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Millqvist-Fureby, AnnaORCID iD iconorcid.org/0000-0001-9891-8968
Publications (10 of 25) Show all publications
Andersson, I. M., Millqvist-Fureby, A., Sommertune, J., Alexander, M., Hellström, N., Glantz, M., . . . Bergenståhl, B. (2019). Impact of protein surface coverage and layer thickness on rehydration characteristics of milk serum protein/lactose powder particles. Colloids and Surfaces A: Physicochemical and Engineering Aspects, 561, 395-404
Open this publication in new window or tab >>Impact of protein surface coverage and layer thickness on rehydration characteristics of milk serum protein/lactose powder particles
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2019 (English)In: Colloids and Surfaces A: Physicochemical and Engineering Aspects, ISSN 0927-7757, E-ISSN 1873-4359, Vol. 561, p. 395-404Article in journal (Refereed) Published
Abstract [en]

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.

Keywords
Confocal raman microscopy, Lactose, Milk serum protein, Phase segregation, Rehydration, Spray drying, Body fluids, Dissolution, Phase separation, Powders, Segregation (metallography), Sugars, Surface segregation, X ray photoelectron spectroscopy, Milk serum proteins, Phase segregations, Proteins
National Category
Natural Sciences
Identifiers
urn:nbn:se:ri:diva-36591 (URN)10.1016/j.colsurfa.2018.10.073 (DOI)2-s2.0-85056673089 (Scopus ID)
Note

Funding details: Lunds Universitet

Available from: 2018-12-17 Created: 2018-12-17 Last updated: 2018-12-17Bibliographically approved
Boge, L., Västberg, A., Umerska, A., Bysell, H., Eriksson, J., Edwards, K., . . . Andersson, M. (2018). Freeze-dried and re-hydrated liquid crystalline nanoparticles stabilized with disaccharides for drug-delivery of the plectasin derivative AP114 antimicrobial peptide. Journal of Colloid and Interface Science, 522, 126-135
Open this publication in new window or tab >>Freeze-dried and re-hydrated liquid crystalline nanoparticles stabilized with disaccharides for drug-delivery of the plectasin derivative AP114 antimicrobial peptide
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2018 (English)In: Journal of Colloid and Interface Science, ISSN 0021-9797, E-ISSN 1095-7103, Vol. 522, p. 126-135Article in journal (Refereed) Published
Abstract [en]

Liquid crystalline nanoparticles (LCNPs), e.g. cubosomes and hexosomes, are receiving more and more attraction as drug delivery vehicles. Dry powder formulation that forms LCNPs upon hydration can be advantageous to make new routes of administration accessible. In this work, we investigate use of three disaccharides (lactose, trehalose and sucrose) as protective matrices for glycerol monooleate based LCNP forming powders produced by freeze-drying. Phase behavior, particle size and size distributions at the different preparation steps were monitored by small angle x-ray scattering (SAXS) and dynamic light scattering (DLS). Particle appearance was imaged by cryogenic transmission electron microscopy (cryo-TEM). Moreover, the therapeutic relevant antimicrobial peptide AP114 (plectasin derivative) was incorporated in the formulations. Peptide encapsulation and release as well as in vitro antibacterial effect were investigated. Results showed that all freeze-dried powders did form particles with liquid crystalline structure upon hydration. However, a phase transition from the bicontinuous cubic Pn3m to the reversed hexagonal was observed, as a consequence of sugar addition and the freeze-drying procedure. Data indicates that trehalose is the preferred choice of lyo-protectant in order to maintain a mono-modal particle size distribution. In addition, antimicrobial activity of AP114-containing formulations was found to be highest for the formulation containing trehalose. The release kinetics of AP114 from the nanoparticles was strongly affected by the dimensions of the hexagonal phase. Larger dimension of the hexagonal phase, significantly improved the release of AP114 and antimicrobial activity of the formulation.

Keywords
Antimicrobial peptide, AP114, Cubosome, Freeze-drying, Glycerol monooleate, Hexosome, Liquid crystal, Plectasin, Drying, Dynamic light scattering, Glycerol, High resolution transmission electron microscopy, Hydration, Liquid crystals, Low temperature drying, Microorganisms, Nanoparticles, Particle size, Particle size analysis, Peptides, Powders, Size distribution, Targeted drug delivery, Transmission electron microscopy, X ray scattering, Cubosomes, Freeze drying, Controlled drug delivery, ap 114, disaccharide, lactose, nanoparticle, polypeptide antibiotic agent, sucrose, trehalose, unclassified drug, Article, bactericidal activity, drug delivery system, drug formulation, drug release, in vitro study, kinetics, molecular stability, nonhuman, phase transition, photon correlation spectroscopy, powder, priority journal, X ray crystallography
National Category
Natural Sciences
Identifiers
urn:nbn:se:ri:diva-34070 (URN)10.1016/j.jcis.2018.03.062 (DOI)2-s2.0-85044472786 (Scopus ID)
Available from: 2018-07-06 Created: 2018-07-06 Last updated: 2018-08-15Bibliographically approved
Andersson, I. M., Glantz, M., Alexander, M., Millqvist-Fureby, A., Paulsson, M. & Bergenståhl, B. (2018). Impact of surface properties on morphology of spray-dried milk serum protein/lactose systems. International Dairy Journal, 85, 86-95
Open this publication in new window or tab >>Impact of surface properties on morphology of spray-dried milk serum protein/lactose systems
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2018 (English)In: International Dairy Journal, ISSN 0958-6946, E-ISSN 1879-0143, Vol. 85, p. 86-95Article in journal (Refereed) Published
Abstract [en]

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.

Keywords
Body fluids, Morphology, Proteins, Spray drying, Milk serum proteins, Molecular diffusion, Particle morphologies, Particle surface, Protein concentrations, Protein surface, Spray dryers, Surface pressures, Surface properties
National Category
Natural Sciences
Identifiers
urn:nbn:se:ri:diva-34363 (URN)10.1016/j.idairyj.2018.04.011 (DOI)2-s2.0-85048984978 (Scopus ID)
Note

Funding details: Lunds Universitet;

Available from: 2018-08-07 Created: 2018-08-07 Last updated: 2018-08-15Bibliographically approved
Badal Tejedor, M., Pazesh, S., Nordgren, N., Schuleit, M., Rutland, M. W., Alderborn, G. & Millqvist-Fureby, A. (2018). Milling induced amorphisation and recrystallization of α-lactose monohydrate. International Journal of Pharmaceutics, 537(1-2), 140-147
Open this publication in new window or tab >>Milling induced amorphisation and recrystallization of α-lactose monohydrate
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2018 (English)In: International Journal of Pharmaceutics, ISSN 0378-5173, E-ISSN 1873-3476, Vol. 537, no 1-2, p. 140-147Article in journal (Refereed) Published
Abstract [en]

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.

Keywords
Amorphisation, Atomic force microscopy, Differential scanning calorimetry, Lactose, Mechanical properties, Milling, Recrystallization, Tableting, TGA, alpha lactose, Article, conformation, crystallization, energy, glass transition temperature, morphology, particle size, powder, priority journal, scanning electron microscopy, spray drying, surface property, thermogravimetry
National Category
Natural Sciences
Identifiers
urn:nbn:se:ri:diva-33233 (URN)10.1016/j.ijpharm.2017.12.021 (DOI)2-s2.0-85038844261 (Scopus ID)
Available from: 2018-02-13 Created: 2018-02-13 Last updated: 2019-07-02Bibliographically approved
Both, E. M., Nuzzo, M., Millqvist-Fureby, A., Boom, R. M. & Schutyser, M. A. (2018). Morphology development during single droplet drying of mixed component formulations and milk. Food Research International, 109, 448-454, Article ID S0963-9969(18)30328-4.
Open this publication in new window or tab >>Morphology development during single droplet drying of mixed component formulations and milk
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2018 (English)In: Food Research International, ISSN 0963-9969, E-ISSN 1873-7145, Vol. 109, p. 448-454, article id S0963-9969(18)30328-4Article in journal (Refereed) Published
Abstract [en]

We report on the influence of selected components and their mixtures on the development of the morphology during drying of single droplets and extend the results to the morphology of whole milk powder particles. Sessile single droplet drying and acoustic levitation methods were employed to study single droplet drying. The influence of carbohydrates (lactose and maltodextrin DE12) and proteins (micellar casein or whey protein) on morphology development is very different, since upon concentration protein systems will jam and undergo a colloidal glass transition, whereas carbohydrate systems will gradually increase in viscosity as a consequence of the concentration. Whey protein gives relatively rigid shells due to jamming of the "hard sphere" proteins, while casein micelles behave as "soft spheres" that can deform after jamming, which gives flexibility to the shell during drying. The influence of the carbohydrates on the final morphology was found much larger than the influence of the proteins. Caseins influenced morphology only in mixtures with lactose at higher concentrations due to its high voluminosity. Similar observations were done for whole milk, where fat appeared to have no influence. With maltodextrin the influence of the casein was again observed in the shape and smoothness of wrinkles. Both sessile and levitated droplet drying methods provide a similar and consistent view on morphology development.

Keywords
Confocal Raman microscopy, Maltodextrin, Milk, Morphology, Single droplet drying
National Category
Natural Sciences
Identifiers
urn:nbn:se:ri:diva-33915 (URN)10.1016/j.foodres.2018.04.043 (DOI)29803471 (PubMedID)2-s2.0-85046446321 (Scopus ID)
Available from: 2018-06-07 Created: 2018-06-07 Last updated: 2019-01-10Bibliographically approved
Badal Tejedor, M., Nordgren, N., Schuleit, M., Millqvist-Fureby, A. & Rutland, M. W. (2017). AFM Colloidal Probe Measurements Implicate Capillary Condensation in Punch-Particle Surface Interactions during Tableting. Langmuir, 33(46), 13180-13188
Open this publication in new window or tab >>AFM Colloidal Probe Measurements Implicate Capillary Condensation in Punch-Particle Surface Interactions during Tableting
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2017 (English)In: Langmuir, ISSN 0743-7463, E-ISSN 1520-5827, Vol. 33, no 46, p. 13180-13188Article in journal (Refereed) Published
Abstract [en]

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.

Keywords
Atomic force microscopy, Cellulose, Characterization, Condensation, Floods, Hydrophilicity, Probes, Sugars, Van der Waals forces, Adhesive interaction, Alpha lactose monohydrate, Capillary condensation, Condensation kinetics, Hydrophilic surfaces, Manufacturing process, Micro-crystalline cellulose, Surface characterization, Drug products
National Category
Natural Sciences
Identifiers
urn:nbn:se:ri:diva-33146 (URN)10.1021/acs.langmuir.7b02189 (DOI)2-s2.0-85034836128 (Scopus ID)
Available from: 2018-01-31 Created: 2018-01-31 Last updated: 2018-08-17Bibliographically approved
Badal Tejedor, M., Nordgren, N., Schuleit, M., Pazesh, S., Alderborn, G., Millqvist-Fureby, A. & Rutland, M. W. (2017). Determination of interfacial amorphicity in functional powders. Langmuir, 33(4), 920-926
Open this publication in new window or tab >>Determination of interfacial amorphicity in functional powders
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2017 (English)In: Langmuir, ISSN 0743-7463, E-ISSN 1520-5827, Vol. 33, no 4, p. 920-926Article in journal (Refereed) Published
Abstract [en]

The nature of the surfaces of particles of pharmaceutical ingredients, food powders, and polymers is a determining factor for their performance in for example tableting, powder handling, or mixing. Changes on the surface structure of the material will impact the flow properties, dissolution rate, and tabletability of the powder blend. For crystalline materials, surface amorphization is a phenomenon which is known to impact performance. Since it is important to measure and control the level of amorphicity, several characterization techniques are available to determine the bulk amorphous content of a processed material. The possibility of characterizing the degree of amorphicity at the surface, for example by studying the mechanical properties of the particles' surface at the nanoscale, is currently only offered by atomic force microscopy (AFM). The AFM PeakForce QNM technique has been used to measure the variation in energy dissipation (eV) at the surface of the particles which sheds light on the mechanical changes occurring as a result of amorphization or recrystallization events. Two novel approaches for the characterization of amorphicity are presented here. First, since particles are heterogeneous, we present a methodology to present the results of extensive QNM analysis of multiple particles in a coherent and easily interpreted manner, by studying cumulative distributions of dissipation data with respect to a threshold value which can be used to distinguish the crystalline and amorphous states. To exemplify the approach, which is generally applicable to any material, reference materials of purely crystalline α-lactose monohydrate and completely amorphous spray dried lactose particles were compared to a partially amorphized α-lactose monohydrate sample. Dissipation data are compared to evaluations of the lactose samples with conventional AFM and SEM showing significant topographical differences. Finally, the recrystallization of the surface amorphous regions in response to humidity was followed by studying the dissipation response of a well-defined surface region over time, which confirms both that dissipation measurement is a useful measure of surface amorphicity and that significant recrystallization occurs at the surface in response to humidity.

National Category
Chemical Sciences
Identifiers
urn:nbn:se:ri:diva-28201 (URN)10.1021/acs.langmuir.6b03969 (DOI)2-s2.0-85011117083 (Scopus ID)
Available from: 2017-04-03 Created: 2017-04-03 Last updated: 2018-08-17Bibliographically approved
Nuzzo, M., Sloth Overgaard, J., Bergenståhl, B. & Millqvist-Fureby, A. (2017). The morphology and internal composition of dried particles from whole milk—From single droplet to full scale drying. Food Structure, 13, 35-44
Open this publication in new window or tab >>The morphology and internal composition of dried particles from whole milk—From single droplet to full scale drying
2017 (English)In: Food Structure, ISSN 2213-3291, Vol. 13, p. 35-44Article in journal (Refereed) Published
Abstract [en]

Powder structure and functionality are expected to be closely linked to the composition and drying process. In order to understand the optimization of the quality of a powder, e.g. encapsulation efficiency, or wetting and dispersion properties, monitoring of the particle microstructure is an attractive concept. However, to study the impact of different parameters in formulation and drying process on full scale is complicated and expensive, hence, studies on smaller scale, even single particle drying, is a potentially useful complement, as long as the results are comparable. The aim of this study is to compare morphology and internal composition of whole milk particles produced at different dryer scales to assess the development of internal structure in powder formed by spray drying. Whole milk was spray dried in the single particle dryer, laboratory dryer, pilot plant dryer and full scale dryer. The morphology and composition of the particles obtained were analyzed by low vacuum-SEM, confocal Raman microscopy and X-ray photoelectron spectroscopy. Phenomena such as adsorption of surface active compounds at the particle surface and phase segregation are observed to different extent, depending on particle size and drying time. The scale of drying influences the internal microstructure and distribution of components in the particles, and to a small extent also the external morphology. These effects are proposed to be related to the drying times for different droplet sizes, although mechanical handling effects and agglomeration in the full scale dryer may also influence the final morphology of these particles, as well as the surface composition.

Keywords
Confocal Raman microscopy, Morphology, Scale-up, Spray drying, Surface Composition, Whole milk powder
National Category
Natural Sciences
Identifiers
urn:nbn:se:ri:diva-33165 (URN)10.1016/j.foostr.2017.02.001 (DOI)2-s2.0-85015260861 (Scopus ID)
Available from: 2018-01-23 Created: 2018-01-23 Last updated: 2019-01-22Bibliographically approved
Munoz-Ibanez, M., Nuzzo, M., Turchiuli, C., Bergenståhl, B., Dumoulin, E. & Millqvist-Fureby, A. (2016). The microstructure and component distribution in spray-dried emulsion particles. Food Structure, 8, 16-24
Open this publication in new window or tab >>The microstructure and component distribution in spray-dried emulsion particles
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2016 (English)In: Food Structure, ISSN 2213-3291, Vol. 8, p. 16-24Article in journal (Refereed) Published
Abstract [en]

Microencapsulation by spray drying of oil-in-water (o/w) emulsions provides a means to encapsulate functional lipophilic ingredients. The active ingredient is dispersed in continuous solid phase providing protection. However, the encapsulation efficiency depends on the microstructure and morphology of the dry particles influenced by several mechanisms occurring during processing such as oil droplet breakup during atomization, ingredient diffusivity, interfacial adsorption of surface active ingredients, and drying kinetics. In this work, sunflower oil (model for lipophilic compounds) was encapsulated in solid particles composed of acacia gum and maltodextrin DE12. Three powders with different initial emulsion size (e.g. about 0.1 and 1 μm) and atomized under high and low shear rate were analysed for the morphology and distribution of oil droplets and matrix constituents within the solid particle (20–100 μm). The microscopic (optical, SEM, LVSEM, confocal Raman), spectroscopic (XPS) and analytical (solvent extraction) techniques used were either qualitative or quantitative. Their combination made it possible to determine both the composition at the surface and inside the particle. The surface differs from the bulk in composition, confirming the constituent segregation during spray drying, and depended on the initial emulsion size and atomization conditions that must be controlled for an efficient encapsulation. Especially, the use of confocal Raman microscopy is promising for the study of processstructure-properties relationship.

Keywords
Confocal raman microscopy, Particle microstructure, Phase segregation, Spray-dried emulsions
National Category
Natural Sciences
Identifiers
urn:nbn:se:ri:diva-27673 (URN)10.1016/j.foostr.2016.05.001 (DOI)2-s2.0-84979583979 (Scopus ID)
Available from: 2016-12-22 Created: 2016-12-21 Last updated: 2019-06-19Bibliographically approved
Nuzzo, M., Sloth, J., Brandner, B., Bergenstahl, B. & Millqvist-Fureby, A. (2015). Confocal Raman microscopy for mapping phase segregation in individually dried particles composed of lactose and macromolecules (ed.). Colloids and Surfaces A: Physicochemical and Engineering Aspects, 481, 229-236
Open this publication in new window or tab >>Confocal Raman microscopy for mapping phase segregation in individually dried particles composed of lactose and macromolecules
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2015 (English)In: Colloids and Surfaces A: Physicochemical and Engineering Aspects, ISSN 0927-7757, E-ISSN 1873-4359, Vol. 481, p. 229-236Article in journal (Refereed) Published
Abstract [en]

The quality of powder is determined by its functionality such as dissolution, encapsulation and flowability. The functionality of powder is in turn determined by their primary properties such as morphology and composition which need to be studied. Hence morphology and surface composition has been largely investigated in spray dried powders and individually dried particles. On the contrary, there is only scarce information regarding the internal structure. With the aim of acquiring a better understanding of the localization of different ingredients in spray dried powders we have used confocal Raman microscopy to investigate the internal microstructure of individually dried particles. In this study three different macromolecules have been investigated: bovine serum albumin, hydroxypropyl methyl cellulose, and triblock co-polymer poloxamer in a lactose matrix are compared at various macromolecule to lactose ratios. The surface and internal component distribution in response to the macromolecule concentration has been established. For the first time phase segregation in particles during a short drying time range is shown. Macromolecules were enriched at the surface of the dried particles and a macromolecule depleted layer was observed below the surface. Macromolecule enriched domains were found segregated from the amorphous lactose matrix in the internal part of the particles. Confocal Raman microscopy was found to be a powerful tool for internal mapping in individually dried particles.

Keywords
Composition, Confocal raman microscopy, Individually dried particles, Mapping, Phase segregation, Confocal Raman microscopy for mapping phase segregation in individually dried particles composed of lactose and macromolecules
National Category
Natural Sciences
Identifiers
urn:nbn:se:ri:diva-26379 (URN)10.1016/j.colsurfa.2015.04.044 (DOI)
Note

A3500

Available from: 2016-12-08 Created: 2016-12-08 Last updated: 2019-07-02Bibliographically approved
Identifiers
ORCID iD: ORCID iD iconorcid.org/0000-0001-9891-8968

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