of various colorants and their intermediates decreased significantly with decreasing of the extraction temperature from 70 °C to 30 °C. Filtrate obtained by dynamic filtration of juice extracted with PEF treatment had a high purity (95.3 ± 0.4%) and low coloration (1.2×10³ IU). Obtained data suggest that PEF-assisted “cold” extraction is a promising method for preparation of sugar beet juices with high purity.     

Effects on Escherichia coli inactivation and quality attributes in apple juice treated by combinations of pulsed light and thermosonication

Pulsed light (PL) and Thermosonication (TS) were applied alone or in combination using a continuous system to study their effect on Escherichia coli inactivation in apple juice. Selected quality attributes (pH, °Brix, colour (L, a, b, ΔE), non-enzymatic browning (NEBI) and antioxidant activity (TEAC)) were also evaluated pre- and post-processing. Two PL (360 μs, 3 Hz) treatments were selected and the juice exposed to energy dosages of 4.03 J/cm² (‘low’ (L)) and 5.1 J/cm² (‘high’ (H)) corresponding to 51.5 and 65.4 J/mL, respectively. The juice was also processed by TS (24 kHz, 100 μm) at 40 °C for 2.9 min (L) or 50 °C for 5 min (H), corresponding to 1456 and 2531 J/ml energy inputs, respectively. The effect of the resulting four energy levels and sequence (PL + TS and TS + PL) was studied. When the technologies were applied individually the maximum reduction achieved was 2.7 and 4.9 log CFU/mL (for TS (H) and PL (H) respectively), while most of the combined treatments achieved reductions in the vicinity of 6 log CFU/mL, showing an additive effect for both technologies when acting in combination, regardless of the sequence applied. All treatments significantly changed the colour of apple juice and the sequence in which the technologies were applied affected colour significantly (P < 0.05). The energy level applied did not affect any of the measured quality attributes.     

Effects of combining ultraviolet and mild heat treatments on enzymatic activities and total phenolic contents in pineapple juice

Ultraviolet (UV) is able to inactivate most microorganisms in fruit juices with a low absorption coefficient but its effect is limited in inactivating undesired enzymes. The aim of this study was to overcome limitation of ultraviolet light (UV) by combining mild heat with UV. Pineapple juice was treated with mild heat (temperature: 50, 55 and 60 °C; holding time: 10, 20 and 30 min) and subsequently exposed to UV (5.61, 7.55 and 11.23 mJ·cm^− 2). The effects of these combined treatments on pectin methylesterase (PME), bromelain activities and total phenolic content (TPC) were determined. Both enzymatic activities were reduced by mild heat but not by UV treatment. Increasing holding time and UV dosage led to higher depletion of TPC. Treating pineapple juice with mild heat at 55 °C for 10 min and UV at 5.61 mJ·cm^− 2 decreased PME by 60.53% whilst retaining 61.57 ± 0.21% and 72.80 ± 0.33% of bromelain and TPC, respectively.Industrial relevanceAs opposed to traditional heat pasteurisation, ultraviolet (UV) treatment has the potential to produce pineapple juice with added value, such as high amount of health benefiting phenols and bromelain. Despite being known for being economically feasible, this technology is not widely adapted by the industry due to its inability to inactivate pectin methylesterase (PME). To overcome the limitation of UV, mild heat (MH) is introduced as hurdle technology. This study demonstrates that combining UV and MH could be able to effectively inactivate the PME in pineapple juice whilst preserving relatively high amount of bromelain and phenols.     

Optimization of supercritical fluid extraction of bioactive compounds from grape (Vitis labrusca B.) peel by using response surface methodology

Supercritical fluid extraction (SFE) was applied for the extraction of valuable compounds from grape (Vitis labrusca B.) peel. Extraction was carried out according to an orthogonal array design (OAD) and independent variables selected were temperature, pressure and modifier concentration. SFE process was optimized by using response surface methodology (RSM) for the extract yield, total phenols, antioxidants and total anthocyanins from grape peel. Effects of extraction temperature and pressure were found to be significant on all responses. Optimal SFE conditions were identified as 45–46 °C temperature, 160–165 kg cm^? 2 pressure and 6–7% ethanol as modifier for maximum extract yield (12.31%), total phenols (2.156 mg GAE/100 mL), antioxidants (1.628 mg/mL) and total anthocyanins (1.176 mg/mL). Experimental values for response variables at these optimal conditions match well with the predicted values. Grape peel extracts obtained by SFE showed more than 93% DPPH radical scavenging activities.Industrial relevanceThis study describes the response surface optimization of supercritical fluid extraction (SFE) process for the enhanced recovery of total phenols, antioxidant and anthocyanins from grape peel. SFE uses CO₂ as supercritical fluid which is environment friendly solvent; allows extraction at lower temperature and the extracts obtained possess higher quality and safety. Industrially, it may be used as a promising technique for the extraction of bioactive compounds from plant materials.     

Radiant energy under vacuum (REV) technology: A novel approach for producing probiotic enriched apple snacks

The feasibility of vacuum impregnation in combination with air drying + radiant energy vacuum (REV) drying to produce shelf stable probiotic enriched apple slices was evaluated. The shelf life of the products was monitored at 25 and 4 °C. The results demonstrated that bacterial stability at 25 °C depended on the dehydration techniques; with the longest shelf life in air drying +REV drying followed by freeze drying and air drying. Storage at 4 °C showed no significant changes in bacterial population up to 180 days in all samples. Sensory properties of the air drying +REV and freeze dried apple slices remained above the acceptable level for 30 days at 25 °C and 180 days at 4 °C. The results also revealed that dried apple slices were able to provide prominent protection to the cells in acidic gastric juice.     

Combined densification and pulsed electric field treatment for selective polyphenols recovery from fermented grape pomace

The aim of this study is to assess a new process for the valorization of fermented grape pomace using pulsed electric fields (PEF). The combination of densification and PEF treatment was applied on grape pomace of low relative humidity, without any addition of conductive liquid. The kinetics of extraction and the composition of polyphenols were evaluated throughout the subsequent hydro-alcoholic extraction at different temperatures.Optimal parameters of PEF treatment (field strength E = 1.2 kV·cm^− 1; energy input W = 18 kJ·kg^− 1; density ρ = 1.0 g·cm^− 3) increased the content of total polyphenols regardless of the temperature of extraction. The ratio of total anthocyanins to total flavan-3-ols at 20 °C was equal to 7.1 and 9.0 for control and PEF treated modalities, respectively. These results demonstrate the selective nature of PEF treatment in anthocyanin extraction, and thus reveal new possibilities to produce extracts with different biochemical compositions.Industrial relevanceThis study examines the feasibility of densification combined with PEF pre-treatment of relatively low humidity grape pomace for the enhancement of bioactive compounds extraction. The concentration of total phenolic compounds obtained after PEF treatment showed that the use of this technique is relevant for an industrial use, since solvent amount and extraction time can be reduced. Moreover, the selective nature of PEF opens the opportunity to produce extracts of different biochemical compositions. This process is an alternative to conventional pre-treatments of raw material (e.g. dehydration and grinding), which have impacts on product quality and are more energy consuming.