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  • 1. Bannow, J.
    et al.
    Benjamins, J. -W
    Wohlert, Jakob
    KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology. KTH, School of Chemical Science and Engineering (CHE), Centres, Wallenberg Wood Science Center.
    Löbmann, K.
    Svagan, Anna J.
    KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology. KTH, School of Chemical Science and Engineering (CHE), Centres, Wallenberg Wood Science Center.
    Solid nanofoams based on cellulose nanofibers and indomethacin—the effect of processing parameters and drug content on material structure2017In: International Journal of Pharmaceutics, ISSN 0378-5173, E-ISSN 1873-3476, Vol. 526, no 1-2, p. 291-299Article in journal (Refereed)
    Abstract [en]

    The unique colloidal properties of cellulose nanofibers (CNF), makes CNF a very interesting new excipient in pharmaceutical formulations, as CNF in combination with some poorly-soluble drugs can create nanofoams with closed cells. Previous nanofoams, created with the model drug indomethacin, demonstrated a prolonged release compared to films, owing to the tortuous diffusion path that the drug needs to take around the intact air-bubbles. However, the nanofoam was only obtained at a relatively low drug content of 21 wt% using fixed processing parameters. Herein, the effect of indomethacin content and processing parameters on the foaming properties was analysed. Results demonstrate that a certain amount of dissolved drug is needed to stabilize air-bubbles. At the same time, larger fractions of dissolved drug promote coarsening/collapse of the wet foam. The pendant drop/bubble profile tensiometry was used to verify the wet-foam stability at different pHs. The pH influenced the amount of solubilized drug and the processing-window was very narrow at high drug loadings. The results were compared to real foaming-experiments and solid state analysis of the final cellular solids. The parameters were assembled into a processing chart, highlighting the importance of the right combination of processing parameters (pH and time-point of pH adjustment) in order to successfully prepare cellular solid materials with up to 46 wt% drug loading.

  • 2. Lobmann, Korbinian
    et al.
    Svagan, Anna J.
    KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology.
    Cellulose nanofibers as excipient for the delivery of poorly soluble drugs2017In: International Journal of Pharmaceutics, ISSN 0378-5173, E-ISSN 1873-3476, Vol. 533, no 1, p. 285-297Article in journal (Refereed)
    Abstract [en]

    Poor aqueous solubility of drugs is becoming an increasingly pronounced challenge in the formulation and development of drug delivery systems. To overcome the limitations associated with these problematic drugs, formulation scientists are required to use enabling strategies which often demands the use of new excipients. Cellulose nanofibers (CNFs) is such an excipient and it has only recently been described in the pharmaceutical field. In this review, the use of CNF in drug formulation with a focus on poorly soluble drugs is featured. In particular, the aim is to describe and discuss the many unique properties of CNFs, which make CNFs attractive as excipients in pharmaceutical sciences. Furthermore, the use of CNF as stabilizers for crystalline drug nanoparticles, as a matrix former to obtain a long-lasting sustained drug release over several weeks and as a film former with immediate release properties for poorly soluble drug are reported. Finally, the preparation of pharmaceutical CNF foams together with poorly soluble drugs is highlighted; foams, which offer a sustained drug delivery system with positive buoyancy.

  • 3. Lombardo, S.
    et al.
    Chen, Pan
    KTH, School of Engineering Sciences in Chemistry, Biotechnology and Health (CBH), Centres, Wallenberg Wood Science Center.
    Larsson, Per A.
    KTH, School of Engineering Sciences in Chemistry, Biotechnology and Health (CBH), Fibre- and Polymer Technology.
    Thielemans, W.
    Wohlert, Jakob
    KTH, School of Engineering Sciences in Chemistry, Biotechnology and Health (CBH), Fibre- and Polymer Technology.
    Svagan, Anna J.
    KTH, School of Engineering Sciences in Chemistry, Biotechnology and Health (CBH), Fibre- and Polymer Technology. KTH, School of Engineering Sciences in Chemistry, Biotechnology and Health (CBH), Centres, Wallenberg Wood Science Center.
    Toward Improved Understanding of the Interactions between Poorly Soluble Drugs and Cellulose Nanofibers2018In: Langmuir, ISSN 0743-7463, E-ISSN 1520-5827, Vol. 34, no 19, p. 5464-5473Article in journal (Refereed)
    Abstract [en]

    Cellulose nanofibers (CNFs) have interesting physicochemical and colloidal properties that have been recently exploited in novel drug-delivery systems for tailored release of poorly soluble drugs. The morphology and release kinetics of such drug-delivery systems heavily relied on the drug-CNF interactions; however, in-depth understanding of the interactions was lacking. Herein, the interactions between a poorly soluble model drug molecule, furosemide, and cationic cellulose nanofibers with two different degrees of substitution are studied by sorption experiments, Fourier transform infrared spectroscopy, and molecular dynamics (MD) simulation. Both MD simulations and experimental results confirmed the spontaneous sorption of drug onto CNF. Simulations further showed that adsorption occurred by the flat aryl ring of furosemide. The spontaneous sorption was commensurate with large entropy gains as a result of release of surface-bound water. Association between furosemide molecules furthermore enabled surface precipitation as indicated by both simulations and experiments. Finally, sorption was also found not to be driven by charge neutralization, between positive CNF surface charges and the furosemide negative charge, so that surface area is the single most important parameter determining the amount of sorbed drug. An optimized CNF-furosemide drug-delivery vehicle thus needs to have a maximized specific surface area irrespective of the surface charge with which it is achieved. The findings also provide important insights into the design principles of CNF-based filters suitable for removal of poorly soluble drugs from wastewater.

  • 4.
    Svagan, Anna
    KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology, Biocomposites.
    Bio-inspired cellulose nanocomposites and foams based on starch matrix2008Doctoral thesis, comprehensive summary (Other scientific)
    Abstract [en]

    In 2007 the production of expanded polystyrene (EPS) in the world was over 4 million tonnes and is expected to grow at 6 percent per year. With the increased concern about environmental protection, alternative biodegradable materials from renewable resources are of interest. The present doctoral thesis work successfully demonstrates that starch-based foams with mechanical properties similar to EPS can be obtained by reinforcing the cell-walls in the foams with cellulose nanofibers (MFC).

    High cellulose nanofiber content nanocomposites with a highly plasticized (50/50) glycerol-amylopectin starch matrix are successfully prepared by solvent-casting due to the high compatibility between starch and MFC. At 70 wt% MFC, the nanocomposites show a remarkable combination of high tensile strength, modulus and strain to failure, and consequently very high work to fracture. The interesting combination of properties are due to good dispersion of nanofibers, the MFC network, nanofiber and matrix properties and favorable nanofiber-matrix interaction.

    The moisture sorption kinetics (30% RH) in glycerol plasticized and pure amylopectin film reinforced with cellulose nanofibers must be modeled using a moisture concentration-dependent diffusivity in most cases. The presence of cellulose nanofibers has a strong reducing effect on the moisture diffusivity. The decrease in zero-concentration diffusivity with increasing nanofiber content could be due to geometrical impedance, strong starch-MFC molecular interaction and constrained swelling due to the cellulose nanofiber network present.

    Novel biomimetic starch-based nanocomposite foams with MFC contents up to 40 wt% are successfully prepared by freeze-drying. The hierarchically structured nanocomposite foams show significant increase in mechanical properties in compression compared to neat starch foam. Still, better control of the cell structure could further improve the mechanical properties. The effect of cell wall composition, freeze-drying temperature and freezing temperature on the resulting cell structure are therefore investigated. The freeze-drying temperature is critical in order to avoid cell structure collapse. By changing the starch content, the cell size, anisotropy ratio and ratio between open and closed cells can be altered. A decrease in freezing temperature decreases the cell size and increases the anisotropy ratio.

    Finally, mechanical properties obtained in compression for a 30 wt% MFC foam prepared by freeze-drying demonstrates comparable properties (Young's modulus and yield strength) to expanded polystyrene at 50% RH and similar relative density. This is due to the reinforcing cellulose nanofiber network within the cell walls.

  • 5.
    Svagan, Anna
    KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology.
    Bio-inspired polysaccharide nanocomposites and foams2007Licentiate thesis, comprehensive summary (Other scientific)
    Abstract [en]

    Today, the majority of materials used for single-use packaging are petroleum-based synthetic polymers. With increased concern about the environmental protection, efforts have been made to develop alternative biodegradable materials from renewable resources. Starch offers an attractive alternative since it is of low cost and abundant. However, the starch material is brittle without plasticizer and the mechanical properties of starch materials are highly sensitive to moisture.

    In nature, the plant cell walls combine mechanical stiffness, strength and toughness despite a highly hydrated state. This interesting combination of properties is attributed to a network based on cellulose microfibrils. Inspired by this, microfibrillated cellulose (MFC) reinforced starch-based nanocomposites films and foams were prepared. Films with a viscous matrix and MFC contents from 10 to 70wt% were successfully obtained by solvent casting. The films were characterized by DSC, DMA, FE-SEM, XRD, mercury density measurements, and dynamic water vapor sorption (DVS). At 70wt% MFC content a high tensile strength together with high modulus and high work of fracture was observed. This was due to the nanofiber and matrix properties, favourable nanofiber-matrix interaction, a good dispersion of nanofibers and the MFC network.

    Novel nanocomposite foams were obtained by freeze-drying aquagels prepared from 8wt% solutions of amylopectin starch and MFC. The MFC content was varied from 10 to 70wt%. For composite foam with MFC contents up to 40wt%, improved mechanical properties were observed in compression. The mechanical properties depended both on the cell wall properties and the cell-structure of the foam. The effect of moisture (20-80% RH) on the dynamical properties of composite foam with 40wt% MFC was also investigated and compared to those of neat starch foam. Improved storage modulus was noted with MFC content, which was a result of the nanofiber network in the cell-wall. In addition, the moisture content decreased with MFC content, due to the less hydrophilic nature of MFC.

  • 6.
    Svagan, Anna
    et al.
    KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology, Biocomposites.
    Azizi Samir, My A. S.
    KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology, Biocomposites.
    Berglund, Lars A.
    KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology, Biocomposites.
    Biomimetic Foams of High Mechanical Performance Based on Nanostructured Cell Walls Reinforced by Native Cellulose Nanofibrils2008In: Advanced Materials, ISSN 0935-9648, E-ISSN 1521-4095, Vol. 20, no 7, p. 1263-1269Article in journal (Refereed)
    Abstract [en]

     A bioinspired foam in which cellulose nanofibrils are used to reinforce cell walls (ca. 3 mu m) is presented. The nanocomposite foams are prepared by a lyophilization technique and show composite structure at the cell-wall scale. The nanocellulosic network shows remarkable mechanical performance, expressed in much-improved modulus and yield strength compared with the neat starch foam.

  • 7.
    Svagan, Anna
    et al.
    KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology.
    Azizi Samir, My Ahmed Said
    KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology.
    Berglund, Lars
    KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology.
    Biomimetic polysaccharide nanocomposites of high cellulose content and high toughness2007In: Biomacromolecules, ISSN 1525-7797, E-ISSN 1526-4602, Vol. 8, no 8, p. 2556-2563Article in journal (Refereed)
    Abstract [en]

    Plant cell walls combine mechanical stiffness, strength and toughness despite a highly hydrated state. Inspired by this, a nanostructured cellulose network is combined with an almost viscous polysaccharide matrix in the form of a 50/50 amylopectin-glycerol blend. Homogeneous films with a microfibrillated cellulose (MFC) nanofiber content in the range of 10-70 wt % are successfully cast. Characterization is carried out by dynamic mechanical analysis, field-emission scanning electron microscopy, X-ray diffraction, and mercury density measurements. The MFC is well dispersed and predominantly oriented random-in-the-plane. High tensile strength is combined with high modulus and very high work of fracture in the nanocomposite with 70 wt % WC. The reasons for this interesting combination of properties include nanofiber and matrix properties, favorable nanofiber-matrix interaction, good dispersion, and the ability of the MFC network to maintain its integrity to a strain of at least 8%.

  • 8.
    Svagan, Anna
    et al.
    KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology.
    Azizi Samir, My
    KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology.
    Berglund, Lars
    KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology.
    Nanocomposite cellulose-starch foams prepared by lyophilizationManuscript (Other academic)
  • 9.
    Svagan, Anna
    et al.
    KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology, Biocomposites.
    Berglund, Lars A.
    KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology, Biocomposites.
    Jensen, Poul
    A cellulose nanocomposite biopolymer foam competing with expanded polystyrene (EPS): hierarchical structure effects on energy absorptionManuscript (Other academic)
    Abstract [en]

    Starch is an interesting biofoam candidate as replacement of expanded polystyrene (EPS) in packaging materials. The main technical problems with starch foam include its hygroscopic nature, sensitivity of its mechanical properties to moisture content and much lower energy  absorption than EPS. In the present study, a starch-based biofoam is able to reach comparable mechanical properties (Young’s modulus, compression yield strength) to expanded polystyrene at 50% relative humidity. The reason is the cellulose nanocomposite concept in the form of a cellulose nanofiber network reinforcing the hygroscopic amylopectin matrix in the cell wall. The biofoams are prepared by freeze-drying and subjected to compressive loading. Cell structure is characterized by FE-SEM of cross-sections. Mechanical properties are related to cell structure and cell wall nanocomposite composition. Hierarchically structured biofoams are demonstrated to be interesting materials with potential for strongly improved mechanical properties. The present study also highlights the challenges involved in preparation and analysis of nanocomposite foams structured at several different scales.

  • 10.
    Svagan, Anna
    et al.
    KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology, Biocomposites.
    Hedenqvist, Mikael
    KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology.
    Berglund, Lars A.
    KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology, Biocomposites.
    Reduced water vapour sorption in cellulose nanocomposites with starch matrix2009In: Composites Science And Technology, ISSN 0266-3538, E-ISSN 1879-1050, Vol. 69, no 3-4, p. 500-506Article in journal (Refereed)
    Abstract [en]

    The effects of microfibrillated cellulose nanofibers from wood on the moisture sorption kinetics (30% RH) of glycerol plasticized and pure high-amylopectin starch films were studied. The presence of a nanofiber network (70 wt% cellulose nanofibers) reduced the moisture uptake to half the value of the pure plasticized starch film. The swelling yielded a moisture concentration-dependent diffusivity. Quite surprisingly, the moisture diffusivity decreased rapidly with increasing nanofiber content and the diffusivity of the neat cellulose network was, in relative terms, very low. It was possible to describe the strong decrease in zero-concentration diffusivity with increasing cellulose nanofiber/matrix ratio, simply by assuming only geometrical blocking using the model due to Aris. The adjusted model parameters suggested a "simplified" composite structure with dense nanofiber layers oriented in the plane of the film. Still, also constraining effects on swelling from the high modulus/hydrogen bonding cellulose network and reduced amylopectin molecular mobility due to strong starch-cellulose molecular interactions were suggested to contribute to the reductions in moisture diffusivity.

  • 11.
    Svagan, Anna J.
    et al.
    KTH, School of Chemical Science and Engineering (CHE), Centres, Wallenberg Wood Science Center. University of Copenhagen, Denmark.
    Benjamins, Jan-Willem
    Al-Ansari, Zeinab
    Bar Shalom, Daniel
    Mullertz, Anette
    Wågberg, Lars
    KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology. KTH, School of Chemical Science and Engineering (CHE), Centres, Wallenberg Wood Science Center.
    Lobmann, Korbinian
    Solid cellulose nanofiber based foams - Towards facile design of sustained drug delivery systems2016In: Journal of Controlled Release, ISSN 0168-3659, E-ISSN 1873-4995, Vol. 244, p. 74-82Article in journal (Refereed)
    Abstract [en]

    Control of drug action through formulation is a vital and very challenging topic within pharmaceutical sciences. Cellulose nanofibers (CNF) are an excipient candidate in pharmaceutical formulations that could be used to easily optimize drug delivery rates. CNF has interesting physico-chemical properties that, when combined with surfactants, can be used to create very stable air bubbles and dry foams. Utilizing this inherent property, it is possible to modify the release kinetics of the model drug riboflavin in a facile way. Wet foams were prepared using cationic CNF and a pharmaceutically acceptable surfactant (lauric acid sodium salt). The drug was suspended in the wetstable foams followed by a drying step to obtain dry foams. Flexible cellular solid materials of different thicknesses, shapes and drug loadings (up to 50 wt%) could successfully be prepared. The drug was released from the solid foams in a diffusion-controlled, sustained manner due to the presence of intact air bubbles which imparted a tortuous diffusion path. The diffusion coefficient was assessed using Franz cells and shown to be more than one order of magnitude smaller for the cellular solids compared to the bubble-free films in the wet state. By changing the dimensions of dry foams while keeping drug load and total weight constant, the drug release kinetics could be modified, e.g. a rectangular box-shaped foam of 8 mm thickness released only 59% of the drug after 24 h whereas a thinner foam sample (0.6 mm) released 78% of its drug content within 8 h. In comparison, the drug release from films (0.009 mm, with the same total mass and an outer surface area comparable to the thinner foam) was much faster, amounting to 72% of the drug within 1 h. The entrapped air bubbles in the foam also induced positive buoyancy, which is interesting from the perspective of gastroretentive drug-delivery.

  • 12.
    Svagan, Anna J.
    et al.
    KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology. KTH, School of Chemical Science and Engineering (CHE), Centres, Wallenberg Wood Science Center.
    Berglund, Lars A.
    KTH, School of Chemical Science and Engineering (CHE), Centres, Wallenberg Wood Science Center. KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology.
    Jensen, Poul
    Cellulose Nanocomposite Biopolymer Foam-Hierarchical Structure Effects on Energy Absorption2011In: ACS APPLIED MATERIALS & INTERFACES, ISSN 1944-8244, Vol. 3, no 5, p. 1411-1417Article in journal (Refereed)
    Abstract [en]

    Starch is an attractive biofoam candidate as replacement of expanded polystyrene (EPS) in packaging materials. The main technical problems with starch foam include its hygroscopic nature, sensitivity of its mechanical properties to moisture content, and much lower energy absorption than EPS. In the present study, a starch-based biofoam is for the first time able to reach comparable mechanical properties (E = 32 MPa, compressive yield strength, 630 kPa) to EPS at 50% relative humidity and similar relative density. The reason is the nanocomposite concept concept in the form of a cellulose nanofiber network reinforcing the hygroscopic amylopectin starch matrix in the cell wall. The biofoams are prepared by the freezing/freeze-drying technique and subjected to compressive loading. Cell structure is characterized by FE-SEM of cross sections. Mechanical properties are related to cell structure and cell wall nanocomposite composition. Hierarchically structured biofoams are demonstrated to be interesting materials with potential for strongly improved mechanical properties.

  • 13.
    Svagan, Anna
    et al.
    KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology, Biocomposites.
    Jensen, Poul
    Berglund, Lars A.
    KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology, Biocomposites.
    Furó, István
    KTH, School of Chemical Science and Engineering (CHE), Chemistry, Physical Chemistry.
    Dvinskikh, Sergey
    KTH, School of Chemical Science and Engineering (CHE), Chemistry, Physical Chemistry.
    Towards tailored hierarchical structures in starch-based cellulose nanocomposite foams prepared by freeze-dryingManuscript (Other academic)
    Abstract [en]

    The properties of nanocomposite foams depend both on cell wall composition and cell structure. In order to fully realize the potential of these materials, both cell wall composition and cell structure must be controlled and tailored. The effect of freezing and freeze-drying temperature on cell structure in nanocomposite foams based on starch and microfibrillated cellulose (MFC) is studied. Freezing experiments are combined with DSC and NMR-analysis of bound water content in order to determine a suitable freeze-drying temperature. The freeze-drying temperature is critical in order to avoid cell structure collapse, as found from cell structure studies by FE-SEM microscopy. Based on this, a foam with mixed open and closed cell structures and as much as 70% MFC in the cell wall was successfully prepared. The study clarifies the interdependence of how the starch-MFC-water suspension composition, in combination with freezing and freeze-drying temperature, will control cell structure of the foams.

  • 14.
    Svagan, Anna
    et al.
    KTH, School of Chemical Science and Engineering (CHE), Centres, Wallenberg Wood Science Center. KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology, Biocomposites.
    Jensen, Poul
    Natl Museum Denmark.
    Dvinskikh, Sergey
    KTH, School of Chemical Science and Engineering (CHE), Chemistry, Physical Chemistry.
    Furó, István
    KTH, School of Chemical Science and Engineering (CHE), Chemistry, Physical Chemistry.
    Berglund, Lars A.
    KTH, School of Chemical Science and Engineering (CHE), Centres, Wallenberg Wood Science Center. KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology, Biocomposites.
    Towards tailored hierarchical structures in cellulose nanocomposite biofoams prepared by freezing/freeze-drying2010In: Journal of Materials Chemistry, ISSN 0959-9428, E-ISSN 1364-5501, Vol. 20, no 32, p. 6646-6654Article in journal (Refereed)
    Abstract [en]

    Cellulose nanofiber (MFC) reinforced starch-based foams, prepared by the freezing/freeze-drying route, are very interesting porous materials due to the strong MFC reinforcement of the cell wall itself. However, in order to fully realize the potential of these nanocomposite biofoams, both cell wall composition and cell structure must be controlled. The effect of starch-MFC-water suspension composition, together with preparation temperature (-27, -78, and -196 degrees C) on the foam cell structure is investigated. NMR-analysis of bound water content, DSC and freezing experiments in combination with freeze-drying experiments and FE-SEM microscopy are used to determine a suitable freeze-drying temperature. The freeze-drying temperature is critical in order to avoid cell structure collapse, as found from FE-SEM studies. By varying the cell-wall composition and preparation temperature, the foam morphology can be manipulated. The connection between cell size and starch content is considered to depend on the inherent properties of starch and a mechanism for ice crystal formation is suggested. Based on improved preparation conditions, foams with mixed open and closed cell structures and as much as 70 wt% MFC in the cell wall are created successfully.

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