Lactose Crystallization from Whey Permeate in an Ethanol-Water Mixture

A 30% concentrated permeate of a whey ultrafiltration process was used for producing crystalline a-lactose monohydrate. Effect of pH (2.75–5.5 pH units) at solvent to solute ratio 10:1 v/w, agitation and seeding (0.004–0.02%) on rate of lactose crystallization were examined. Conditions which were favorable in terms of crystallized lactose yield, and time of crystallization were: pH 5.5, agitation with or without seeding and 22°C. The first-order reaction-rate constant for crystallization ranged from 0.0178 to 0.200 hr^?1 depending on conditions.     

Evaluating the crystallization of lactose at different cooling rates from milk and whey permeates in terms of crystal yield and purity

The cooling rate of supersaturated lactose solution is one of the important parameters determining the yield and size distribution of lactose crystals. The influence of increasing cooling rate on lactose crystallization and quality of lactose crystals was evaluated in concentrated solutions prepared from deproteinized whey powder (DPW) and milk permeate powder (MPP). Concentrated permeates (DPW and MPP) with 60% (wt/wt) total solids were prepared by reconstituting permeate powders in water at 80°C for 2 h for lactose dissolution. Three cooling rates, 0.04°C/min (slow), 0.06°C/min (medium), and 0.08°C/min (fast) were studied in duplicate. A common rapid cooling step (80 to 60°C at 0.5°C/min) followed by slow, medium, and fast cooling rates were applied as per the experimental design from 60 to 20°C. After crystallization, the crystal slurry was centrifuged, washed with cold water, and dried. The dried lactose crystals were weighed to calculate the lactose yield. Final mean particle chord lengths were measured at the end of crystallization using focused beam reflectance measurement for slow, medium, and fast cooling rates, and observed to be not significantly different for DPW (27–33 µm) and MPP (31–34 µm) concentrates. Similarly, the lactose yield for slow, medium, and fast cooling rates in the DPW and MPP concentrates were in the range of 71 to 73% and 76 to 81%, respectively, and no significant difference between the 3 cooling rates was found. Qualitative analysis of dried lactose crystals exhibited no noticeable differences in the crystal purity with increasing cooling rate. This study evaluated the possibility of reducing the crystallization times by 8 h compared with current industrial practice without compromising the crystal yield and quality.     

Chemical composition and nutritive value of spray dried permeate powder

Reconstituted skimmed milk (10% TS) was ultrafiltered, and the permeate was concentrated threefold by reverse osmosis and then spray dried at different temperatures (145–195° C). The drying conditions had no effect on the moisture content or the major constituents of permeate powder. The powder was mainly lactose (85%) with 6.35460% ash. A small percentage of the lactose in the permeate powder was present as a-lactose. Sodium, potassium and citrate were present in high concentrations nearly equivalent to their average percentage in skimmed milk. The calcium, magnesium and inorganic phosphorus contents of permeate powder were also determined. The thiamine, riboflavin and niacin contents of permeate powder averaged 0.445, 0.947 and 0.729 mg/100 g respectively. The drying temperatures had no effect on the vitamin contents of the powder. The permeate powder had average Fe, Zn, Mn and Cu contents of 94.7, 21.1, 3.1 and 9.5 Fg/100 g respectively.     

Recovery of lactose from simulated delactosed whey permeate by a low-temperature crystallization process

Delactosed whey permeate is the mother liquor/by-product of lactose manufacture, but it still contains around 20 wt% lactose. The high mineral content, stickiness, and hygroscopic behavior prevent further recovery of lactose in the manufacturing process. Therefore, its use is currently limited to low-value applications such as cattle feed, and more often it is seen as waste. This study investigates a new separation technique operating at sub-zero conditions. At low temperature, precipitation of calcium phosphate is expected to be reduced and the lower solubility at sub-zero temperature makes it possible to recover a large portion of the lactose. We found that lactose could be crystallized at sub-zero conditions. The crystals had a tomahawk morphology and an average size of 23 and 31 µm. In the first 24 h, the amount of calcium phosphate precipitated was limited, whereas the lactose concentration was already close to saturation. The overall rate of crystallization was increased compared with the crystals recovered from a pure lactose solution. Mutarotation was rate limiting in the pure system but it did not limit the crystallization of lactose from delactosed whey permeate. This resulted in faster crystallization; after 24 h the yield was 85%.     

Process for calcium retention during skim milk ultrafiltration

Lactose is separated from milk or other fluid dairy products for a variety of reasons. Ultrafiltration is a known process of removing lactose from these products. However, during ultrafiltration, valuable minerals, such as calcium in soluble form, are also lost into permeate. In this study, a process was developed in which first the lactose reduction in skim milk was achieved by ultrafiltration (4x volumetric concentration) using a 10-kDa membrane. Then, the calcium present in permeate was precipitated using one of three methods: 1) heat treatment, 2) pH adjustment, or 3) a combination of pH adjustment and heat treatment to permeate, then recovered by refiltering permeate. The process was first developed at laboratory scale, and then its applicability was tested at the pilot scale. Skim milk, retentates, permeates, and the treated permeates were analyzed for total solids, ash, protein, or total nitrogen, calcium, and lactose content. About 76% of the total lactose and about 16% of the calcium present in skim milk permeated through the membrane during ultrafiltration. The three treatments applied produced white precipitates and turned the clear permeates turbid. On refiltering the treated permeates approximately 42, approximately 50, and approximately 70% of the total calcium present could be recovered from 1) heat-treated, 2) pH-adjusted, and 3) pH-adjusted and heat-treated permeates, respectively. There was no marked change in the lactose content due to any of the three treatments and subsequent refiltering of the treated permeates.     

APPLICABILITY OF ALGINATE ENTRAPPED YEAST CELLS FOR THE PRODUCTION OF LACTOSE-HYDROLYZED MILK

To overcome the problem of enzyme extraction and poor permeability of cell membrane to lactose, permeabilized Kluyveromyces marxianus NCIM 3465 cells as a source of β‐D‐galactosidase were employed for the production of lactose‐hydrolyzed milk. In view of the advantages of an immobilized cell system over a free cell system, the yeast cells were entrapped in alginate gel for their subsequent use in lactose hydrolysis. Different process parameters (alginate concentration, bead size, biomass load, temperature, agitation and incubation time) were monitored to enhance lactose hydrolysis in milk. Maximum lactose hydrolysis (87.9%) was observed with yeast cells immobilized in 2% (w/v) alginate concentration with a bead size of 2.90 mm at 30C under agitation (80 rpm) after 150 min of incubation. The developed system was highly stable and the alginate entrapped yeast cells can be recycled up to the eight cycle without any marked change in their ability to carry out the lactose hydrolysis.     

Use of whey permeate for cultivating Ganoderma lucidum mycelia

A novel approach to utilizing whey permeate, the cultivation of mycelia of the edible mushroom Ganoderma lucidum, is introduced. The major objective of this research was to use whey permeate as an alternative growth medium for the cultivation of mycelia of edible mushroom G. lucidum and to find an optimum condition for solid-state cultivation. Response surface analysis was applied to determine the combination of substrate concentration (25 to 45 g of lactose/L), pH (3.5 to 5.5), and temperature (25 to 35°C) resulting in a maximal mycelial growth. The radial extension rates, estimated by measuring the diameters of growing colonies on the Petri dishes, were used as the growth of the mycelia at different conditions. In the model, pH and temperature significantly affected mycelial growth, but lactose concentration did not. The condition predicted to maximize the radial extension rate of 17.6 ± 0.4 mm/d was determined to be pH 4.4 and temperature 29.4°C. Therefore, the results suggest that whey permeate could be utilized as a growth substrate for the cultivation of mycelia from the edible mushroom G. lucidum, enhancing the use of this by-product by the cheese manufacturing industry.     

Conversion of glucose in lactase-hydrolyzed whey permeate to fructose with immobilized glucose isomerase

The maximum conversion of glucose to fructose in lactase-hydrolyzed whey permeate by glucose isomerase was approximately 52% at .1 g enzyme/ml substrate after 7 h incubation at 60 degrees C. Removal of minerals from the substrate was essential for enzyme activity. The dependence of the enzyme on Mg++ and Co++ for activity in the presence of high ash concentration was demonstrated. Optimum Mg++ and Co++ additions were 250 and 100 ppm, respectively. The isomerization reaction was enhanced more when both 100 ppm Mg++ and 50 ppm Co++ were added. Hydrolyzed isomerized lactose whey syrup with sweetness equivalent to sucrose was successfully produced through enzymatic isomerization of glucose in lactase-hydrolyzed whey permeate after supplementation with pure glucose. Fructose in hydrolyzed isomerized lactose whey syrup was effectively separated from other sugars by Dowex 1X8-200 anion exchange resin in the bisulfite form.     

Utilization of Cheese Whey Permeate in Canned Beans and Plums

Navy and kidney beans (Phaseolus vulgaris) were hydrated in water, then canned in brines designated as control, whey permeate (WP), and hydrolyzed lactose whey permeate (HP). Hunter Lab Color Difference and Kramer Shear texture analyses indicated general darkening and increased firmness in permeate treated beans. Total solids and ash increased significantly in the treated samples. There was a significantly lower preference for beans treated with permeate fractions than for control beans. Plums were canned in a control sucrose syrup (20° Brix) and in syrups with 5, 10, 15, 20, and 25% replacement of sucrose with HP, or crystalline glucose-galactose (GG) mixture. HP plums were generally darker in color and similar in texture to the control samples. Sensory tests showed that general acceptability of HP plums was similar to control samples.     

Water Sorption and Plasticization Behavior of Spray-dried Lactose/Protein Mixtures

ABSTRACT: Water sorption properties, effects of proteins on glass transition temperature, and time-dependent lactose crystallization of spray-dried lactose and lactose in lactose/WPI (3:1), lactose/Na-caseinate (3:1), lactose/albumin (3:1), and lactose/gelatin (3:1) mixtures were investigated. Brunauer-Emmett-Teller (BET) and Guggenheim-Anderson-de Boer (GAB) models were used to model water sorption. Lactose/protein mixtures sorbed high amounts of water at low relative vapor pressure (RVP) up to 23.1%. Above 23.1% RVP levels, water sorbed by pure lactose was higher, up to 44.1% RVP, except in the case of the lactose/gelatin mixture. Lactose/ gelatin also sorbed a high amount of water at 33.2% RVP. Loss of sorbed water resulting from crystallization of amorphous lactose was observed. Crystallization of pure lactose and lactose crystallization in lactose/protein mixtures occurred at RVP ≥ 44.1% within 24 h. After crystallization at RVP ≥ 54.5%, water contents remained higher for lactose/protein mixtures than for pure lactose. The rate of lactose crystallization was less in all lactose/protein mixtures than was observed for pure lactose. WPI had the lowest effect on lactose crystallization. Crystallization occurred most slowly in lactose/gelatin mixtures. Both GAB and BET models fitted to water sorption data up to 0.441 a_w. It seems that different proteins interact with lactose differently. Water sorption and time-dependent lactose crystallization of lactose/protein mixtures have important consequences to processing and storage behavior of lactose-protein based products.     

Production of an Alcoholic Beverage by Fermentation of Whey Permeate with Kluyveromyces fragilis I: Primary Metabolism

Whey permeate from the ultrafiltration processing of cheese manufacturing was used for alcoholic fermentation with Kluyveromyces fragilis, the objective being the production of an alcoholic beverage of low alcoholic grade. The effect of temperature, initial pH, agitation and initial biomass on yeast growth and ethanol production were assayed in batch cultures. In addition, continuous culture behaviour was studied due to interest in a continuous industrial process for a new product. An unstructured kinetic model (a Riccati kinetic equation) is proposed; batch data being employed to obtain the kinetic parameters. This model fits the continuous culture results well except for ethanol production, where calculated values were lower than experimental data. When the fermentation temperature was changed from 18 to 37°C, a maximum of Y_P/S close to 30°C was observed, which gives an efficiency in the conversion of lactose to ethanol of 88%. The initial pH of the whey did not affect yeast growth significantly. Experiments carried out at different initial biomass concentrations showed that an initial dry weight close to 0.5 g/litre was sufficient to carry out the fermentation. An increase in ethanol concentrations was found at higher rates of agitation. In continuous culture, a maximum productivity for biomass and ethanol was attained at a dilution rate of 0.11 h^?1. Higher efficiencies (96%) were achieved in continuous culture rather than in batch cultivation mode.     

Short communication: Cultivation of Lentinus edodes mycelia using whey permeate as an alternative growth substrate

The major objective of this research was to use whey permeate as an alternative growth medium for the cultivation of mycelia of the edible mushroom Lentinus edodes and to find an optimum condition for solid-state cultivation. Response surface analysis was applied to determine the combination of substrate concentration (40 to 60 g of lactose/L), temperature (20 to 30°C), and pH (4 to 6) resulting in a maximal mycelial growth rate. The radial extension rates, estimated by measuring the diameters of growing colonies on the Petri dishes, were used as the growth rate of the mycelia at different conditions. The conditions predicted to maximize the mycelial growth of 6.41 ± 0.47 mm/d were determined to be 40 g of lactose/L, temperature 23.6°C, and pH 5.0. It was concluded that a partial cubic equation could accurately model the response surface of, and predict optimal growth conditions for, L. edodes mycelia using whey permeate because the model prediction agreed with the experimental growth rate, 6.39 ± 0.22 mm/d. The results suggest that whey permeate could be utilized as a growth substrate for the cultivation of mycelia from the edible mushroom L. edodes, enhancing the use of this by-product by the cheese manufacturing industry.     

Development of Hydrolyzed and Hydrolyzed-lsomerized Syrups from Cheese Whey Ultrafiltration Permeate and Their Utilization in Ice Cream

Hydrolyzed lactose syrup (HLS) was produced from cheese whey ultrafiltration permeate by treatment with immobilized β-galactosidase, deionization, and evaporation. The degree of hydrolysis was 97.2%. Hydrolyzed-isomerized lactose syrup (HILS) was produced from hydrolyzed, deionized ultrafiltration permeate by treatment with immobilized glucose isomerase, deionization and evaporation. The degree of isomerization was 34.8%. HLS and HILS were substituted for 25% or 50% of the sucrose (on a solids basis) in vanilla ice cream. The mix freezing time increased when HLS or HILS was substituted for sucrose at a level of 50%. There were no significant differences in melting rates (P < 0.05) and few differences in sensory quality.     

Crystallization and X-ray Diffraction of Crystals Formed in Water-Plasticized Amorphous Spray-dried and Freeze-dried Lactose/Protein Mixtures

ABSTRACT: Effects of proteins (whey protein isolate [WPI], Na-caseinate, and gelatin), drying method, storage relative vapor pressure (RVP), and time on lactose crystallization and crystals formed were investigated using x-ray diffraction (XRD). Crystallization was observed from increasing peak intensities of XRD patterns. Lactose in lactose/protein (5:1,3:1) mixtures crystallized in samples stored at RVP of 44.1% and above in both spray-dried and freeze-dried materials, except in freeze-dried lactose/Na-caseinate and lactose/gelatin mixtures, which showed lactose crystallization at 54.5% RVP and above. The rate of crystallization increased with increasing RVP and storage time. The rate of crystallization in spray-dried materials was higher than in freeze-dried materials, and the crystallization rate decreased with increasing protein content. Lactose crystallized mainly as α-lactose monohydrate in spray-dried lactose/WPI and lactose/gelatin mixtures. Crystals formed in freeze-dried lactose/WPI and lactose/gelatin mixtures were anhydrous β-lactose and α-lactose monohydrate crystals. Lactose crystallized as a-lactose monohydrate in both spray-dried and freeze-dried lactose/Na-caseinate mixtures. Trace amounts of anhydrous β-lactose were present in spray-dried lactose/WPI (5:1) and lactose/gelatin (5:1) mixtures. Peak intensities of XRD patterns for anhydrous β-lactose decreased with increasing protein content and storage time. The crystallization data were successfully modeled using Avrami equation at an RVP of 65.6% and above. These data are important in understanding and predicting storage stability of lactose- and protein-containing food and pharmaceutical materials.     

Effects of Whey Permeate-Based Medium on the Proximate Composition of Lentinus edodes in the Submerged Culture

ABSTRACT:  Biomass production, crude water-soluble polysaccharide (WSP), ash content, mineral profile, and crude protein content were determined for Lentinus edodes mycelia grown on whey permeate (WP)-based medium with lactose content of 4.5% or defined synthetic medium, and harvested after 5, 10, 15, or 20 d of fermentation at 25 °C. Harvesting time and the type of media interact to alter the chemical content of mycelia. Mycelia grown in WP had greater ( P < 0.05) WSP and ash than mycelia grown in the synthetic media. A maximum production of WSP was obtained on the 10th day (4.1 × 10²± 71 mg WSP/g dried mycelia) from mycelia grown on the WP-based media. Mycelia grown on WP harvested on the 20th day had the highest value in ash content (18 ± 3%). Potassium was found to be the main constituent in the ash of mushroom mycelia, which was followed by phosphorus, sodium, calcium, and magnesium. A steady increase of ash content was only noted in mycelia grown on WP. The calcium content of WP-grown mycelia was at least 10 times higher compared to mycelia grown in the control media regardless the harvesting time. Data in this research suggested that WP was more favorable than the synthetic media in the production of WSP, which is traditionally known for their medicinal value in L. edodes .     

Crystallization Kinetics and X-ray Diffraction of Crystals Formed in Amorphous Lactose, Trehalose, and Lactose/Trehalose Mixtures

ABSTRACT: Effects of storage time and relative humidity on crystallization kinetics and crystal forms produced from freeze-dried amorphous lactose, trehalose, and a lactose/trehalose mixture were compared. Samples were exposed to 4 different relative water vapor pressure (RVP) (44.1%, 54.5%, 65.6%, 76.1%) environments at room temperature. Crystallization was observed from time-dependent loss of sorbed water and increasing intensities of peaks in X-ray diffraction patterns. The rate of crystallization increased with increasing storage humidity. Lactose crystallized as α-lactose monohydrate, β-anhydrous, and anhydrous forms of α- and β-lactose in molar ratios of 5:3 and 4:1 in lactose and lactose/trehalose systems. Trehalose seemed to crystallize as a mixture of trehalose dihydrate and anhydrate in trehalose and lactose/trehalose systems. The crystal forms in a mixture of lactose and trehalose did not seem to be affected by the component sugars, but crystallization of the component sugars was delayed. Time-dependent crystallization of lactose and trehalose in the lactose-trehalose mixture could be modeled using the Avrami equation. The results indicated that crystallization data are important in modeling of crystallization phenomena and predicting stability of lactose and trehalose-containing food and pharmaceutical materials. Keywords: crystallization, lactose, trehalose, crystal form, X-ray diffraction     

Multivariate near-infrared and Raman spectroscopic quantifications of the crystallinity of lactose in whey permeate powder

The use of near-infrared (NIR) and Fourier transform Raman spectroscopy for quantification of crystalline lactose content in whey permeate powder was investigated using chemometric methods. Sample sets consisting of binary mixtures of crystalline (50.0–98.0%) and amorphous lactose and process whey permeate samples with different amounts of crystalline lactose (75.0–95.5%) added were analyzed. The best results for quantification of crystallinity were obtained by partial least squares (PLS) regression on NIR data in five selected intervals in the range 1100–2498 nm. Data analysis on the total sample set of 35 samples yielded a prediction error (root mean square error of cross validation) of 0.627%. The corresponding result for Raman spectroscopy in the range 3500–100 cm⁻¹ was 1.62%. Interval-PLS regression was used for the selection of relevant spectral intervals as well as for improving the spectral interpretation. Alternating regression was used to show that the amorphous lactose preparation contained only a negligible amount of crystalline lactose.     

Lactose Hydrolysis in Ultrafiltration-Treated Cottage Cheese Whey with Various Whey Protein Concentrations

Lactose hydrolysis by soluble Aspergillus oryzaeβ-galactosidase was studied in (a) ultrafiltration (UF) permeate containing varying concentrations of isolated β-lactoglobulin or serum albumin; (b) UF retentate at four protein levels; and (c) cottage cheese whey during the UF treatment in an Amicon stirred cell unit. The rate and extent of lactose hydrolysis achieved in all the conditions studied was independent of protein concentration in the whey preparations used. After 6 hr of the simultaneous UF-lactose hydrolysis process at room temperature, similar hydrolysis level was achieved in the retentate as in the batch hydrolysis process. The average degree of hydrolysis in the permeate was 52.6%. The retentate added to milk at room temperature hydrolysed 93% of the lactose in 15 hr.     

Crystallization behavior of lactose/sucrose mixtures during water-induced crystallization

The crystallization behavior of lactose/sucrose mixtures during water-induced crystallization was studied to gain more insight about their crystallization during storage. Solutions with different ratios of lactose and sucrose, 75:25 and 50:50, were spray dried to produce amorphous powders. The powders were kept at a controlled temperature and humidity to study their sorption–desorption behavior. X-ray diffraction and light microscopy analysis were performed to study their crystallization behavior. Two-step desorption was observed after sieving the powders as sample preparation. Sieving decreased the crystallization time for lactose/sucrose mixture 75:25 from 22 days to 2.5 days. Based on the X-ray diffraction analysis during this two-step process of water desorption, it was concluded that lactose crystallizes first and more quickly than sucrose. The degree of crystallization for the lactose crystals increases by 89% (relative to their final level of crystallinity), whereas sucrose crystals increase their level of crystallinity by only 28% during the first step of crystallization in the lactose/sucrose (75:25) mixtures. The light microscopy images also suggested that the crystallization of amorphous lactose/sucrose powders during water-induced crystallization may occur as a solution rather than in the solid phase.     

Lactose crystallization delay in model infant foods made with lactose, beta-lactoglobulin, and starch

Handling and storage alter infant food powders due to lactose crystallization and interactions among components. Model infant foods were prepared by colyophilization of lactose, β-lactoglobulin (β-LG), and gelatinized starch. A mixture design was used to define the percentage of each mixture component to simulate a wide range of infant food powders. The kinetics of crystallization was studied by a gravimetric method (dynamic vapor sorption) at 70% relative humidity (RH). After freeze-drying, lactose was amorphous and crystallized at 70% RH. The delay before crystallization depends on the contents of β-LG and starch in the formulations. A mathematical model was proposed to predict crystallization time (delay) at 70% RH. For the formulation containing 50% lactose, 25% β-LG, and 25% starch, lactose was still amorphous after 42 h at 70% RH, whereas pure amorphous lactose crystallized after approximately 70 min. Calculated and experimental results of adsorbed moisture from the formulations were compared. Adsorbed water of formulation containing lactose could not be calculated from moisture sorption properties of each component at a given RH because β-LG and gelatinized starch prevented lactose crystal growth.