FinPowder: Wood hemicelluloses are effective wall materials for spray dried microencapsulation of bioactive compounds from bilberry with improved functional properties of produced microcapsules

Two years have passed since Abedalghani Halahlah (Abed) who is working as a doctoral researcher commenced in the FinPowder project (here) at the University of Helsinki (Abed, Figures a and b).  We are now back to deliver more interesting findings/outcomes to add to the previously revealed results (here) that have already been published as two impactful articles.

First article: Abedalghani Halahlah, Vieno Piironen, Kirsi S. Mikkonen, and Thao M. Ho. “Wood Hemicelluloses as Innovative Wall Materials for Spray-Dried Microencapsulation of Berry Juice: Part 1—Effect of Homogenization Techniques on their Feed Solution Properties.” Food and Bioprocess Technology 16, no. 4 (2023): 909-929.

Second article: Abedalghani Halahlah, Heikki Räikkönen, Vieno Piironen, Fabio Valoppi, Kirsi S. Mikkonen, and Thao M. Ho. “Wood hemicelluloses as sustainable wall materials to protect bioactive compounds during spray drying of bilberries.” Powder Technology 415 (2023): 118148.

In the first article we revealed that, magnetic stirring is the best choice for preparing wood hemicellulose (glucuronoxylans and galactoglucomannans) feed solutions for the spray-dried microencapsulation of bilberry juice. This is because microfluidization caused a loss of total anthocyanin content of the feed solutions. Furthermore, galactoglucomannans feed solutions formed a gel-like structure within a short time after ultrasonication and microfluidization, making these solutions unsuitable for spray-drying. Here also, we reported, for the first time, the formation of gel-like structures from a pressurized hot water extraction galactoglucomannans solution which was further investigated in a separate study (here). While in the second article, we demonstrated that wood-based hemicelluloses are efficient wall materials for the spray-dried microencapsulation of bilberry juice. The encapsulation efficiency values of wood-based hemicelluloses were relatively high and close to that of gum arabic (∼ 73%). Due to the natural presence of lignin-derived phenolic compounds in the structure of wood-based hemicelluloses, their microencapsulate powders had significantly higher phenolic content and antioxidant activities than gum arabic powders.

The findings of these two studies provide another value-added application of wood hemicelluloses obtained from waste and by products of the forest industry. Wood hemicelluloses can replace the currently used wall materials in the production of high-quality bilberry powders via a more cost-effective method (i.e., spray drying) than those currently used (freeze drying and freezing), thus offering an economic opportunity to bring bilberry products to global consumers. Alongside these financial gains, wood hemicelluloses also bring health benefits by adding dietary fibres and antioxidant functionality to the final products.

The experimental work was continued by further advancing the functional properties of produced microcapsules, for example by optimizing the ability of wood hemicelluloses to retain and protect bioactive compounds during spraying. In this regard, we carefully planned two models/approaches of experiments to obtain the best bioactive compounds retention and functional properties of the produced microcapsules. The first approach involved the use of carboxymethyl cellulose as a co-wall material combined with wood hemicelluloses to produce the microcapsules at fixed spray drying conditions. During this stage, we also used an advanced analytical technique (computed X-ray microtomography) in collaboration with Department of Chemistry at University of Helsinki to reveal interesting information regarding the internal and external structure and thickness of coating layer of the microcapsules (Figure-c) In the second approach we used wood hemicelluloses alone as wall materials but aimed to find the best processing conditions including inlet and outlet temperatures and the ratio between wood hemicellulose and bioactive compounds (Figure-d). The optimal microcapsules were further analyzed for their phenolic compounds profile including anthocyanins by Ultra-High-Performance Liquid Chromatography (Figure-e).

Luckily, we were able to improve the retention of the bioactive compounds in both approaches with very interesting observations and results that are currently under preparation for publication. The results provide valuable steps towards production of food powders and functional ingredients with high added nutritional values and functional properties with minimal cost.

The FinPowder project has received a third year of funding from the Finnish Natural Resources Research Foundation to conduct further investigations on microcapsule stability and digestibility. In the near future, the optimal microcapsules of wood hemicellulose will be studied for their storage stability over 6 months and in vitro digestion. More to come!

Figure: (a) Abed next to the Liquid Chromatography instrument and (b) conducting spray drying experiments (c) X-ray microtomography images exhibiting the internal and external structure, wall thickness and diameter, (d) The effect of spray drying conditions on the encapsulation efficiency, illustrated as three-dimensional plots and (e) Chromatogram shows 9 peaks of different anthocyanins compounds were found in the microcapsules.

iOLEO state of play: a synchrotron study of lipid carriers

Last December, four FoMSci group members travelled to Italy to work in the Elettra Sincrotrone Trieste facilities. This experiment is a part of the iOLEO project (three-year research grant), which aims to develop novel oleogels with tailorable digestibility, unlocking the potential of oleogels as a tool for fat replacement and bodyweight management.

MSc Tiago C. Pinto, who is working as a doctoral researcher for the iOLEO project, under the supervision of Docent Fabio Valoppi, carefully oversaw the planning of this intensive study. After months of painstakingly planning the work, the 48-hour experiment took place at the XRD1 beamline, with the intent of shedding light on the evolution of lipid crystals contained in engineered oleogel-based emulsions during simulated gastrointestinal digestion. This very ambitious experiment encompassed the in-situ analysis of 16 emulsion formulations with different lipid core materials and emulsifiers, each of them requiring at least 4 hours of simulated digestion. Time constraints were evident, and the complexity of the experiment required Tiago and Fabio to be joined by MSc Afsane Kazerani Garcia and BSc Christos Papadogiannakis. As they are both working on oleogel-related projects, their proficiency in the lab and familiarity with the topic was very valuable in making this experiment a fruitful one. Cooperation and teamwork were the factors that made this a successful venture, but the ability to keep calm even when things weren’t working in the researchers’ favour was key.

“Keeping the morale up while working two consecutive 20-hour shifts, with a small break of about 4 hours between them is not easy, especially when everything seemed to be stacked against us. After all the months of preparation and planning, having only 48 hours to accomplish everything that I intended brought a lot of pressure. Luckily, we were able to make it through and come out on the other side with very interesting observations. The dataset is still under processing, but we are confident that these are results that can provide a very valuable step towards revolutionising the field.”, Tiago said.

The results are being analysed with the collaboration of beamline scientist Dr. Luisa Barba, whose expertise and availability were essential during the planning and execution of the experiment. After the beam time, the team took a much-deserved day of rest with some exploring of the city of Trieste, as well as a short visit across the border to the historic port town of Koper, in Slovenia.

One of the most prevalent targets in the study of oleogels is their use as a replacement of fats from food chains, with one of the biggest hurdles being the achievement of similar macroscopic properties to replicate them. The characterisation of matter via X-rays can reveal structural differences at the molecular level that justify macroscopic properties and their variations. X-rays are an invaluable probe of the structure of matter, and the range of problems where X-rays have proved to be decisive in unravelling a material structure is very wide. In this case, understanding the evolution of lipid crystals (lipid crystal size, shape, and polymorphic form) will allow a better design of emulsions, leading to a tailored lipid digestion and release. This knowledge is of paramount importance when designing and developing engineered emulsions with tailorable digestibility. The synchrotron analysis offers the possibility to structurally characterise matter at many different levels, in a way that wouldn’t be possible using benchtop X-ray diffraction equipment. The level of detail that these results provide will play a pivotal role in understanding the structural response of simple differences in the composition of engineered emulsions.

Writing retreat in Tvärminne 19.-21.10.2022

The writing retreat has been an annual event, organized by the Food Materials Science Research Group since 2018, with the intent of setting aside the experimental work and shifting the focus to scientific writing activities. This year, we embarked on a journey to a different location and experienced three fruitful days at the Tvärminne zoological station of the University of Helsinki.

During our retreat in Tvärminne, a beautiful rural area in southern Finland, the members of our group, along with our group leader, Kirsi Mikkonen, got the chance to get together and be productive in a breathtaking place by the sea. We spent most of our time in the classroom, reserved for quiet working, which helped us productively engage in writing, some of us commencing new applications, others finishing old, nearly forgotten publications. Group meetings and fertile scientific discussions were held outside of the classroom. In addition to the hard-working time, everyone enjoyed the delicious meals and desserts during lunch and dinner. The group members sat together chatting, while admiring the amazing sea views. This gave us the opportunity to talk about each other’s work, and get to know new and old lab members better.

Following lunch, some chose to take a walk, enjoy the serene environment and admire wild berries and mushrooms. To reward ourselves after a long day of work, we indulged in going to the sauna and swimming in the cold waters, amongst some friendly jellyfish. After the sauna, we all got together to eat, play games and sing karaoke.

Overall, it was a unique experience, as we had the ability to work productively and share thoughts and ideas with our colleagues.

Creating More Sustainable Cosmetics with Spruce Gum and Birch Gum

The food and the cosmetics industries share some similarities – ingredients are a major one. This research will help both industries by providing them new information about candidate raw materials. Stabilizers, viscosity controlling agents, emulsifiers, to name a few – it’s possible to use the same innovative solutions to provide greener food and cosmetic ingredients. Spruce and birch gum are examples of new promising ingredients that could progress these industries.

A Bachelor of Beauty and Cosmetics (estenomi) student from Laurea University of Applied Sciences, Anne Parkkonen completed her thesis on the use of spruce and birch gum in cosmetics. It was a practical-oriented project and the goal was to plan, formulate and manufacture different kinds of cosmetic products by including spruce or birch gum as an ingredient. The thesis presents the legal regulations related to cosmetics. As previous research is mainly made for food ingredients, using wood gums for cosmetic purposes is a new idea. The thesis provides more detailed information about the legislation behind the use of ingredients/chemicals in cosmetic products.

The emulsion stabilizing features of spruce and birch gums lead Anne’s work to focus on exploring their effect on texture and composition when used in emulsion-based products (e.g. skin creams and serums). Additionally, evidence also indicates these gums have antioxidant, prebiotic, and anti-inflammatory properties. Some very promising findings from these experiments included how spruce and birch gum made a comfortable and pleasant film-like feel and appearance on the skin when the emulsions dried. Spruce and birch gum seemed to have moisture binding properties which are desirable features in many cosmetic products. These findings support the need for further studies on the use of wood gums in cosmetics.

This thesis project was completed under the guidance of Assoc. Prof. Kirsi Mikkonen and Dr. Satu Kirjoranta who study hemicelluloses (spruce and birch gum) and their potential applications. New avenues have been opened from their initial research, expanding into the field of cosmetics, with nine candidate spruce and birch gum-based products created. These products could inspire future research and collaborations with industry in Finland and further abroad to elucidate how to incorporate spruce and birch gum effectively in different applications.

Spruce and birch gum are ingredients from sustainable sources, manufactured using environmentally-friendly technology from wood. This thesis explores just one example of how many small solutions could make the world and its goods more sustainable within a circular economy. There is a need to replace existing ingredients with greener alternatives which are produced locally and from renewable sources. Spruce and birch gum are hopefully an example to support a better future for the cosmetics industry without compromising on product quality. Anne’s thesis will be released later this year. Petri Kilpeläinen from Natural Resources Institute Finland (Luke) is thanked for providing the spruce and birch gum samples for the study.

Unravelling the assembly mechanisms of emulsions: a new collaboration between FoMSci (University of Helsinki), BiCMat-Aalto and BiCMat-UBC groups (Aalto University and University of British Columbia)

We are pleased to announce the launching of a research collaboration between FoMSci (University of Helsinki) and Biobased Colloids and Materials operating both in Aalto University (BiCMat-Aalto) and University of British Columbia, Canada (BiCMat-UBC), led by Prof. Orlando Rojas. This collaboration is boosted by the joining of two postdoctoral researchers, Drs. Mamata Bhattarai and Emilie Ressouche working under the joint supervision of Profs. Rojas and Mikkonen. Mamata finished her PhD from FoMSci in November 2020, and Emilie comes from the Department of Applied Physics, in the Molecular Materials group, led by Prof. Olli Ikkala.

The research topics and the know-how available in both groups are complementary: FoMSci brings expertise in emulsions, hemicelluloses, and food applications.; BiCMat also works with multiphase systems based on lignocellulosic bio-colloids. Together, the groups will investigate the mechanisms responsible for the formation of emulsions stabilized by bio-based compounds such as lignin/hemicellulose complexes, and plant- as well as marine-derived bioresources.

This research project aligns with the goals of the BioElCell Research project, funded by Advanced ERC (2018-2023) in BiCMat, and will also bring an expansion to our Academy of Finland funded ENVISION project, leading to a wider comprehension of emulsions stabilized by wood hemicelluloses.

We nailed it again: four new funded projects to FoMSci

Between November and December 2020 our FoMSci group has received four new grants: three to Fabio Valoppi (iOLEO, ENGEL, and iFOOD), and one to Thao Minh Ho (FinPowder).

Fabio’s projects: The iOLEO and ENGEL projects, funded by the University of Helsinki three-year research grant scheme (7% success rate – only 9 projects were funded among 128 submitted) and the Jane and Aatos Erkko Foundation, respectively. These projects aim to develop new oleogels with body weight managing abilities unlocking the potential of oleogels as multi-functional fat substitutes. Mr. Tiago Pinto has been selected and hired as a new PhD student in the iOLEO project and will begin his work in April 2021. For the other project, ENGEL, we are currently in the process of hiring a postdoctoral researcher. The iFOOD project, funded by HELSUS, aims to develop a new digital tool to simulate mechanical properties of food products using finite element method simulation. This project is based on the existing and fruitful collaboration between FoMSci and the Electronics Research Laboratories (ETLA) also from the University of Helsinki.

Thao’s project: The FinPowder project, funded by the Finnish Natural Resources Research Foundation, aims to design powder particles to protect functional compounds of wild berry during spray drying. These coating materials originate from sustainable and natural sources that are extremely low in calories and cost, namely wood-based celluloses and hemicelluloses. Mr. Abedalghani Halahlah has been selected and hired as our new PhD student to work in the FinPowder project and will join the FoMSci group within a couple of months. Abedalghani will be co-supervised by Associate Professor Kirsi Mikkonen and Dr. Thao Minh Ho, in collaboration with Professor Vieno Piironen.

The cherry on the cake is that thanks to these new projects, our group will now be able to purchase a brand-new lab scale spray dryer!

Even though 2020 has been a tough year, we ended it in the best way possible with new funding, new people joining FoMSci, and new equipment. Writing proposals can be very energy demanding, but the doors that these new projects will open make it worth all the effort we put in during the writing process.

2021 has already started, and new and exciting times are waiting for us ahead!

PARTIFACE: Green route to wood-derived Janus particles for stabilized interfaces

We are extremely thrilled to start our new research project “PARTIFACE” since the beginning of June 2020, supported by the European Research Council and led by Assist. Prof. Kirsi S. Mikkonen. This project aims to develop a green conversion route using enzymatic crosslinking to build a novel concept, in which tailored bi-facial “Janus” particles will be prepared from two of the most abundant, but underexploited wood-based biopolymers: lignin and hemicelluloses.

Using environmentally friendly technology, this project will design sophisticated and sustainable hierarchical architectures from the abovementioned biopolymers. Due to their two ‘faces’ with opposite properties, these tailored wood-based particles are expected to have a superior capacity to stabilize emulsion interfaces.

Therefore, we envision a breakthrough in interface and colloid science, contributing to more sustainable use of the Earth’s resources.

Okay, this is remote work!

COVID-19 forced the FoMSci research group to work remotely.  We rapidly took use of versatile online tools and Kirsi started to host weekly group meetings. Staying home made us realize how important human interactions are in working life, and hence we also opened remote coffee breaks. A video call over a cup of morning coffee makes things seem more normal again. 

While we do not have access to laboratories, otherwise moving to remote working was an easy step. It also proves to be an incredibly efficient way to advance writing publications or planning new project proposals. FoMSci has been very productive already! 

Yet, we cannot deny how much we miss working in the laboratories and the hands on work.  

During regular working days, one can easily reach a daily goal of 10K steps of walking. In remote working, UniSport video exercises help us keep in shape, and many of us has given a try to various workouts. A daily routine of stretching and getting fresh air is good for the mood!

FoMSci thanks the University of Helsinki for an excellent job during the corona crisis. The university offers to co-operate with hospitals and help authorities with their facilities and laboratory equipment. The administration and IT helpdesk are working brilliantly by clear communication and instructions, which has made these exceptional times and the digital leap much easier for teachers and researchers. We are working together for a better future. #WeAreHelsinkiuni

ENVISION: Oil-water interface characterization

Ever wonder why your salad dressing can be so smooth, even though it is basically made of oil and vinegar? Vinaigrette, like mayonnaise, milk, and ice cream, are examples of what we call emulsions. Commonly used in the pharmaceutical, cosmetics, biotechnology and food industries, emulsions let us enjoy liquid products that feel good to our senses, while at the same time they protect bioactive compounds contained inside the mixture. They are formed by mixing two liquids that do not spontaneously mix (typically oil and water) and stabilized by a surfactant. The behaviour and properties of the surfactant on the border between oil and water determine the stability of emulsions, but the relationship between how the surfactants arrange themselves on the oil droplets and how they stabilize the mixture is still unknown. Our project, called “ENVISION”, is ongoing to provide insights about interfacial properties of emulsions. This project is funded by The Academy of Finland (1.9.2019–31.8.2023), led by Assistant Professor Kirsi Mikkonen, and conducted by Postdoctoral Researcher Thao Minh Ho and Doctoral Student Felix Abik.

In this project, we will be using a technique called atomic force microscopy (AFM). Imagine entering a dark room; your first instinct would be to look for the light switch on the wall by touching it with your hand, feeling the surface until you found the switch. With AFM, we are doing the same thing, but with a much smaller ‘hand’ to ‘touch’ the surface of our emulsions and make an image of what is happening on the droplets. We have successfully investigated trials on the preparation of emulsions with different surfactants. Next steps will be the characterization of the stability of emulsions. This will be followed by development of an innovative method for interfacial characterization using AFM. The result of this project will potentially open new scenarios in manipulating and designing intelligent delivery systems in forms of emulsions, for many bioactive compounds in numerous applications in technology and life sciences.

Photo: Felix and his doctoral thesis committee (who met for the first time just before the COVID-19 outbreak spread in Finland). From left to right: Postdoctoral Researcher Thao Minh Ho, University Researcher Laura Flander, Professor Orlando Rojas (Aalto University), Assistant Professor Kirsi Mikkonen (PI), University Lecturer Marianna Kemell, and Doctoral Student Felix Abik.

Have FUN with OLEOgels! New HiPOC grant for turning oleogels into functional materials

In December 2019, Fabio Valoppi obtained the Proof of Concept grant (HiPOC) from the Helsinki Institute of Life Science (HiLIFE) of the University of Helsinki for his project entitled “Functional oleogels with health enhancing ability (FUN-OLEO)”. Within this project, Fabio and his collaborators are transforming oleogels into novel functional materials using an unusual route.

Oleogels are considered the “fat of the future” and were developed to replace saturated, hydrogenated and trans fats in food products. They contain high fractions of liquid oil (85 – 99.5%) entrapped in a network made of structuring molecules. However, oleogels have some drawbacks that slow down their application in certain type of foods. Fabio came up with a novel concept that could extend oleogels’ applicability to a broader range of food products while introducing a new health enhancing ability: this is how you kill two pigeons with one stone!

The purpose of this HiPOC grant is to accelerate the patenting of Fabio’s novel idea. Unfortunately, we cannot reveal too much about the idea behind the project at this time. We can only say that we already obtained encouraging results! Stay tuned for more updates and to find out how this project will evolve.