Permeate Flux During Ultrafiltration of Whey: Influence of Milk Coagulant Used for Cheese Manufacture

A pilot-scale plate and frame UF system was used to fractionate Cheddar cheese whey and study the effects of different commercial milk coagulants on permeate flux. Coagulants used in this study were calf rennet, Mucor pusillus protease, and Mucor miebei protease. Whey UF performance studies were conducted at a commercial Cheddar cheese plant and at Cornell under controlled conditions. Ultrafiltration was done in a continuous mode and initial concentration factor was set at 2× to simulate the first stage of a multistage whey UF system.Permeate flux decline was rapid in the first 30 min of UF for all wheys studied. More important, the type of milk coagulant used in cheese making had a profound effect on permeate flux during whey UF. No differences in the gross composition of the various wheys were correlated with differences in permeate flux. The highest permeate flux was measured for UF of whey produced during manufacture of Cheddar cheese using coagulant derived from Mucor pusillus. Lowest permeate flux was measured for UF of whey produced during manufacture of Cheddar cheese using calf rennet. Whey from cheese manufactured using Mucor miebei coagulant had flux performance intermediate to Mucor pusillus and calf rennet. The impact of milk coagulants on whey UF process efficiency should be considered by cheese makers.     

Preparation of milk protein concentrates by ultrafiltration and continuous diafiltration: Effect of process design on overall efficiency

High-milk-protein concentrates (>80% on a dry weight basis) are typically produced by ultrafiltration (UF) with constant-volume diafiltration (DF). To maximize protein retention at a commercial scale, polymeric spiral-wound UF membranes with a molecular weight cut-off (MWCO) of 10 kDa are commonly used. Flux decline and membrane fouling during UF have been studied extensively and the selection of an optimal UF-DF sequence is expected to have a considerable effect on both the process efficiency and the volumes of by-products generated. The objective of this study was to characterize the performance of the UF-DF process by evaluating permeate flux decline, fouling resistance, energy and water consumption, and retentate composition as a function of MWCO (10 and 50 kDa) and UF-DF sequence [3.5×–2 diavolumes (DV) and 5×–0.8DV]. The UF-DF experiments were performed on pasteurized skim milk using a pilot-scale filtration system operated at 50°C under a constant transmembrane pressure of 465 kPa. The results showed that MWCO had no effect on permeate flux for the same UF-DF sequence. Irreversible resistance was also similar for both sequences, whatever the MWCO, suggesting that soluble protein deposition within the pores is similar for all conditions. Despite lower permeate fluxes and greater reversible resistance for the 5×–0.8DV sequence, the overall energy consumption of the 2 UF-DF sequences was similar. However, the 3.5×–2DV sequence required more water for DF and generated larger volumes of permeate to be processed, which will require more membrane area and lead to greater environmental impact. A comparative life cycle assessment should however be performed to confirm which sequence has the lowest environmental impact.     

Flux pattern and fouling of membranes during ultrafiltration of some dairy products

The flux pattern of milk (whole milk, skimmed milk and buttermilk) showed a distinct contrast to whey (sweet whey and acid casein whey) systems during ultrafiltration (UF) at constant composition. For milk systems, the initial flux was lower than for whey systems, but the flux stabilised within a few minutes of operation. However, for both acid and sweet whey, the flux continued to fall with time for nearly 1 h. The fouling coefficient (FC) for buttermilk was 0.6 after 5 min, rising to 0.68 after 60 min. During this time flux did not decline, suggesting that concentration polarisation (CP), rather than fouling, was controlling the flux rate. In contrast, the FC for whey was 0.5 after 5 min with a progressive rise over the next 55 min, but the flux also fell throughout this period suggesting that flux was controlled by fouling rather than CP. The higher concentration of protein in milk systems appeared to be responsible for CP, rather than fouling, being the controlling mechanism.     

Influence of partial acidification of skim milk on ultrafiltration performance and physicochemical properties of the produced streams

The influence of partial acidification of skim milk (SM) using glucono-δ-lactone (GDL), citric acid (CA) or lactic acid (LA), on physicochemical properties (e.g. viscosity and calcium balance) of ultrafiltration (UF) retentates produced at 10 and 55°C was investigated. Ultrafiltration retentates produced using CA showed a significantly lower amount (P < 0.05) of ionic calcium and higher apparent viscosity than GDL and LA. Regardless of the acid used, total calcium concentration and apparent viscosity of streams were modified compared with SM, which impaired UF overall performance. Specifically, CA at 10°C and GDL at 55°C, both reduced the permeate flux when compared to the other acids.     

Concentration of Skim Milk by a Cascade Comprised of Ultrafiltration and Nanofiltration: Investigation of the Nanofiltration of Skim Milk Ultrafiltration Permeate

In order to reach a high volume reduction ratio (VRR) prior to drying of skim milk, a membrane cascade comprising of an ultrafiltration (UF) coupled with a nanofiltration (NF) can be applied. The present study investigated the impact of processing (filtration temperature, transmembrane pressure (TMP)) and product (feed pH) parameters on the NF of skim milk UF permeate. It could be shown that a low filtration temperature of 10 °C is more advantageous in terms of flux stability and rejection of the solute fraction as compared to higher filtration temperatures up to 45 °C. The solution pH did not affect permeate flux and lactose retention. However, in order to avoid calcium losses, it is more favorable to conduct the concentration at a pH of 6.8 instead of at a lower pH of 5. The application of a higher TMP (up to 4 MPa) enhances permeate flux and VRR as well as solute rejection during concentration of UF permeate. It was also shown that the retention of solutes decreases towards the end of the concentration process. As a consequence, the achievement of high final VRR must be weighed against increased product losses at the end.     

Effects of hydrodynamic cavitation and temperature on nanofiltration performance for concentrating ultrafiltered skim milk

The performance of nanofiltration (NF) as influenced by hydrodynamic cavitation (HC) and filtration temperature during the concentration of milk protein concentrate (MPC) was investigated. Pasteurised skim milk was concentrated using ultrafiltration (UF) to prepare UF retentate (MPC80, 20% total solids, TS), which was then further concentrated using NF at 22°C and 50°C with or without HC treatments until permeate flux declined to 0.1 L/m²/h. Results showed that UF retentate can be concentrated to higher TS (up to 31.5%) at higher filtration temperature or by applying HC, with synergistic effect in combination of both treatments, during NF.     

Comparison of Rat Hepatic Cholesterol Biosynthesis During Skim Milk Versus Whey Permeate Ingestion

Whey permeate is an ultrafiltrate of whey that is devoid of protein but contains lactose, salts, and other soluble low molecular weight compounds. These experiments compared cholesterol concentrations of blood plasma, hepatic lipids, and hepatic cholesterol biosynthesis of rats ingesting skim milk powder versus whey permeate powder. Groups of young male rats weighing 90 to 92 g were fed a casein-based diet into which skim milk powder or whey permeate powder was incorporated isocalorically. No effects of skim milk or whey permeate on plasma cholesterol concentrations were observed at any time during 5-wk of feeding. However, 3-hydroxy-3-methylglutaryl coenzyme A reductase activity was increased by either skim milk or whey permeate feeding. Hepatic cholesterol, triglyceride, and phospholipid concentrations at wk 5 were unchanged. Plasma and hepatic cholesterol responses of rats to whey permeate ingestion are similar to those that occur with skim milk consumption, and plasma and hepatic cholesterol concentrations do not reflect necessarily an increase in hepatic cholesterol biosynthesis.     

Performance assessment of membrane distillation for skim milk and whey processing

Membrane distillation is an emerging membrane process based on evaporation of a volatile solvent. One of its often stated advantages is the low flux sensitivity toward concentration of the processed fluid, in contrast to reverse osmosis. In the present paper, we looked at 2 high-solids applications of the dairy industry: skim milk and whey. Performance was assessed under various hydrodynamic conditions to investigate the feasibility of fouling mitigation by changing the operating parameters and to compare performance to widespread membrane filtration processes. Whereas filtration processes are hydraulic pressure driven, membrane distillation uses vapor pressure from heat to drive separation and, therefore, operating parameters have a different bearing on the process. Experimental and calculated results identified factors influencing heat and mass transfer under various operating conditions using polytetrafluoroethylene flat-sheet membranes. Linear velocity was found to influence performance during skim milk processing but not during whey processing. Lower feed and higher permeate temperature was found to reduce fouling in the processing of both dairy solutions. Concentration of skim milk and whey by membrane distillation has potential, as it showed high rejection (>99%) of all dairy components and can operate using low electrical energy and pressures (<10 kPa). At higher cross-flow velocities (around 0.141 m/s), fluxes were comparable to those found with reverse osmosis, achieving a sustainable flux of approximately 12 kg/h·m² for skim milk of 20% dry matter concentration and approximately 20 kg/h·m² after 18 h of operation with whey at 20% dry matter concentration.     

Effective control of microbial populations in polysulfone ultrafiltration membrane systems

Sanitizers currently used in the food industry are not efficient in destroying bacterial populations in polysulfone UF membrane systems. A new sanitizer composition that releases chlorous acid and chlorine dioxide from sodium chlorite at pH 2.7 was evaluated. Polysulfone UF membranes were soiled for 2.5 h by circulating and concentrating Cheddar cheese whey and skim milk. A cleaning regimen was established whereby acid and caustic cleaning solutions were circulated to clean the UF membrane system. Restoring permeate flux to initial values did not indicate that the system was effectively cleaned. The UF system was sanitized by recycling sanitizer solutions. Stainless steel and membrane surfaces were examined by swabbing to determine bacterial populations and sections of membranes were removed for examination using a scanning electron microscope. The new sanitizer appeared to control microbial populations effectively in UF membrane systems.     

Potential application of high hydrostatic pressure to eliminate Escherichia coli O157:H7 on alfalfa sprouted seeds

Sprouts eaten raw are increasingly being perceived as hazardous foods as they have been implicated in Escherichia coli O157:H7 outbreaks where the seeds were found to be the likely source of contamination. The objective of our study was to evaluate the potential of using high hydrostatic pressure (HHP) technology for alfalfa seed decontamination. Alfalfa seeds inoculated with a cocktail of five strains of E. coli O157:H7 were subjected to pressures of 500 and 600 MPa for 2 min at 20 degrees C in a dry or wet (immersed in water) state. Immersing seeds in water during pressurization considerably enhanced inactivation of E. coli O157:H7 achieving reductions of 3.5 log and 5.7 log at 500 and 600 MPa, respectively. When dry seeds were pressurized, both pressure levels reduced the counts by <0.7 log. To test the efficacy of HHP to completely decontaminate seeds whilst meeting the FDA requirement of 5 log reductions, seeds inoculated with a ~5 log CFU/g of E. coli O157:H7 were pressure-treated at 600 and 650 MPa at 20 degrees C for holding times of 2 to 20 min. A >5 log reduction in the population was achieved when 600 MPa was applied for durations of > or =6 min although survivors were still detected by enrichment. When the pressure was stepped up to 650 MPa, the threshold time required to achieve complete elimination was 15 min. Un-inoculated seeds pressure-treated at 650 MPa for 15 min at 20 degrees C successfully sprouted achieving a germination rate identical to untreated seeds after eight days of sprouting. These results therefore demonstrate the promising application of HHP on alfalfa seeds to eliminate the risk of E. coli O157:H7 infections associated with consumption of raw alfalfa sprouts.     

Effect of Fouling on Flux and on Energy Requirements in Reverse Osmosis of Skim Milk

The effects of fouling on the permeate flux and on the power and energy required in the process of concentrating skim milk by a plate and frame type reverse osmosis unit with 990 type cellulose-acetate membranes were investigated. The permeate flow characteristics indicate that the fouling layer is rapidly formed and that its resistance is nearly constant over reasonable processing intervals. These fouling properties permit the correlation of permeate flow, overall mass transfer coefficient, and osmotic pressure difference in terms of the energy required per permeate volume versus time. This correlation shows a decrease in energy required per permeate volume with increasing mass transfer coefficient and time. These flow characteristics permit the estimation with confidence of the permeate flow energy requirements and the capacity of a full scale plant. Mass transfer coefficients were estimated for the membrane, the polarized layer, and the fouling layer. The overall mass transfer coefficient was then calculated. The polarized and fouling layers are films of components from the skim milk. Fouling was the controlling resistance.     

High pressure effects on the colloidal calcium phosphate and the structural integrity of micellar casein in milk. Part 1. High pressure dissolution of colloidal calcium phosphate in heated milk systems

Results of this study confirm that high temperature (118°C/15 min) and high pressure (400 MPa/5 min) processing of skim milk, skim milk ultrafiltration and ultracentrifugation fractions, and model milk salt solutions cause dramatic shifts in their colloidal and soluble Ca phospate equilibrium that affect their pH, dissolved Ca content, turbidity, and casein micelle microstructure. The relations between high temperature and high pressure processing-induced changes in the colloidal and soluble Ca phosphate equilibrium were evaluated in raw, pasteurized, and high temperature treated skim milk, ultrafiltration retentate and permeate of pasteurized skim milk, clear ultracentrifugation infranatant of pasteurized skim milk, and synthetic milk ultrafiltrates with and without lactose or Ca. The magnitude of the pH and dissolved Ca shifts caused by high temperature and high pressure processing was a function of casein micelle concentration. Ultrafiltration permeate exhibited the most drastic shifts in pH and dissolved Ca contents due to high temperature and high pressure processing. Although high temperature processing reduced the pH of ultrafiltration permeate from 6.59 to 6.03 and the dissolved Ca from 100% to 58%, high pressure processing reversed both of these changes. These changes in high temperature and high pressure processed milk, milk fractions, and model milk salt solutions were related to microstructural changes in the casein micelles as revealed by electron microscopy.     

Pilot-scale ceramic membrane filtration of skim milk for the production of a protein base ingredient for use in infant milk formula

The protein composition of bovine skim milk was modified using pilot scale membrane filtration to produce a whey protein-dominant ingredient with a casein profile closer to human milk. Bovine skim milk was processed at low (8.9 °C) or high (50 °C) temperature using ceramic microfiltration (MF) membranes (0.1 μm mean pore diameter). The resulting permeate stream was concentrated using polyethersulfone ultrafiltration (UF) membranes (10 kDa cut-off). The protein profile of MF and UF retentate streams were determined using reversed phase-high performance liquid chromatography and polyacrylamide gel electrophoresis. Permeate from the cold MF process (8.9 °C) had a casein:whey protein ratio of ∼35:65 with no α_S- or κ-casein present, compared with a casein:whey protein ratio of ∼10:90 at 50 °C. This study has demonstrated the application of cold membrane filtration (8.9 °C) at pilot scale to produce a dairy ingredient with a protein profile closer to that of human milk.     

THE FOULING AND CLEANING OF ULTRAFILTRATION MEMBRANES DURING THE FILTRATION OF MODEL TEA COMPONENT SOLUTIONS

Proteins and polyphenols are the principal fouling constituents in the ultrafiltration (UF) of black tea liquor. The aim of this study was to determine the relative importance of individual components in the fouling process, to investigate any synergetic interactions that were occurring and to compare the cleaning characteristics of different fouled membranes. A 30‐kD molecular weight cutoff polysulfone UF membrane in dead‐end mode was challenged with model solutions of tea components. Model solutions consisted of tea proteins, theaflavins (TFs), thearubigins and caffeine. Sodium hydroxide was used as a cleaning reagent. Permeate flux decline curves were presented for single components and mixtures. Individual component transfer fluxes and rejections were also presented. An unexpected finding was that protein in a mixture with TFs could permeate the membrane to a degree, while a protein solution in the absence of the polyphenol was completely rejected. The inspection of membranes fouled by different solutions revealed different foulant morphologies. Membrane cleaning with 0.2 wt % sodium hydroxide was generally found to be effective.     

Partition of lactic streptococcal bacteriophage during the ultrafiltration concentration of milk and whey

Milk and whey inoculated with lactic streptococcal bacteriophages 316, or 322, or both were concentrated by UF using a DDS Mini-Lab 20. The plate and frame unit was fitted with Type GR61PP polysulfone membrane with a 20,000 molecular weight cutoff. The unit was operated at an inlet pressure of .40 MPa and an outlet pressure of .23 MPa with an initial flux of 2.0 to 3.0 L/h. Samples of retentate, permeate, and membrane were analyzed for the presence of bacteriophages. Under the conditions established in this study, phage particles did not pass through the membrane but instead became trapped in the polarization concentration layer or in the membrane. Phages were recovered from the membrane by extraction in sterile buffered water with the Stomacher. The UF concentration of milk containing the host species of Streptococcus cremoris resulted in phage propagation and lysis of the host but did not result in the passage of phages through the membrane. The UF processing of milk or whey should produce a phage-free permeate.     

Combined pH and high hydrostatic pressure effects on Lactococcus starter cultures and Candida spoilage yeasts in a fermented milk test system during cold storage

The combined effects of high pressure processing (HPP) and pH on the glycolytic and proteolytic activities of Lactococcus lactis subsp. lactis, a commonly used cheese starter culture and the outgrowth of spoilage yeasts of Candida species were investigated in a fermented milk test system. To prepare the test system, L. lactis subsp. lactis C10 was grown in UHT skim milk to a final pH of 4.30 and then additional samples for treatment were prepared by dilution of fermented milk with UHT skim milk to pH levels of 5.20 and 6.50. These milk samples (pH 4.30, 5.20 and 6.50) with or without an added mixture of two yeast cultures, Candida zeylanoides and Candida lipolytica (10⁵ CFU mL⁻¹ of each species), were treated at 300 and 600 MPa (≤20 °C, 5 min) and stored at 4 °C for up to 8 weeks. Continuing acidification by starter cultures, as monitored during storage, was substantially reduced in the milk pressurised at pH 5.20 where the initial titratable acidity (TA) of 0.40% increased by only 0.05% (600 MPa) and 0.10% (300 MPa) at week 8, compared to an increase of 0.30% in untreated controls. No substantial differences were observed in pH or TA between pressure-treated and untreated milk samples at pH 4.30 or 6.50. The rate of proteolysis in milk samples at pH values of 5.20 and 6.50 during storage was significantly reduced by treatment at 600 MPa. Treatment at 600 MPa also reduced the viable counts of both Candida yeast species to below the detection limit (1 CFU mL⁻¹) at all pH levels for the entire storage period. However, samples treated at 300 MPa showed recovery of C. lipolytica from week 3 onwards, reaching 10⁶–10⁷ CFU mL⁻¹ by week 8. In contrast, C. zeylanoides did not show any recovery in any of the pressure-treated samples during storage.     

Partial Characterization of Protease Activity in Squid (Todaropsis eblanae) Mantle: Modification by High-pressure Treatment

ABSTRACT: Optimal conditions for proteolytic activity in both nonpressurized and pressurized (300 MPa, 7°C, 20 min) squid ( Todaropsis eblanae ) muscle occurred at acid pH levels (pH 3) over a broad range of temperatures. Pressure treatment did not modify optimal pH and temperatures but did increase proteolytic activity. The acid cysteine proteases, and to a lesser extent the acid serine proteases, were the enzymes mainly affected by the high-pressure treatment. The sodium dodecyl sulfate-polyacrylamide gel electrophoresis (SDS-PAGE) was indicative of increased protein hydrolysis by pressurization. Myosin heavy chain in both nonpressurized and pressurized squid was degraded at all the temperatures tested, but actin was susceptible only to proteolysis in the pressure-treated muscle at 7°C and 40°C. This behavior was not observed at 55°C.     

High hydrostatic pressure modification of whey protein concentrate for improved functional properties

Whey protein concentrate (WPC) has many applications in the food industry. Previous research demonstrated that treatment of whey proteins with high hydrostatic pressure (HHP) can enhance solubility and foaming properties of whey proteins. The objective of this study was to use HHP to improve functional properties of fresh WPC, compared with functional properties of reconstituted commercial whey protein concentrate 35 (WPC 35) powder. Fluid whey was ultrafiltered to concentrate proteins and reconstituted to equivalent total solids (8.23%) as reconstituted commercial WPC 35 powder. Solutions of WPC were treated with 300 and 400 MPa (0- and 15-min holding time) and 600 MPa (0-min holding time) pressure. After HHP, the solubility of the WPC was determined at both pH 4.6 and 7.0 using UDY and BioRad protein assay methods. Overrun and foam stability were determined after protein dispersions were whipped for 15 min. The protein solubility was greater at pH 7.0 than at pH 4.6, but there were no significant differences at different HHP treatment conditions. The maintenance of protein solubility after HHP indicates that HHP-treated WPC might be appropriate for applications to food systems. Untreated WPC exhibited the smallest overrun percentage, whereas the largest percentage for overrun and foam stability was obtained for WPC treated at 300 MPa for 15 min. Additionally, HHP-WPC treated at 300 MPa for 15 min acquired larger overrun than commercial WPC 35. The HHP treatment of 300 MPa for 0 min did not improve foam stability of WPC. However, WPC treated at 300 or 400 MPa for 15 min and 600 MPa for 0 min exhibited significantly greater foam stability than commercial WPC 35. The HHP treatment was beneficial to enhance overrun and foam stability of WPC, showing promise for ice cream and whipping cream applications.     

Development and optimization of a carbon dioxide-aided cold microfiltration process for the physical removal of microorganisms and somatic cells from skim milk

Physical removal of microorganisms from skim milk by microfiltration (MF) is becoming increasingly attractive to the dairy industry. Typically, this process is performed at temperatures of approximately 50°C. Additional shelf-life and quality benefits might be gained by conducting the MF process at low temperatures. Cold MF could also minimize microbial fouling of the membrane and prevent the germination of thermophilic spores. The objective of this study was to optimize a cold MF process for the effective removal of microbial and somatic cells from skim milk. An experimental MF setup containing a tubular Tami ceramic membrane with a nominal pore size of 1.4 μm was used for MF of raw skim milk at a temperature of 6 ± 1°C. The processing conditions used were cross-flow velocities of 5 to 7 m/s, and transmembrane pressures of 52 to 131 kPa. All MF experiments were performed in triplicate. The permeate flux was determined gravimetrically. Microbiological, chemical, and somatic cell analyses were performed to evaluate the effect of MF on the composition of skim milk. The permeate flux increased drastically when velocity was increased from 5 to 7 m/s. The critical transmembrane pressure range conducive to maximum fluxes was 60 to 85 kPa. When MF was conducted under optimal conditions, very efficient removal of vegetative bacteria, spores, and somatic cells, as well as near complete transmission of proteins into the MF milk, was achieved. To further enhance the flux, a CO₂ backpulsing system was developed. This technique is able both to increase the flux and to maintain it steadily for an extended period of time. The CO₂-aided cold MF process has the potential to become economically attractive to the dairy industry, with direct benefits for the quality and shelf life of dairy products.     

A physicochemical investigation of membrane fouling in cold microfiltration of skim milk

The main challenge in microfiltration (MF) is membrane fouling, which leads to a significant decline in permeate flux and a change in membrane selectivity over time. This work aims to elucidate the mechanisms of membrane fouling in cold MF of skim milk by identifying and quantifying the proteins and minerals involved in external and internal membrane fouling. Microfiltration was conducted using a 1.4-μm ceramic membrane, at a temperature of 6 ± 1°C, cross-flow velocity of 6 m/s, and transmembrane pressure of 159 kPa, for 90 min. Internal and external foulants were extracted from a ceramic membrane both after a brief contact between the membrane and skim milk, to evaluate instantaneous adsorption of foulants, and after MF. Four foulant streams were collected: weakly attached external foulants, weakly attached internal foulants, strongly attached external foulants, and strongly attached internal foulants. Liquid chromatography coupled with tandem mass spectrometry analysis showed that all major milk proteins were present in all foulant streams. Proteins did appear to be the major cause of membrane fouling. Proteomics analysis of the foulants indicated elevated levels of serum proteins as compared with milk in the foulant fractions collected from the adsorption study. Caseins were preferentially introduced into the fouling layer during MF, when transmembrane pressure was applied, as confirmed both by proteomics and mineral analyses. The knowledge generated in this study advances the understanding of fouling mechanisms in cold MF of skim milk and can be used to identify solutions for minimizing membrane fouling and increasing the efficiency of milk MF.