One option for the management of wastewater from tofu production: Freeze concentration in a falling-film system

Tofu whey is a liquid by-product from tofu production. Although it contains oligosaccharides, proteins and isoflavones, which could be isolated and used as ingredients for functional products, it is currently not utilized but disposed as a waste stream. However, when disposed directly to the environment tofu whey can cause bad odours and pollution of the surface and ground water, so that treatment is necessary. The wastewater treatment of industrial tofu production by current technologies is problematic, because of the high expenses and the lack of knowledge about their efficient operation. Hence the need to use alternative technologies such as freeze concentrations. Falling-film freeze concentration tests of tofu whey were carried out on pilot-scale equipment in three stages. The increase in soluble solids content of the tofu whey and the amount and purity of the ice formed were analysed. It was observed that the concentration could be increased by a factor of 8 (from an initial concentration of 1.9°Brix to a final concentration of 15.5°Brix). The electrical conductivity of the tofu whey at the last stage was 6.48 mS/cm and the pH was 5.22. The process efficiency was 82.9% at the first stage but dropped to lower values at later stages. Falling film freeze concentration is a promising alternative to recover the solutes retained in the effluent from the tofu industry, reducing its volume and improving environmental management.     

Behavior of functional compounds during freeze concentration of tofu whey

The liquid waste generated from tofu production, denominated as Tofu Whey (TW), contains important amounts of isoflavones that can be evaluated by various separation techniques. In this work TW was concentrated by falling-film freeze concentration from 1.9 to 15.5 °Brix, up to levels of 208 mg of isoflavones per 100 g solids. The levels of isoflavones, proteins, sugars, calcium and magnesium were determined both in the ice and in the concentrate obtained. It was found by rheological characterization that TW shows a Newtonian behavior at concentrations between 1.9 and 15.5 °Brix with freezing points of −0.6 to −2.7 °C.     

Estimation of the freezing point of concentrated fruit juices for application in freeze concentration

In freeze concentration operations the fluids remain at temperatures below 0 °C. For a good study of this concentration operation is very important to know the values of freezing point. The aim of this work was to establish a model that predicts the freezing point of fruit juices at various concentrations within the range of interest for freeze concentration (10-40 °Brix). The model proposed relates the freezing point of a juice with the concentrations of main sugars present in the juice: sucrose, glucose and fructose. The freezing point of apple juice, pear juice and peach juice was determined experimentally at various concentrations, and experimental results were well correlated with model calculations.     

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 high or low molecular weight of components of feed on transmembrane flux during forward osmosis

The possible mechanism of water transport from feed to osmotic agent side during forward osmosis in situation when feed contains high or low molecular weight compounds and their combination has been presented. The orientation of membrane was found to influence the transmembrane flux. When the feed contains mixture of low and high molecular weight compounds mode I (feed towards the support layer) was found to result in lower flux values as compared to Mode II (feed towards active layer) due to significant external concentration polarization. Forward osmosis resulted in the concentration of betalains content in beetroot juice and anthocyanin content in grape juice from 50.92 mg/L to 2.91 g/L (57.1 fold) and from 104.85 mg/L to 715.6 mg/L (6.8 fold), respectively. Total soluble solids in case of beetroot, grape and pineapple juice were found to increase from 2.3 to 52 °Brix, from 8.0 to 54.6 °Brix from 4.4 to 54 °Brix, respectively.     

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.     

Effect of freezing rate on quality parameters of freeze dried soursop fruit pulp

The effect of freezing rate on the final moisture and ascorbic acid content, water solubility, wettability and color of freeze dried soursop fruit pulp treated with maltodextrin was studied. Different size ice crystals derived from distinct freezing rates origins diversity of product specific surface area that influence both water desorption and water dissolution, but in opposite manners. After a constant drying time of 6 h the moisture content of the dried samples was in the range of 8.68–13.09% being higher for higher values of freezing rate. An inverse linear dependence between initial freezing rate and final water solubility (85.75–81.51%) of freeze dried samples was also found. Faster freezing rates also affected the wetting time (0.36–1.26 min) because they produced decreasing in pore size and simultaneously increasing in capillary tortuosity of the final micro-structure of the dried samples. Freeze-dried powders were much brighter in color compared to the maltodextrin treated pulp. Among the freeze dried samples, those prepared with higher freezing rates were lighter in color.     

A study of the ice crystal sizes of red muscle of pre-rigor Atlantic salmon (Salmo salar) fillets during superchilled storage

Pre-rigor salmon fillets were superchilled in an impingement freezer and stored at −1.7 ± 0.3 °C for 29 days. The objective of this work was to study the ice crystal sizes in red muscle of pre-rigor salmon fillets that were partially frozen at fast (−30 °C, 227 W/m² K, 2.1 min) which is referred to as process F and slow (−20 °C, 153 W/m² K, 4.2 min) which is referred to as process S during superchilled storage. It was observed that the size of intracellular ice crystals in pre-rigor muscles at faster superchilling rate was significantly (p < 0.05) smaller than that at slower superchilling rate. The size of ice crystals formed in pre-rigor muscle was significant (p < 0.05) smaller than that formed in post-rigor muscle. It was also observed that the size of intracellular ice crystals formed in pre-rigor red muscles was significant smaller than that in white muscle. In addition, a large number of small ice crystals are formed within the muscle during partial freezing of pre-rigor muscle compared to post-rigor muscle. Future research should focus on tests of the quality parameters separately in red and white muscles (pre- and post-rigor) during superchilled storage of food products in order to understand more about their characteristics (quality and shelf life).     

Freeze concentration of must in a pilot plant falling film cryoconcentrator

The standard methods of producing concentrated grape must are vacuum evaporation and reverse osmosis. Concentration by freezing is the system that comes closest to the ideal objective of separating water from the food product without affecting the other components. This article examines the process for freeze concentration of white must from Macabeo variety grapes.The pilot plant equipment designed at the Technical University of Catalonia is based on freezing the water content of fluids in direct contact with a cold surface. Different parameters were studied to allow tracking of the process: evolution of soluble solids and the ice production. Freeze concentration tests with forty five litters of must were made at an initial concentration of 16.4 °Brix. A final concentration of 29.5 °Brix was obtained. An average rate of 1.38 °Brix/h was obtained working at flow rates of 0.8 L/s. The ice production ranged from 1.32 to 1.05 g?m^? 2?s^? 1 as the concentration of the must increased.Industrial relevanceSometimes the must has low contents in sugars. The freeze concentration can achieve the appropriate level of concentration in some favorable conditions without losses of aroma and sensorial properties. With this purpose INCAVI (Catalonian Institute of vineyard and wine) provided 100 L of grape juice for the test presented in this article. In this work has been applied this technology to concentrate must (grape juice) obtaining promising results.     

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.     

Effect of high-pressure versus conventional thawing on color, drip loss and texture of Atlantic salmon frozen by different methods

Atlantic salmon (Salmo salar) samples were frozen by conventional air freezing, plate freezing and liquid nitrogen (LN) freezing, and subjected to different thawing treatments: water immersion thawing (WIT) (4°C and 20°C) and high-pressure thawing (HPT) at 100, 150 and 200 MPa with water (containing 2 g oil/100 g) as pressure medium at 20°C. Temperature and phase change behavior of fish samples were monitored during freezing and thawing. The phase change point of frozen salmon was lowered to −14°C, −19°C and −25°C for the HPT processes at 100, 150 and 200 MPa, respectively. These phase change temperatures were lower than for pure ice at the same pressures possibly due to the presence of solutes in salmon. The HPT times were 22.6±1.4, 18.1±1.4 and 17.0±1.3 min at 100, 150 and 200 MPa, respectively, as compared with 26.6±2.1 and 94.3±3.4 min for the WIT process at 20°C and 4°C, respectively. Employing pressures above 150 MPa caused noticeable color changes in salmon during the HPT process and the product texture was significantly modified during HPT at 200 MPa. Different freezing rates prior to thawing resulted in differences in drip loss in salmon samples, but they did not induce specific color and texture changes. A significant (P<0.05) reduction of drip loss by the HPT process was observed only for the LN frozen samples in which mechanical cracking occurred and much of the drip appeared after WIT process. Drip loss formed during pressure thawing seems to be a complicated process, for which further studies are needed.     

Modelling of rheological behaviour of soursop juice concentrates using shear rate–temperature–concentration superposition

The effect of temperature and concentration on rheological behaviour of freeze dried soursop juice concentrates were investigated using a rheometer over a wide range of temperatures (10–70 °C) and concentrations (10–50 °Brix) at shear rates of 0–400 1/s. The Power law is the best fitted model to the rheological data due to the high value of coefficient of determination (R² = 0.9989). The soursop juice concentrates exhibited shear thinning or pseudoplastic behaviour with n < 1. The consistency coefficients dependency on temperature and concentration were well described by Arrhenius relationship and exponential relationship respectively. The flow activation energy of soursop juice concentrates were 8.32–30.48 kJ/mol. The superposition technique with Power law model sufficiently modelled the overall rheological characteristics of soursop juice concentrates into a single master curve using shift factors based on double shifting steps with R² = 0.9184. This technique also showed that the soursop juice concentrates increases in viscosity and pseudoplasticity behaviour with concentration.     

Effects of temperature,solid content and pH on the stability of black carrot anthocyanins

Anthocyanin stability of black carrots was studied at various solid contents (11, 30, 45 and 64° Brix) and pHs (4.3 and 6.0) during both heating, at 70–90 °C, and storage at 4–37 °C. Monomeric anthocyanin degradation fitted a first-order reaction model. Degradation of monomeric anthocyanins increased with increasing solid content during heating, while it decreased during storage. For example, at pH 4.3, half-life periods for anthocyanins at 30, 45 and 64° Brix were, respectively, 8.4, 6.9 and 5.2 h during heating at 80 °C and 18.7, 30.8 and 35.9 weeks during storage at 20 °C. At 30–64° Brix, increasing pH from 4.3 to 6.0 enhanced the degradation of anthocyanins during heating. The effect of pH on thermal stability of anthocyanins was also studied at six different pHs (2.5–7.0) in citrate-phosphate buffer solutions and significant decrease in anthocyanin stability was observed at pHs above 5.0. Higher activation energies (E_a) were obtained during heating than during storage with increasing solid contents. At 30–64° Brix, E_a values ranged from 68.8 to 95.1 kJ mol⁻¹ during heating and from 62.1 to 86.2 kJ mol⁻¹ during storage. Q₁₀ values at 20–37 °C were as high as 3.1 at 45° Brix and 3.6 at 64° Brix.     

Experimental study on the freezing characteristics of four kinds of vegetables

Mushroom, green cauliflower, navy bean and pea pod are four kinds of favored vegetables. Their freezing characteristics are studied in this paper. For fresh samples, the moisture contents of mushroom, navy bean, pea pod and green cauliflower were 88.7±4.9, 92.9±0.4, 87.7±1.0 and 89.7±0.9 g/100 g, respectively. After pre-treating, cooling curve method and differential scanning calorimetry (DSC) were employed to measure the end-points of freezing and glass transition temperatures. The initial freezing points varied from −0.1 to −2.7 °C. The end-points of freezing were all below −20.0 °C. The partial glass transition temperatures varied from −50.3 to −76.1 °C. With a cryomicroscope, the sizes of ice crystals in frozen vegetable saps were found to decrease from 26 to 3 μm when the freezing rates increased from 1.0 to 10.0 °C/min.     

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.     

Influence of brine concentration and temperature on composition, microstructure, and yield of feta cheese

The protein matrix of cheese undergoes changes immediately following cheesemaking in response to salting and cooling. Normally, such changes are limited by the amount of water entrapped in the cheese at the time of block formation but for brined cheeses such as feta cheese brine acts as a reservoir of additional water. Our objective was to determine the extent to which the protein matrix of cheese expands or contracts as a function of salt concentration and temperature, and whether such changes are reversible. Blocks of feta cheese made with overnight fermentation at 20 and 31°C yielded cheese of pH 4.92 and pH 4.83 with 50.8 and 48.9 g/100 g of moisture, respectively. These cheeses were then cut into 100-g pieces and placed in plastic bags containing 100 g of whey brine solutions of 6.5, 8.0, and 9.5% salt, and stored at 3, 6, 10, and 22°C for 10 d. After brining, cheese and whey were reweighed, whey volume measured, and cheese salt, moisture, and pH determined. A second set of cheeses were similarly placed in brine (n = 9) and stored for 10 d at 3°C, followed by 10 d at 22°C, followed by 10 d at 3°C, or the complementary treatments starting at 22°C. Cheese weight and whey volume (n = 3) were measured at 10, 20, and 30 d of brining. Cheese structure was examined using laser scanning confocal microscopy. Brining temperature had the greatest influence on cheese composition (except for salt content), cheese weight, and cheese volume. Salt-in-moisture content of the cheeses approached expected levels based on brine concentration and ratio of brine to cheese (i.e., 4.6, 5.7 and 6.7%). Brining at 3°C increased cheese moisture, especially for cheese with an initial pH of 4.92, producing cheese with moisture up to 58 g/100 g. Cheese weight increased after brining at 3, 6, or 10°C. Cold storage also prevented further fermentation and the pH remained constant, whereas at 22°C the pH dropped as low as pH 4.1. At 3°C, the cheese matrix expanded (20 to 30%), whereas at 22°C there was a contraction and a 13 to 18 g/100 g loss in weight. Expansion of the protein matrix at 3°C was reversed by changing to 22°C. However, contraction of the protein matrix was not reversed by changing to 3°C, and the cheese volume remained less than what it was initially.     

Fish oil encapsulation with chitosan using ultrasonic atomizer

An encapsulation technique was developed using an ultrasonic atomizer and three processing steps: emulsification, ultrasonic atomization, and freeze drying. Emulsion preparation variables such as concentration of wall materials [chitosan (CS), maltodextrin (MD) and whey protein isolate (WPI)] and tuna oil were optimized. The size and stability of the emulsion droplet and the properties of the encapsulated powders after freeze drying were characterized. At 20 g/100 g tuna oil, the optimum ratios of CS to MD and of CS to WPI were 1:10 and 1:1, respectively. There was a significant difference (P<0.05) in the emulsion particle sizes when the preparation conditions were varied. The combination of CS and MD giving the smallest particle size had the highest emulsion stability. The EPA and DHA content (240 mg/g) of the encapsulated powder were slightly higher than commercial specification (100 mg/g) and they had low moisture content and water activity, acceptable appearance and encapsulation efficiency. The ultrasonic technology used in this study could lead to application in the food industry improving the stability of tuna and other oils.     

Heat-induced aggregation of whey proteins in the presence of κ-casein or sodium caseinate

Aggregates were formed by heating mixtures of whey protein isolate (WPI) and pure κ-casein or sodium caseinate at pH 7 and 0.1 M NaCl. The aggregates were characterized by static and dynamic light scattering and size exclusion chromatography. After extensive heat-treatment at 80 °C for 24 h, almost all whey proteins and κ-casein formed mixed aggregates, but a large proportion of the sodium caseinate did not aggregate. At a given WPI concentration the size of the aggregates decreased with increasing κ-casein or sodium caseinate concentration, but the overall self-similar structure of the aggregates was the same. The presence of κ-casein or caseinate therefore inhibited growth of the heat-induced whey protein aggregates. The results were discussed relative to the reported chaperone-like activity of casein molecules towards heat aggregation of globular proteins.     

沙棘原浆冷冻浓缩工艺的响应面优化

为了避免在热浓缩过程中沙棘原浆里V_C、含硫氨基酸等热敏性物质的损耗,缓解褐变现象。以沙棘原浆为试材,利用单因素实验研究冷冻浓缩加工过程中冷冻温度、沙棘浆浓度、冷冻时间对取冰质量、取冰纯度的影响。并采用Box-behnken响应面设计,进一步对冰晶质量和冰晶纯度进行联合优化。结果表明,经过响应面联合优化并验证后得到的最佳的工艺条件为:冷冻温度-7℃、沙棘浆浓度12.4 Brix、冷冻时间13 min,此条件下实际结晶强度为33.67 g,结晶纯度为8.1 Brix。此时能够在最经济的浓缩条件下得到最大的冰晶生成量,且冰晶纯度最高。通过对冷冻浓缩前后以及复原汁的营养成分对比得知,浓缩后沙棘汁的总酸、总可溶性固形物和总黄酮的含量显著上升,浓缩过程对各营养成分的损失均低于10%。     

Short communication: Development of a novel method for the extraction of norbixin from whey and its subsequent quantification via high performance liquid chromatography

Norbixin is the primary carotenoid in annatto coloring, which imparts the desired orange color in Cheddar cheese. However, a portion of the colorant remains in the cheese whey and is undesirable; therefore, a bleaching step is often applied. Restrictions exist for norbixin concentrations in products destined for infant formula. As such, evaluation of norbixin concentrations in whey and whey ingredients is desirable. Current extraction methods are laborious and require solvents that are banned in many countries. The objective of this study was to develop a fast and inexpensive norbixin extraction and quantitation technique using approved solvents with similar sensitivity to current established methods. Instead of solvent extraction and column purification, acetonitrile was added directly to fluid wheys, retentates, and rehydrated whey protein concentrates. An isocratic mobile phase [70% acetonitrile and 30% water with 0.1% (wt/vol) formic acid] was used and, to increase sensitivity, a large volume (50 μL) was injected onto the column. The column used was a C18 column with a particle size of 2.6 μm and column length of 10 cm. The column inner diameter was 4.6 mm and the pore size was 100 ?. All of the previously described conditions allowed the run time to be only 4 min. The sample was sent through a photodiode array detector and quantified at 482 nm. Norbixin was quantified using external standard curves. The developed method had a >90% norbixin recovery in both milk and whey (9.39 μg/L–2.35 mg/L). The limit of detection of norbixin in fluid whey was 2.7 μg/kg and the limit of quantitation was 3.5 μg/kg, both of which are significantly lower than in previously described methods. The extracts were stable over 30 min at 21°C and stable over 24 h at 4°C. Repeatability and precision of the method had relative standard deviations of less than 13%. The developed method provides time and cost savings for evaluation of norbixin concentration in whey and whey products.