| 1. |
- Andersson, I. M., et al.
(författare)
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Impact of protein surface coverage and layer thickness on rehydration characteristics of milk serum protein/lactose powder particles
- 2019
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Ingår i: Colloids and Surfaces A. - : Elsevier BV. - 0927-7757 .- 1873-4359. ; 561, s. 395-404
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Tidskriftsartikel (refereegranskat)abstract
- Spray-dried powders were produced from milk serum protein concentrate and lactose in varying ratios, and the rehydration characteristics of the powders were evaluated. The dissolution rate was estimated with a flow-cell based technique, and the external and internal distribution of the powder components were evaluated with X-ray photoelectron spectroscopy and confocal Raman microscopy, respectively. The surface of the powder particles is more or less covered by a thin protein layer. A phase segregation between protein and lactose is observed in the interior of the particle resulting in a protein rich layer in the vicinity of the surface. However, the protein layer in the vicinity of the particle surface tends to become thinner as the bulk protein concentration increases in the powders (from 10 to 60% w/w). The time for the spontaneous imbibition to occur show a linear correlation with the protein surface coverage. The dissolution rate of powders containing 0.1% w/w protein is around 60 times faster than for a powder containing 1% w/w protein but the dissolution rate of powders containing 1% and 100% w/w differ only by a factor of 2. Thus, it is suggested that the outer protein layer becomes denser at the interface as the protein content increases in the powders, thereby causing poorer rehydration characteristics of the powders (especially for low protein concentrations 0.1–1% w/w). This insight has relevance for the formulation of whey protein powders with improved rehydration characteristics. © 2018 Elsevier B.V.
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| 2. |
- Andersson, I. M., et al.
(författare)
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Impact of surface properties on morphology of spray-dried milk serum protein/lactose systems
- 2018
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Ingår i: International Dairy Journal. - : Elsevier BV. - 0958-6946 .- 1879-0143. ; 85, s. 86-95
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Tidskriftsartikel (refereegranskat)abstract
- This study investigated milk serum protein concentrate/lactose systems with varying ratios and how the morphology of the spray-dried particles of these systems could be described by the surface properties of the feed as well as the protein surface coverage of the particles. An extrapolation of the surface pressure of the feed to 0.3 s, the approximate time for molecular diffusion in an atomised droplet in the spray-dryer, showed a relationship with the particle morphology. At low protein concentrations (<1%), the particles were almost totally smooth. At higher protein concentrations (≥1%), the particles became dented and ridged, and these tended to become deeper and thicker as the protein concentration increased. It is suggested that the surface pressure of the feed at low protein concentrations is the most prominent surface property, whereas the modulus of elasticity seems to be the most prominent surface property for particle surface deformation at higher protein concentrations.
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| 3. |
- Andersson, I. M., et al.
(författare)
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Particle morphology and rehydration properties of spray-dried microgels and fractal aggregates with varying fractions of native milk serum proteins
- 2021
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Ingår i: International Dairy Journal. - : Elsevier Ltd. - 0958-6946 .- 1879-0143. ; 112
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Tidskriftsartikel (refereegranskat)abstract
- To keep their functional properties, it is crucial that protein aggregates maintain their structure after spray drying and that the powders can be fully rehydrated. In this study, microgels and fractal aggregates were prepared by heating a mixture of milk serum protein concentrate and lactose (40/60; %, w/w) at 85 °C for 15 min by varying the pH. Various fractions of native proteins were added to the systems prior to spray drying. This study showed that microgels and fractal aggregates kept their structure after spray drying and reconstitution. The particle morphology could be correlated to the stiffness of the interface of the feed droplet. The forced imbibition rate showed a negative correlation with increasing amount of aggregated proteins in the powders that seems to be a result of denatured/aggregated proteins present at the surface. These findings are of importance for the formulation of spray-dried powders with improved rehydration characteristics. © 2020 The Author(s)
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| 4. |
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| 5. |
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| 6. |
- Badal Tejedor, Maria, 1986-, et al.
(författare)
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AFM Colloidal Probe Measurements Implicate Capillary Condensation in Punch-Particle Surface Interactions during Tableting
- 2017
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Ingår i: Langmuir. - : American Chemical Society (ACS). - 0743-7463 .- 1520-5827. ; 33:46, s. 13180-13188
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Tidskriftsartikel (refereegranskat)abstract
- Adhesion of the powders to the punches is a common issue during tableting. This phenomenon is known as sticking and affects the quality of the manufactured tablets. Defective tablets increase the cost of the manufacturing process. Thus, the ability to predict the tableting performance of the formulation blend before the process is scaled-up is important. The adhesive propensity of the powder to the tableting tools is mostly governed by the surface-surface adhesive interactions. Atomic force microscopy (AFM) colloidal probe is a surface characterization technique that allows the measurement of the adhesive interactions between two materials of interest. In this study, AFM steel colloidal probe measurements were performed on ibuprofen, MCC (microcrystalline cellulose), α-lactose monohydrate, and spray-dried lactose particles as an approach to modeling the punch-particle surface interactions during tableting. The excipients (lactose and MCC) showed constant, small, attractive, and adhesive forces toward the steel surface after a repeated number of contacts. In comparison, ibuprofen displayed a much larger attractive and adhesive interaction increasing over time both in magnitude and in jump-in/jump-out separation distance. The type of interaction acting on the excipient-steel interface can be related to a van der Waals force, which is relatively weak and short-ranged. By contrast, the ibuprofen-steel interaction is described by a capillary force profile. Even though ibuprofen is not highly hydrophilic, the relatively smooth surfaces of the crystals allow "contact flooding" upon contact with the steel probe. Capillary forces increase because of the "harvesting" of moisture - due to the fast condensation kinetics - leaving a residual condensate that contributes to increase the interaction force after each consecutive contact. Local asperity contacts on the more hydrophilic surface of the excipients prevent the flooding of the contact zone, and there is no such adhesive effect under the same ambient conditions. The markedly different behavior detected by force measurements clearly shows the sticky and nonsticky propensity of the materials and allows a mechanistic description.
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| 7. |
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| 8. |
- Badal Tejedor, Maria, et al.
(författare)
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Freeze-dried cake structural and physical heterogeneity in relation to freeze-drying cycle parameters
- 2020
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Ingår i: International Journal of Pharmaceutics. - : Elsevier B.V.. - 0378-5173 .- 1873-3476. ; 590
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Tidskriftsartikel (refereegranskat)abstract
- Freeze-drying is the preferred method to manufacture proteins in their solid state thus the understanding of the relationship between cycle parameters and cake properties remains of great interest. The present study aims to investigate the influence of the freezing conditions in the material properties at different layers throughout the dried structure, in the presence and absence of a protein. Placebo and protein formulations were dried applying different cooling rates: slow, fast and fast cooling with annealing. Non-uniform visual cake appearance, different pore sizes and endothermic events for release of structural water were observed throughout the cake at different freezing rates indicating heterogeneous properties of the dried material likely due to heating gradients during freezing. However, annealing increased the crystallinity and eliminated material inhomogeneities across the cake. The crystalline phase was mainly comprised of δ and hemihydrate mannitol (MHH) distributed at different ratios and influenced by the presence of the protein. The undesired formation of MHH is associated to currently used freezing temperatures or amorphous to crystalline material ratios. Thus, the correlation between the freezing step parameters and resulting material structure is a step forward to provide a better understanding of the freeze-dried cake formation and product quality improvement.
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| 9. |
- Badal Tejedor, Maria, 1986-, et al.
(författare)
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Milling induced amorphisation and recrystallization of α-lactose monohydrate
- 2018
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Ingår i: International Journal of Pharmaceutics. - : Elsevier BV. - 0378-5173 .- 1873-3476. ; 537:1-2, s. 140-147
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Tidskriftsartikel (refereegranskat)abstract
- Preprocessing of pharmaceutical powders is a common procedure to condition the materials for a better manufacturing performance. However, such operations may induce undesired material properties modifications when conditioning particle size through milling, for example. Modification of both surface and bulk material structure will change the material properties, thus affecting the processability of the powder. Hence it is essential to control the material transformations that occur during milling. Topographical and mechanical changes in surface properties can be a preliminary indication of further material transformations. Therefore a surface evaluation of the α-lactose monohydrate after short and prolonged milling times has been performed. Unprocessed α-lactose monohydrate and spray dried lactose were evaluated in parallel to the milled samples as reference examples of the crystalline and amorphous lactose structure. Morphological differences between unprocessed α-lactose, 1 h and 20 h milled lactose and spray dried lactose were detected from SEM and AFM images. Additionally, AFM was used to simultaneously characterize particle surface amorphicity by measuring energy dissipation. Extensive surface amorphicity was detected after 1 h of milling while prolonged milling times showed only a moderate particle surface amorphisation. Bulk material characterization performed with DSC indicated a partial amorphicity for the 1 h milled lactose and a fully amorphous thermal profile for the 20 h milled lactose. The temperature profiles however, were shifted somewhat in the comparison to the amorphous reference, particularly after extended milling, suggesting a different amorphous state compared to the spray-dried material. Water loss during milling was measured with TGA, showing lower water content for the lactose amorphized through milling compared to spray dried amorphous lactose. The combined results suggest a surface-bulk propagation of the amorphicity during milling in combination with a different amorphous structural conformation to that of the amorphous spray dried lactose. The hardened surface may be due to either surface crystallization of lactose or to formation of a low-water glass transition.
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| 10. |
- Badal Tejedor, Maria, et al.
(författare)
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Tablet mechanics depend on nano and micro scale adhesion, lubrication and structure
- 2015
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Ingår i: International Journal of Pharmaceutics. - : Elsevier. - 0378-5173 .- 1873-3476. ; 486:1-2, s. 315-323
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Tidskriftsartikel (refereegranskat)abstract
- Tablets are the most convenient form for drug administration. However, despite the ease of manufacturing problems such as powder adhesion occur during the production process. This study presents surface and structural characterization of tablets formulated with commonly used excipients (microcrystalline cellulose (MCC), lactose, mannitol, magnesium (Mg) stearate) pressed under different compaction conditions. Tablet surface analyses were performed with scanning electron microscopy (SEM), profilometry and atomic force microscopy (AFM). The mechanical properties of the tablets were evaluated with a tablet hardness test. Local adhesion detected by AFM decreased when Mg stearate was present in the formulation. Moreover, the tablet strength of plastically deformable excipients such as MCC was significantly decreased after addition of Mg stearate. Combined these facts indicate that Mg stearate affects the particle-particle bonding and thus elastic recovery. The MCC excipient also displayed the highest hardness which is characteristic for a highly cohesive material. This is discussed in the view of the relatively high adhesion found between MCC and a hydrophilic probe at the nanoscale using AFM. In contrast, the tablet strength of brittle materials like lactose and mannitol is unaffected by Mg stearate. Thus fracture occurs within the excipient particles and not at particle boundaries, creating new surfaces not previously exposed to Mg stearate. Such uncoated surfaces may well promote adhesive interactions with tools during manufacture.
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