Factors affecting droplet size of sodium caseinate‐stabilized O/W emulsions containing β‐carotene

This work was initiated to prepare an oil‐in‐water (O/W) emulsion containing β‐carotene by microfluidization. The β‐carotene was dissolved in triolein and microfluidized with an aqueous phase containing sodium caseinate (SC) as the emulsifier. Microfluization at 140 MPa resulted in O/W emulsions with a mean droplet diameter of ca. 120 nm, which was further confirmed by transmission electron microscopy analysis. The influences of SC concentration and microfluidization parameters on the droplet size of the emulsions were studied. The results showed that the mean droplet diameter decreased significantly (p <0.05) from 310 to 93 nm with the increase in SC concentration from 0.1 to 2 wt‐%. However, a further increase in SC concentration did not much change the droplet diameter, although the polydispersity of the emulsions was slightly improved. The droplet diameter of the emulsions was found to decrease from 200 to 120 nm with increasing microfluidization pressure, with narrower droplet size distribution. The storage study showed that the emulsions were physically stable for about 2 weeks at 4 °C in the dark. The results provide a better understanding of the performance of SC in stabilizing the O/W emulsions.     

High‐Pressure Homogenization as a Process for Emulsion Formation

Emulsions find a wide range of application in industry and daily life. In the pharmaceutical industry lipophilic active ingredients are often formulated in the disperse phase of oil‐in‐water emulsions. Milk, butter, and margarine are examples of emulsions in daily life. In the metal processing industry emulsions are used in the form of coolants. Emulsions can be produced with different systems. In the following, the process of high‐pressure homogenization is briefly compared to other common mechanical emulsification systems. To facilitate the selection of an emulsification system, the influence of the most important parameters of the emulsion formulation on the resulting mean droplet diameter in the most prevalent continuous emulsification systems is outlined. Subsequently, the most common high‐pressure homogenization systems are discussed in detail. On the basis of data from the literature and own experimental results the described high‐pressure homogenization systems will be compared regarding their attainable mean droplet diameter. It shows that homogenizers with a relatively simple geometry like the patented “combined orifice valve” (Kombi‐Blende) attain the smallest mean droplet diameters. The advantage of the “combined orifice valve” compared to other high‐pressure homogenization systems is not more efficient droplet disruption but rather more efficient droplet stabilization against coalescence immediately after the droplet breakup. The greatest research potential concerning the development of new high‐pressure homogenization systems is still to be seen in improvements of droplet stabilization, i.e., the reduction of coalescence.     

A Comparative Study of O/W Nanoemulsions Using Extra Virgin Olive or Olive‐Pomace Oil: Impacts on Formation and Stability

Nanoemulsions are considered an innovative approach for industrial food applications. The present study explored the potential use of olive‐pomace oil (OPO) for oil‐in‐water (o/w) nanoemulsion preparations and compared the effectiveness of extra virgin olive oil (EVOO) and OPO at nanoemulsion formulations. The ternary‐phase diagrams were constructed and the o/w nanoemulsions properties were evaluated in relation to their composition. The results showed that it is possible to form OPO nanoemulsions using Polysorbate 20 or Polysorbate 40. Nanoemulsions with EVOO and OPO presented desirable properties, in terms of kinetic stability (emulsion stability index % [ESI%]), mean droplet diameter (MDD), polydispersity index (PDI), ζ‐potential, viscosity, and turbidity. EVOO exhibited lower surface and interfacial tension forming nanoemulsions with a high ESI% and a low MDD. However, OPO led to nanoemulsions with a high ESI% but with a higher MDD. It was observed that by increasing the emulsifier concentration the MDD decreased, while increasing the dispersed phase concentration led to a higher MDD and a lower ESI%. Finally, nanoemulsions with the smallest MDD (99.26 ± 4.20 nm) and PDI (0.236 ± 0.010) were formed using Polysorbate 40, which presented lower surface and interfacial tension. Specifically, the nanoemulsion with 6 wt% EVOO and 6 wt% Polysorbate 40 demonstrated an interfacial tension of 51.014 ± 0.919 mN m^?1 and an MDD of 99.26 ± 4.20 nm. However, the nanoemulsion with 6 wt% OPO and 8 wt% Polysorbate 20 presented an interfacial tension of 54.308 ± 0.089 mN m^?1 and an MDD of 340.5 ± 7.1 nm.     

Enhanced Droplet Size Control in Liquid‐Liquid Emulsions Obtained in a Wire‐Guided X‐Mixer

The droplet size in a liquid‐liquid emulsion can be controlled by placing a metal wire along the centerline of an X‐mixer. Droplets gradually form when flowing along the wire, with droplet separation occurring at the tip of the wire rather than at the channel intersection in the X‐mixer. The droplet size is now defined by the Plateau‐Rayleigh instability developing in the axisymmetric annular flow region rather than by a sophisticated and hardly predictable three‐dimensional flow at the channel intersection. The wire‐guided droplet formation allows for fine control of the droplet size by changing the wire diameter, the position of the wire tip, and the flow rates. Further control of the droplet size can be achieved by adjusting the surface tension by adding a surfactant.     

Rotor‐Stator and Disc Systems for Emulsification Processes

Emulsions now find a wide range of applications in industry and daily life. In the pharmaceutical industry lipophilic active ingredients as well as many nutritional products such as vitamins are often formulated in the dispersed phase of oil‐in‐water emulsions. Emulsions can be produced with different mechanical emulsification techniques. In the following review, the process of rotor‐stator systems and disc systems are compared to other popular mechanical emulsification systems. On the basis of experimental results from the authors' laboratory, a discontinuous gear‐rim dispersing system, discontinuous disc system, and a continuous high pressure system are compared with regard to their attainable mean droplet diameter and drop size distribution in an oil‐in‐water emulsion. It can be shown that dissolver discs with a very simple geometry attain very small mean droplet diameters and a very narrow droplet size distribution, comparable to the emulsions obtained with established rotor‐stator systems such as gear‐rim dispersers.     

Thixotropic Behavior of Oil‐in‐Water Emulsions Stabilized with Ethoxylated Amines at Low Shear Rates

Oil‐in‐water (O/W) emulsification is a lubricating pipeline method based on the reduction of the energy frictional loss produced during viscous flow. The flow behavior of heavy O/W emulsions formulated with nonionic surfactants is described. The effects of pH and salinity of the aqueous phase on droplet diameter, stability, and apparent viscosity of O/W emulsions were evaluated. The low‐shear Couette flow of O/W emulsions displayed intense shear‐thinning and thixotropic behavior. Thixotropy was associated to the droplet deformation energy caused by shear rate changes. The droplet deformation and alignment led to the apparent viscosity reduction compared to the fluid at rest. Thixotropic behavior is supposed to balance between the breakdown and recovery of droplet ordered structures. Emulsion formulation parameters were influenced by the aqueous phase pH, enabling to manage the emulsion properties. The droplet mean diameter of < 18 µm resulted in very stable emulsions.     

Effect of air blowing on the morphology and nanofiber properties of blowing‐assisted electrospun polycarbonates

Polycarbonate (PC) nanofibers are prepared using the air blowing‐assisted electrospinning process. The effects of air blowing pressure and PC solution concentration on the physical properties of fibers and the filtration performance of the nanofiber web are investigated. The air blowing‐assisted electrospinning process produces fewer beads and smaller nanofiber diameters compared with those obtained without air blowing. Uniform PC nanofibers with an average fiber diameter of about 0.170 μm are obtained using an applied voltage of 40 kV, an air blowing pressure of 0.3 MPa, a PC solution concentration of 16%, and a tip‐to‐collection‐screen distance (TCD) of 25 cm. The filtration efficiency improvement of the air blowing‐assisted electrospun web can be attributed to the narrow distribution of fiber diameter and small mean flow pore size of the electrospun web. Performance results show that the air blowing‐assisted electrospinning process can be applied to produce PC nanofiber mats with high‐quality filtration. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

Influence of Flow Conditions in High‐Pressure Orifices on Droplet Disruption of Oil‐in‐Water Emulsions

Flow conditions in and behind high‐pressure orifices are described by a characteristic correlation between discharge coefficient and Reynolds number. The use of a pressure vessel and variations in viscosity allowed for non‐pulsating flow conditions from laminar to turbulent flow. Emulsions were homogenized under each condition. A considerable difference was observed in the final droplet size distribution depending on laminar, transitional, and turbulent flow. When the flow was pulsating as found when applying a plungers pump, transition of the flow from laminar to turbulence was more difficult to detect. Emulsions homogenized under these conditions indicated broader droplet size distributions. The Sauter mean diameter, however, was not affected by the pulsating flow.     

A low‐energy emulsification batch mixer for concentrated oil‐in‐water emulsions

This work shows the formation of a high internal phase ratio oil‐in‐water (O/W) emulsion using a new type of a two‐rod batch mixer. The mixture components have sharply different viscosities [1/3400 for water‐in‐oil (W/O)], similar densities (1/0.974 for W/O), and an O/W ratio of 91% (wt/wt). The simple design of this mixer leads to a low‐energy process (10⁶ < energy density [J m^?3] < 10⁷), characterized by low rotational speed and laminar flow. The droplet size distribution during the emulsification was investigated according to different physical and formulation parameters such as stirring time (few minutes < t < 1 h), rotational speed (60 < Ω < 120 rpm), surfactant type (Triton X‐405 and X‐100), concentration (from 1 to 15.9 wt % in water), and salt addition (30 g/L). We show that all studied parameters allow a precise control of the droplet size distribution and the rheology. The resulting emulsions are unimodal and the mean droplet diameter is between 30 μm and 8 μm. © 2010 American Institute of Chemical Engineers AIChE J, 2011     

In situ encapsulation of tetradecane droplets in oil‐in‐water emulsions using amino resins

Microcapsules of tetradecane enclosed by a polymeric wall of amino resin were synthesized by the in situ polymerization using melamine‐formaldehyde precondensates. It was found that resin concentrations of 60–240 g L^‐1 for a phase volume fraction of 0.14 and 0.29 and concentrations of 50–240 g L^‐1 for a phase volume fraction of 0.43 lead to stable microcapsules. Furthermore, the dependence of the shell thickness from the resin concentration for a phase volume fraction of 0.29 was investigated whereas the shell thickness was calculated from the density and the mean diameter of the capsules. It was found that below a concentration of 100 g L^?1 the density and thus the shell thickness increases linear with the resin concentration whereas at higher concentrations it almost remains constant and only the amount of the resin precipitated in solution increases. Additionally, it was shown that the mean droplet size (which is almost equal to the capsule size) in dependence of the stirring speed can be derived from the theory of droplet disruption. Thereby the coherence beginning with the stirring speed and the mean diameter to the total surface and the shell thickness is described. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

Parameter Selection of Emulsification Processes: Conditions for Nano‐ and Macroemulsions

Beside factors like nature of the emulsifier as well as rheology of the interface and continuous phase, the droplet size distribution of an emulsion governs emulsion properties such as long‐term stability over months or years, texture, and optical appearance. Consequently, emulsions with droplets in nano‐scale are of interest when well‐defined emulsion properties are needed. The formation of emulsions consisting of water, corn oil, and nonionic surfactants using disc systems and high‐pressure homogenizers was studied. The emulsion droplet size distributions were obtained by means of a laser diffraction method. The influence of parameters affecting the emulsion formation, such as emulsification time, viscosity for the disc system, pressure, and homogenizing steps for high‐pressure homogenization, was investigated. Data to determine the effect of the surfactant type and concentration were collected for both systems. The emulsification process using a disc system was evaluated in order to highlight its advantages and limits in comparison to high‐pressure homogenization.     

Dimensional analysis of a novel low‐pressure device for the production of size‐tunable nanoemulsions

A novel low pressure device was used to generate nanoemulsions of methyl methacrylate. This device is based on a strong elongational flow known to be more efficient than the shear flow for dispersive mixing. The influence of process parameters (pressure drop number of cycles, number and size of holes) and composition parameters (monomer fraction, surfactant concentration, etc) on droplet size has shown that the average droplet size can be tailored in the range 30–200 nm by adjusting these parameters. The objective of the present paper is to find correlations that relate the obtained droplet size to the studied process and composition parameters. This model is based on a dimensional analysis using the Buckingham theorem in order to determine appropriate dimensionless numbers. This approach represents a first step for scaling up the device besides giving a set of parameters allowing to achieve a given droplet size. © 2014 American Institute of Chemical Engineers AIChE J, 61: 23–30, 2015     

The role of microexplosions in flame spray synthesis for homogeneous nanopowders from low‐cost metal precursors

One of the most versatile and rapid manufacturing processes for a variety of nanopowders is flame spray pyrolysis (FSP). The production costs of this scalable process are largely controlled by the raw materials, pushing for the utilization of low‐cost metal precursors. These, however, typically yield inhomogeneous products containing large particles up to micrometer size along with fine nanoparticles. Here, the release mechanism of nitrate and carboxylate precursors from spray droplets has been investigated by single‐droplet combustion experiments and thermogravimetric analysis. The results show that neither precursor evaporation nor choice of solvents is prerequisite for homogeneous nanopowders but droplet microexplosions with continuing combustion. It is shown that even low‐cost metal nitrates yield homogeneous nanopowders if precursors are formulated such that droplet microexplosions occur by internal superheating. The proposed precursor release mechanisms are verified with lab‐ and pilot‐scale FSP, demonstrating that single‐droplet combustion experiments can be employed to predict the product quality. © 2015 American Institute of Chemical Engineers AIChE J, 62: 381–391, 2016     

Effect of fortified milk on lyso‐platelet‐activating factor acetyltranferase and lipoprotein‐associated phospholipase A2 in hypercholesterolemic adults

Hypercholesterolemia is associated with subclinical inflammation, characterised by elevated proinflammatory mediators. Lyso‐platelet‐activating factor acetyltransferase (lyso‐PAF AT) and lipoprotein‐associated phospholipase A₂ (Lp‐PLA₂) are two key metabolic enzymes of platelet‐activating factor (PAF), a potent inflammatory lipid mediator. Little information is available concerning the efficacy of a dietary intervention on the metabolism of PAF. The objective of the study was to evaluate the effect of fortified milk on the activity of these enzymes. Forty‐three adults (mean age 49.8 ± 8.1 years) with body mass index <35 kg/m², and total cholesterol >200 but <310 mg/dL were randomised to two groups; (i) intervention group received 500 mL/day (two glasses) of a low‐fat milk fortified with phytosterols, linoleic and alpha linolenic acids, vitamin C, vitamin E, vitamin A, vitamin B6, vitamin B12, folic acid, magnesium and selenium (n = 22), and (ii) placebo group received 500 mL/day of a conventional low‐fat milk (n = 21) for 3 months. Outcome measures were the activities of lyso‐PAF AT from leukocytes and serum Lp‐PLA₂ determined with established methods. None of the activities changed significantly during the study in the intervention group, lyso‐PAF AT (95% confidence interval: ?1.7, 2.3 nmol/min/mg; p = 0.246), and Lp‐PLA₂ (?7.8, 5.8 nmol/min/mL, p = 0.591). No difference was observed between the two groups. In conclusion, daily intake of two glasses of phytosterols, antioxidants, linoleic and linolenic acids via fortified milk for three months had no effect on the activity of either lyso‐PAF AT or Lp‐PLA₂. Practical applications: Platelet‐activating factor (PAF) was the first intact phospholipid known to have messenger functions in which the signaling results from the molecule binding to specific receptors on the plasma membrane or other membranes of the cell. It has a number of pro‐inflammatory properties, and affects several critical points of atherogenesis including thrombosis, inflammation, and oxidation. Fortification of milk with nutrients that possess anti‐inflammatory properties and administration to adults with elevated blood cholesterol could provide a means to controlling inflammatory process through the synthesis and degradation of PAF in a population group at risk for cardiovascular morbidity and mortality.     

Preparation and characterization of highly stable monodisperse argan oil‐in‐water emulsions using microchannel emulsification

Argan oil is well known for its nutraceutical properties. Its specific fatty acid composition and antioxidant content contribute to the stability of the oil and to its dietetic and culinary values. There is an increasing interest to use argan oil in cosmetics, pharmaceutics, and food products. However, the formulation of highly stable emulsions with prolonged shelf life is needed. In this study, argan oil‐in‐water (O/W) emulsions were prepared using microchannel (MC) emulsification process, stabilized by different non‐ionic emulsifiers. The effects of processing temperature on droplet size and size distribution were studied. Physical stability of argan O/W emulsions was also investigated by accelerated stability testing and during storage at room temperature (25 ± 2°C). Highly monodisperse argan O/W emulsions were produced at temperatures up to 70°C. The obtained emulsions were physically stable for several months at room temperature. Furthermore, emulsifier type, concentration, and temperature were the major determinants influencing the droplet size and size distribution. The results indicated that a suitable emulsifier should be selected by experimentation, since the interfacial tension and hydrophilic–lipophilic balance values were not suitable to predict the emulsifying efficiency. Practical applications: MC emulsification produces efficiently monodisperse droplets at wide range of temperatures. The findings of this work may be of great interest for both scientific and industrial purposes since highly stable and monodisperse argan oil‐in‐water emulsions were produced which can be incorporated into food, cosmetic, or pharmaceutical formulations.     

黄芩甙纳米乳的制备

研制了黄芩甙纳米乳并对其进行了质量评价。通过绘制伪三元相图优选处方,以肉豆蔻酸异丙酯(IPM)、液体石蜡和维生素E油为油相,蓖麻油聚氧乙烯醚(EL-40)为表面活性剂,乙醇为助表面活性剂制备黄芩甙纳米乳,用透射电子显微镜(TEM)、Nicomp388/ZetaPALS激光粒度测定仪分别考察了其形态和粒径;通过恒温加速实验检验了其稳定性。黄芩甙纳米乳在透射电镜下呈圆球形,分布均匀,平均粒径为(35.3±0.27)nm,恒温加速实验结果显示其未分层,仍为澄清透明纳米乳状液。纳米乳质量稳定,能提高黄芩甙的溶解度,且有很好的皮肤渗透性,提高了化妆品在皮肤上的延展性,可望用作皮肤化妆品基质。     

In Situ Viscosity‐Controlled Electrospinning with a Low Threshold Voltage

In the present study, a novel electrospinning method is proposed,where jet formation is aided by shearing the solution in situ. With a generalpolymer solution, viscosity decreases by shearing, that is, the solution isshear‐thinning. Poly(ethylene‐oxide) is used as a model polymer andthe effects of rotation speed, solution concentration, and gap size (the widthof the annular orifice) on the process and the morphology of the obtainedfibers are investigated. It is found that the threshold voltage for generatingmultiple jets decreased from 35 to 12 kV when rotation speed is higher than60 rpm (or shear rate more than 310 s^?1). Additionally, the results show thatfiber diameter increases as the concentration of the solution increases. Thechi‐square two‐sample test is used to compare the distribution of fibersproduced by the capillary method and the novel electrospinning process. Inthe authors' method, the viscosity of the solution can be changed by applyingmechanical forces on it during the electrospinning process, which results inthe initiation of the electrospinning jet at a low threshold voltage. It is alsofound that gap size has a similar effect on fiber diameter as needle diameter in classical electrospinning.     

Control of the morphology and the size of complex coacervate microcapsules during scale‐up

Scale‐up of complex coacervation, a fat encapsulation technology, is not trivial since the microcapsules morphology and size are highly affected by the processing conditions. So far it has been achieved empirically (trial and error approach). The goal of this study was to produce at various scale capsules with a single‐oil droplet as the core material and small enough to be below sensory threshold. The turbulence level was identified as the main scale‐up criterium and a master‐curve could be drafted showing the capsule mean diameter as function of the Reynolds number, independent of the level of production scale. From a parent emulsion with specific oil droplets size (12–15 μm), the Reynolds number had to be maintained above a critical value (15,000) to avoid capsules agglomeration with multiple oil cores and large particle sizes. To avoid aggregation, this turbulence level had to be kept until the temperature dropped below a critical value (14°C for a cooling rate of 35°C/2 h). Applying these learning led to a successful scale‐up from bench (2 L) to a pilot plant scale of 50 L. © 2009 American Institute of Chemical Engineers AIChE J, 2009     

An Electrospray Method Using a Multi‐Capillary Nozzle Emitter

A multi‐capillary nozzle emitter consisting of one metal plate with capillary nozzles and a ring type counter electrode was used as a multi‐electrospray atomizer. The number of capillary nozzles, flow rate of the liquid and the interval between the capillary nozzles were changed, and the droplet diameter and the voltage required for a steady cone‐jet mode were measured. For the multi‐capillary nozzle emitter, the interaction between the capillary nozzles is the important factor for obtaining fine droplets of uniform size. These fine droplets are obtained when there is only a small interaction between the capillary nozzles, and the equations obtained from the single capillary nozzle case are also applicable for the multi‐capillary nozzle emitter. When the number of capillary nozzles decreases (a situation which is not good for obtaining a large amount of droplets) or the interval between the capillary nozzles increases, the interaction between the capillary nozzles can be reduced. As the number of capillary nozzles increase, a higher voltage is required to obtain a fine droplet of uniform size.     

Actual air separation through poly(aniline‐co‐toluidine)/ethylcellulose blend thin‐film composite membranes

Several multilayer thin‐film composite membranes were fabricated of ethylcellulose (EC) and poly(aniline‐co‐ortho‐toluidine) or poly(ortho‐toluidine) blend as selective thin films and three ultrafiltration membranes with a 10‐ to 45‐nm pore size and 100‐ to 200‐μm thickness as porous supports. The relationships between the actual air‐separation performance through the composite membranes and layer number, composition, casting solution concentration of the thin selective film are discussed. The oxygen‐enriched air (OEA) flux through the composite membranes increases steadily with increasing operational temperature and pressure. The oxygen concentration enriched by the composite membranes appears to decrease with operating temperature, but increases with operating pressure. The actual air‐separation property through the composite membranes seems to remain nearly constant for at least 320 days. The respective highest OEA flux, oxygen flux, and oxygen concentration, respectively, were found to be 4.78 × 10⁻⁵ cm³ (STP)/s · cm², 2.2 × 10⁻⁵ cm³ (STP)/s · cm², and 46% across EC/poly(o‐toluidine) (80/20) blend monolayer thin‐film composite membranes in a single step at 20°C and 650 kPa operating pressure. © 2000 John Wiley & Sons, Inc. J Appl Polym Sci 75: 458–463, 2000