Ultrafiltration and reverse osmosis for clarification and concentration of fruit juices at pilot plant scale

The process of ultrafiltration of raw juices (peach, pear, apple and mandarin) through tubular polysulphone membranes (8 kDa) and finally concentrated by reverse osmosis membranes of tubular composite polyamide film (99 g/100 g NaCl rejection) with filtration area of 0.9 m² was studied. Furthermore, in order to obtain a higher permeate flow, the fluids were previously treated with commercial pectinolytic enzyme.The following parameters were analyzed: permeate flow, soluble solids, viscosity, density, pH, acidity, formol index, starch, pulp content, color and presence of pectin. The use of a pectinolytic enzyme provides increased permeate flux of approximately 40%, retaining the juice properties. The highest total soluble solids content was clarified peach juice from 12.2 °Brix concentrated up to 30.5 and 21.52 °Brix by using RO with transmembranes pressures of 4 and 2 MPa respectively.The results show a cross-flow velocity (1.8 m/s) which corresponds with Reynolds number that is on the lower border of a laminar flow and above of transition rate (2090 < Re < 2900). Also the (VCF) for mandarin (1.49), pear (1.53), apple (1.56) and peach (1.58) was obtained for RO process. The membranes used were characterized morphologically using scanning electron microscopy.     

Chicory juice clarification by membrane filtration using rotating disk module

Clarification is the first step of inulin production from chicory juice, and membrane filtration as an alternative can greatly simplify this process, increase juice yield, improve product quality, and reduce the cost and waste volume. In this study, a rotating disk module (RDM) was used to investigate the clarification of chicory juice by four micro- and ultrafiltration membranes. Compared with dead end filtration, the RDM had a much higher permeate flux and product quality. High rotating speeds produced high permeate fluxes and reduced flux decline, because of the strong back transport of foulant from fouling layer to feed solution. At high rotating speeds of 1500–2000 rpm, the permeate flux increased with membrane pore size and transmembrane pressure (TMP), while at low rotating speeds (<1000 rpm), permeate flux was independent of membrane type and TMP due to a thick deposited fouling layer as a dominant filtration resistance, while carbohydrate transmission decreased at higher TMP because of denser cake layer as an additional selective membrane. The highest carbohydrate transmission (∼98%) and desirable permeate turbidity (2.4 NTU) was obtained at a TMP of 75 kPa and a rotating speed of 2000 rpm for FSM0.45PP membrane. With the RDM, the Volume Reduction Ratio (VRR) could reach 10 with a high permeate flux (106 L m⁻² h⁻¹) in the concentration test, and permeate was still rich in carbohydrate and well clarified. Chemical cleaning with 0.5% P3-ultrasil 10 detergent solution was able to recover 90% water flux of fouled membrane.     

Analysis of the fouling mechanisms during cross-flow ultrafiltration of apple juice

The purpose of this work was to study the fouling mechanisms of a Carbosep^® M8 membrane during the cross-flow ultrafiltration of apple juice. A new fouling model has been developed that simultaneously considers membrane blocking within the pores, at the pore mouths and by cake formation at the membrane surface. Membrane fouling by apple juice was due to internal pore blocking as well as cake formation. When operating ultrafiltration at a transmembrane pressure of 150 kPa and a cross-flow velocity of 7 m/s, fouling was minimal with a gradual decrease of the relative contribution of cake formation; however, transmembrane pressure still exceeds critical pressure. The fouling model predicts no cake formation at a cross-flow velocity of 7.4 m/s and a transmembrane pressure of 150 kPa or at a cross-flow velocity of 7.0 m/s and a transmembrane pressure of 120 kPa. Under these conditions, internal membrane blocking would be the only mechanism responsible for the decrease of permeate flux.     

EFFECTS OF PECTINASE IMMOBILIZATION DURING HOLLOW FIBER ULTRAFILTRATION OF APPLE JUICE

The immobilization of commercial pectinases by physical adsorption on hollow fiber ultrafiltration (HFUF) membranes was studied in view of its possible application in fruit juice clarification. The optimal pH during immobilization and washing was investigated, as well as the effects of enzyme and pectin concentrations and retentate flow on the operation. Results indicated that permeate flux was not initially increased when pectin solution or apple juice was ultrafiltred through pectinase immobilized on HFUF membranes. However, enzyme immobilization greatly extended the membrane operation, by keeping permeate flux constant during prolonged periods at a reasonable yield.     

The effect of pre-treatment on the anthocyanin and flavonol content of black currant juice (Ribes nigrum L.) in concentration by reverse osmosis

Reverse osmosis process for the concentration of black currant juice was carried using AFC-99 tubular membrane at 30 °C and 45 bar. The contents of selected flavonols and anthocyanins were analyzed after centrifugation; enzyme treatment by Panzym Super E and by Rohapect berry followed by centrifugation; and ultrafiltration black currant juices and juice concentrates. The total soluble solid (TSS) content of the juices increased from the initial 17.6–17.9 °Brix to 24–24.8 °Brix in the case of the centrifuged juice in the concentration process. Similarly, it increased from 14.5–15.5 °Brix to 23.1–23.4 °Brix for the Panzym Super E treated juice, and from 16.1–16.9 °Brix to 22.5–23.1 °Brix for the Rohapect berry treated black currant juices. The ultrafiltered juice had the lowest initial TSS content between 14.1 and 14.9 °Brix and it increased to 22.1–23.1 °Brix. The average permeate fluxes during the concentration process were 7.3 L m⁻² h⁻¹ for the centrifuged juice, 11.9 L m⁻² h⁻¹ for the Panzym Super E treated juice, 9.2 and 13.1 L m⁻² h⁻¹ for the Rohapect berry treated and ultrafiltered juice, respectively. Analysis indicated that the enzymatic treatment resulted in the increase of anthocyanin and flavonol content of the juices. The centrifugation process decreased the amount of anthocyanins and flavonols to some extent. The juice clarified by ultrafiltration had significantly lower concentrations of anthocyanins and flavonols, while the juices treated by Panzym Super E had the highest levels of these flavonoids. This study recommends enzymatic pre-treatment by Panzym Super E, since it improves the permeate flux in reverse osmosis during the concentration process, and results in a juice concentrates highest in anthocyanins and flavonols.     

Effect of ultrafiltration on concentrated apple juice colour and turbidity

Colour and turbidity of conventional bentonite-gelatin clarified apple juice was compared with 30,000–50,000 and 100,000DA hollow fibre ultrafiltered apple juice, with and without pectinolytic enzyme treatment. Results indicated that objective quality of ultrafiltered apple juice compared favourably with conventionally clarified apple juice over 30 weeks of storage at 37.5°C. However, treatment with pectinolytic enzymes before ultrafiltration increased both the initial colour and the browning rate. No significant differences were found in the values of the transmission haze after storage.     

Application of osmotic membrane distillation process in red grape juice concentration

The osmotic membrane distillation process was applied in dehydration of red grape juice (Most de Raïm Concentrat Negre) of different concentrations (5–20 °Brix). Experiments were performed using polytetrafluoroethylene (PTFE) hydrophobic membranes of different nominal pore diameter. Red grape juice solution and concentrated calcium chloride solution (50 wt.%) were used as feed and stripping solutions, respectively. The permeate flux, the initial and the final juice concentration, the total phenolic content (TPC) and the antioxidant activity (TEAC) were measured for each single experiment.     

Clarification of apple juice by electroflotation

Apple Juice industry is in search of a simplified technology which enables a quick clarification and stabilisation of apple juice. This study aimed to evaluate the potential of electroflotation as an alternative for the clarification of apple juice. Clarification of apple juice by electroflotation was first done at various current densities (10, 20 and 40 mA/cm²) with and without addition of gelatin (200 mg/l). Afterwards, the electroflotation treatments were done at a current density of 20 mA/cm² with various concentrations of added gelatin (0, 50, 100 and 200 mg/l). It was shown that electroflotation treatments alone was efficient to reduce the tannin and protein contents of apple juice. However, the decrease in the protein content was in large part due to the use of pectinases prior to the electroflotation treatments. The use of gelatin in combination with the electroflotation aided in the clarification process. The highest gelatin concentration used in this study (200 mg/l) resulted in a better reduction of tannin and protein levels, while a current density of 20 mA/cm² was found to be optimal. Turbidity observed in the juices clarified with electroflotation treatments was in average lower than 10 NTU but higher than 2 NTU which is generally required to produce a stable clarified juice. Brix degree and pH of the apple juice was not affected by the electroflotation treatments while the color was improved.

Industrial relevance

The production of clarified and stable apple juice is a subject of interest for the beverages industries. The clarification step which remained long and discontinuous implied the addition of a large quantity of pectolytic enzyme and of clarifying agents (such as gelatin) to the freshly pressed juice to induce the precipitation of proteins and other suspended matter in 15–20 h. Fining treatments were followed by a separation step usually consisting of decantation and classical filtration on filter-press, or flotation by dispersed gas. The development of membrane separation processes to replace the traditional approach has enabled the automation of the whole production resulting in lower labor requirement and a considerably shorter process time than the traditional process.However, the performance of membrane separation processes is influenced by the declining permeate flux with time, which is due to membrane fouling. In some instances, permeate flux decline makes membrane separation processes unattractive for the clarification of apple juice. To our knowledge, we are the first research group to use electroflotation (EF) for clarification of apple juice. It was shown that EF treatments alone were efficient to reduce the tannin and protein contents of apple juice. In addition, the use of gelatin in combination with the EF aided in the clarification process. Turbidity observed in the juices clarified with EF treatments for 30 min was in average lower than 10 NTU. Brix degree and pH of the apple juice were not affected by the EF treatments while the color was improved.When compared to the values reported in the literature for flotation by dispersed gas, it seems that EF shows better efficiency than flotation in decreasing the juice turbidity (99% decrease for EF as compared to 90% decrease for flotation). In addition, for experiments carried out by conventional flotation larger amount of fining agent are used (70–150 mg of gelatin/l, 400–800 mg/l of silica sol and 200–500 mg/l of bentonite). For these reasons, the new process we propose is advantageous when compared to the traditional flotation approach and it should have a measurable impact on the advancements in the production of clarified apple juice. If used as a pre-treatment to ultrafiltration clarification, it is expected that it would reduce membrane fouling resulting in higher productivity.     

Production of Apple Juice by Single Pass Metallic Membrane Ultrafiltration

A new process utilizing single pass metallic membrane ultrafiltration (UF) was developed to produce apple juice. Pureed whole apples were treated with cellulase and pectinase at 50°C for 2 hr, resulting in a 60% decrease in viscosity. To obtain clarified juice, enzyme treated puree was pumped through a single-pass, tubular membrane system consisting of a metallic oxide membrane formed-in-place on the porous structure of sintered stainless steel tubes. Juice yields of 80–85% were obtained with a single pass, and gas chromatographic profiles of ultrafiltered juice were nearly identical to that of the original apple puree. Permeabilities and sugar rejection characteristics of the UF system were dependent on tube diameter.     

Impact of apple processing modes on extracted juice quality: Pressing assisted by pulsed electric fields

The purpose of this study was to compare the effects of pulsed electric field (PEF) on apple juice characteristics (turbidity, polyphenolic content and antioxidant capacities). The pressing was used as a standard method for juice extraction. Experiments were carried out at a constant pressure (P = 3 bar) using a laboratory press cell. Two different methods for PEF application at 400 V/cm were investigated (PEF treatment of whole samples before cutting and PEF treatment of apple slices after cutting). PEF treatment resulted in increase of the juice yield from 44 g/100 g apple (untreated samples) to 58 g/100 g apple (treatment of whole apples) and 64 g/100 g apple (treatment of slices) after 30 min of pressing. The analysis of pH and conductivity showed no significant difference between untreated and PEF-treated samples. However, the total soluble matter content of juice increased after PEF treatment. The obtained turbidity and transmittance data evidence a noticeable improvement of juice clarity for PEF-treated samples. The PEF pre-treatment was accompanied by an increase of the content of polyphenols and intensification of the antioxidant capacities of juice. Most of these effects (juice clarity and content of antioxidants) were more pronounced for the whole treated apples as compared to untreated apples and PEF-treated apple slices. The evolution of apple browning before and after PEF treatment was more pronounced for whole samples. PEF treatment accelerates browning. The obtained data can contribute to the determination of an optimum time for PEF application. The results evidence that PEF-enhanced expression is promising for production of higher quality juices. PEF treatment of whole apples reduces the energy consumption and is advantageous for industrial applications as compared to the treatment of apple slices. PEF combined with pressing can become a good alternative to traditional process.     

Inactivation of Escherichia coli by ozone treatment of apple juice at different pH levels

This research investigated the efficacy of gaseous ozone on the inactivation of Escherichia coli ATCC 25922 and NCTC 12900 strains in apple juice of a range of pH levels, using an ozone bubble column. The pH levels investigated were 3.0, 3.5, 4.0, 4.5 and 5.0. Apple juice inoculated with E. coli strains (10⁶ CFU/mL) was treated with ozone gas at a flow rate of 0.12 L/min and ozone concentration of 0.048 mg/min/mL for up to 18 min. Results show that inactivation kinetics of E. coli by ozone were affected by pH of the juice. The ozone treatment duration required for achieving a 5-log reduction was faster (4 min) at the lowest pH than at the highest pH (18 min) studied. The relationship between time required to achieve 5 log reduction (t_5d) and pH for both strains was described mathematically by two exponential equations. Ozone treatment appears to be an effective process for reducing bacteria in apple juice and the required applied treatment for producing a safe apple juice is dependant on its acidity level.     

Effect of membrane property and operating conditions on phytochemical properties and permeate flux during clarification of pineapple juice

The effects of membrane property on the permeate flux, membrane fouling and quality of clarified pineapple juice were studied. Both microfiltration (membrane pore size of 0.1 and 0.2 μm) and ultrafiltration (membrane molecular weight cut-off (MWCO) of 30 and 100 kDa) membranes were employed. Membrane filtration did not have significant effects on the pH, reducing sugar and acidity of clarified juice whereas the suspended solids and microorganism were completely removed. The 0.2 μm membrane gave the highest permeate flux, total vitamin C content, total phenolic content and antioxidant capacity as well as the highest value of irreversible fouling. Based on these results, the membrane with pore size of 0.2 μm was considered to be the most suitable membrane for the clarification of pineapple juice. The optimum operating conditions for the clarification pineapple juice by membrane filtration was a cross-flow velocity of 3.4 ms⁻¹ and transmembrane pressure (TMP) of 0.7 bar. An average flux of about 37 lm⁻² h⁻¹ was obtained during the microfiltration of pineapple juice under the optimum conditions using batch concentration mode.     

Effect of pectinase treatment on extraction of antioxidant phenols from pomace,for the production of puree-enriched cloudy apple juices

Effects of pomace maceration on yield, turbidity, cloud stability, composition of phenolics, antioxidant activity and colour properties were studied, to evaluate the potential applicability of enzyme preparations in puree-enriched cloudy apple juice production. The yield of mixed juice and puree from pomace obtained in the enzymatic processing of apple ranged from 92.3% to 95.3%, significantly higher than the yield from the control without enzymatic pomace treatment (81.8%). Higher turbidity was obtained upon pomace treatment with Pectinex XXL and Pectinex Ultra SPL enzymes. The total content of phenolic compounds in apple pomace was higher than in raw juices (1520 mg/kg and 441 mg/L, respectively). The total polyphenol yields were higher in juices treated with Pectinex AFP L-4, Pectinex Yield Mash and Pectinex XXL, as compared to the control treatment. During 6 months of storage, a significant change was observed in the content of polyphenols, especially in procyanidin fractions.     

Effect of UV irradiation on enzymatic activities and physicochemical properties of apple juices from different varieties

The influence of ultraviolet irradiation (UV) on some quality attributes (colour, pH, soluble solids content, formol index, total phenolics, sugars and vitamin C) and enzymatic activities (polyphenol oxidase, peroxidase and pectinolytic enzymes) of fresh apple juice was investigated. Apple juices made from four different varieties (Golden, Starking, Fuji and King David) were irradiated during 120 min with a high-pressure mercury lamp of 400 W that emits in a range between 250 and 740 nm with a resulting incident energy of 3.88·10⁻⁷ E·min⁻¹. The treatment was effective in the inactivation of the assayed enzymes. Polyphenol oxidase was inactivated in 100 min, while peroxidase was completely destroyed in only 15 min in all the four varieties. No variations were observed in pH, soluble solids content, formol index, total phenolics and sugars. The colour of the juice made from King David was unvariable during all the experiment. In the ones made from Golden, Starking and Fuji, UV radiation impaired some of the pigments present in the juice, either initially present or the ones formed later. This fact can be especially observed in the increase of the CIELab parameter L*, which increased from 23.2 to 24.6 in Fuji juice. The content of vitamin C in juices from Golden, Starking and Fuji slightly changed during the experiment, decreasing a 4.0% in Fuji juice, 5.7% in Golden one and 5.6% in Starking one. Meanwhile, in the juice from King David the loss was 70.0%. This significant difference can be attributed to the lack of pigmentation of this juice.     

Clarification of passion fruit juice by microfiltration: Analyses of operating parameters,study of membrane fouling and juice quality

In this study, the performance of two membranes were compared – tubular ceramic and hollow fiber poly(imide) – under transmembrane pressure of 0.5 and 1 bar, for the clarification of passion fruit pulp pre-treated by centrifugation and enzymatic treatment at the concentrations of 150 and 300 ppm. Nutritional and sensorial qualities of the clarified juice obtained were evaluated. Thus, it was possible to observe that the most adequate condition for the clarification of passion fruit pulp was with enzymatic treatment at 150 ppm and its posterior microfiltration at the ceramic tubular membrane of 0.3 μm with transmembrane pressure of 0.5 bar. The fouling mechanism was identified by estimation of model parameters according to a nonlinear regression by Bayesian inference. Analysis of the fouling mechanism results revealed that hollow fiber membrane is controlled by a cake filtration mechanism, and internal pore blocking fouling mechanism controls ceramic tubular membrane.     

Clarification and sterilization of raw depectinized apple juice by ceramic ultrafiltration membranes

Raw depectinized apple juice was clarified and sterilized in a cross‐flow pilot scale ultrafiltration system using ceramic tubular membranes (MEMBRALOX^®, Pall) with mean pore size of 100 nm. The permeate flux significantly decreased with time until a steady‐state was established. An increase in filtration pressure increased the permeate flux while there is an optimum pressure (about 0.85 bar) above which the increase of pressure does not increase the flux significantly. The higher the cross‐flow velocity was, the higher was the transmembrane flux. When the operating temperature increased, the permeation rate increased subsequently. Analytical measurement showed that suspended solids and turbidity could almost be removed by the ceramic ultrafiltration membrane, but pH, acidity, sugar and soluble solid content of the juices showed no significant change. The bacteria challenge tests with Micrococcus flavus showed that the logarithm value of the bacteria reduction rate came up to above 9 in the cross‐flow tubular ceramic system. When the permeate was collected in sterile bottles in a laminar flow shell and kept at 4 °C, 8 °C, 25 °C and 35 °C, for 28 days, the apple juice experienced minimal changes in physicochemical properties at lower temperatures of 4 °C, or 8 °C. Copyright © 2005 Society of Chemical Industry     

Preparation of casein phosphopeptides using a novel continuous process of combining an enzymatic membrane reactor with anion-exchange chromatography

A novel process for continuous preparation of casein phosphopeptides (CPPs) was developed using an enzymatic membrane reactor (EMR) and anion-exchange chromatography (AEC). Alcalase was selected to hydrolyse casein (with an initial concentration of 6% (w/w)) at pH 8.5 and temperature 50 °C in an enzymatic membrane reactor. CPPs were then separated from the enzymatic hydrolysates through a weakly basic macroporous anion-exchanger. The yields of CPPs and phosphorus from casein were 8.11%, 15.66% and 21.41%, and 19.10%, 52.70% and 90.01% for EMR fitted with 3 kDa, 5 kDa and 10 kDa membranes, respectively. The yield and quality of CPPs improved with increase in the nominal molecular weight cut-off (NMWCO) of the membrane. However, use of a high NMWCO membrane resulted in substantial enzyme leakage in the permeate.     

Spray evaporation of liquid foods

‘Spray evaporation’ based on the principle of adiabatic humidification was examined as an evaporation technique for the concentration of two types of representative liquid foods, namely, fruit juice and milk. The concentration of apple juice could be increased from 10.0 to 13.0 °Brix by this technique without application of heat utilizing the humidity potential to an extent of 89%. Employing heated process air during processing increased the amount of water evaporation owing to increased saturation humidity level, enabling higher concentrations to be achieved in apple juice (48 °Brix), reconstituted milk (29 °Brix) and single toned milk (22 °Brix). Feed flow rate had an inverse effect on the final concentration under otherwise similar conditions. Evaporative cooling associated with spray evaporation actually delivered the concentrate at a relatively lower temperature. By manipulating the operating conditions, humidity potential could be utilized to the extent of 55% with heated process air. The spray evaporation technique seemed to have a good potential for the concentration of liquid foods.     

Combined effect of temperature and pulsed electric fields on apple juice peroxidase and polyphenoloxidase inactivation

Pulsed electric fields (PEF) were applied to freshly prepared apple juice using a laboratory scale continuous PEF system to study the feasibility of inactivating peroxidase (POD) and polyphenoloxidase (PPO). Square wave PEF using different combinations of electric field strength, pre-treatment temperature and treatment time were evaluated in this study and compared to conventional pasteurisation (72 °C; 26 s). Inactivation curves for the enzyme were plotted for each parameter and inactivation kinetics were calculated. Results showed the highest level of decrease in the enzymatic activity of 71% and 68%, for PPO and POD, respectively, were obtained by using a combination of preheating to 50 °C, and a PEF treatment time of 100 μs at 40 kV/cm. This level of inactivation was significantly higher (P < 0.05) than that recorded in juice processed by conventional mild pasteurisation where the activity of PPO and POD decreased by 46% and 48%, respectively. The kinetic data for the inactivation of both enzymes could be described using a 1st-order model (P < 0.001).     

Application of biosensors in early detection of contamination with lactic acid bacteria during apple juice and concentrate production

The aim of Collective Research Project QUALI-JUICE (COLL-CT-2005, Co Nr 012461) was to introduce the biosensors in control of microbiologically pure apple juice production. Three commercial lactate biosensors were used and compared with enzyme kits assays. Parallel the microbiological analysis of the production process at one juice producing enterprise was done. The results of lactic acid assay with biosensors were in good correlation with those obtained by enzyme kits. The main benefit of biosensor use was shortening of measurement time as compared with assay by enzyme kit and possibility to measure at line. The concentration of l-lactic acid in apple pulp could be correlated with the number of lactic acid bacteria. Pasteurization process was eliminating lactic acid bacteria and the concentration of lactic acid was at this stage not exceeding 0.1 g L⁻¹. The final product (apple concentrate) contained in some cases very high amounts of lactic acid indicating secondary microbiological contamination after pasteurization step. Parallel microbiological analysis of production process and lactate assay indicated that the critical point during production was prolonged vacuum filtration after pasteurization.