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Demonstration of innovative filter aid technology to reduce undesirable substances (pesticides and mycotoxins) in beverages such as wine and beer

Final Report Summary - ADFIMAX (Demonstration of innovative filter aid technology to reduce undesirable substances (pesticides and mycotoxins) in beverages such as wine and beer)

Executive Summary:
ADFIMAX project aims at improving liquid food safety by selectively removing undesirable substances such as mycotoxins and plant protection products (PPP). ADFIMAX is a demonstration project that follows a FP7 R&D project named DEMYBE. Five SME’s active at different level of the business chain grouped in a consortium whose objective was to demonstrate that foreground from DEMYBE was commercially exploitable.
The ADFIMAX technology is based on an innovative Active Vegetable Fiber (AVF) with high adsorption capacity. It is this adsorption capacity that selectively removes undesirable substances from liquid.
Using the ADFIMAX product as a filter media is the most effective way to valorize the specific adsorption activity of AVF. The first mode of use is to integrate the ADFIMAX product into a Kieselguhr/DE (Diatomaceous earth) filtration. In this setup the ADFIMAX product replaces the pre-coat layer. The second mode of use is to integrate the ADFIMAX product into a filter sheet and to use this filter sheet in a filtration. In both cases the set up does not require any material investment.
The consortium had two major objectives:
1. demonstrate that it is possible to product this AVF at industrial scale
2. demonstrate at industrial scale that the mode of use of this AVF achieved significant results without any other impact on the food liquids.
The Consortium produced batches of around 100kg. Specific work was performed to improve the production cost and reliability by developing a continuous production concept. The quality and characteristics of the large scale continuous production process was not significantly different than the lab scale batches produced during the previous project.
Filter-sheet, integrating the AVF, were produced at lab-scale with filtration characteristic compatible with normal filter sheets.
More than 10 large scale industrial filtrations were performed in commercial wineries. In each of these filtrations significant reduction of undesirable substances was achieved. No impact on chemical parameter of the wine was observed in the final tank. No taste impact was detected 15 days after filtration.
Numerous actions were aimed at getting a regulatory approval for the technology.
All demonstration objectives were achieved. At the end of the project the partners have the intention to increase the production capacity, to continue the regulatory work and to start to commercialize the product in niche markets.

Project Context and Objectives:
The primary motivation of the ADFIMAX project was to demonstrate that the foreground created in a previous research project DEMYBE was commercially viable. In a first step we will remind the objectives and foreground created by DEMYBE and in a second step we will explain de specific objectives of ADFIMAX.
The primary motivation for the DEMYBE project was focused on the needs of liquid food producers to safely reduce or remove mycotoxin contaminants from everyday beverages. Mycotoxins are fungal secondary metabolites which have been subject to examination by the World Health Organisation (WHO), and are considered harmful for humans.
The DEMYBE foreground included:
(a) identification of new sources of natural fibre material with higher adsorption potential than original product (micronised wheat envelopes) and good aptitude to be used as a filter aid
(b) discovery, implementation and validation of a soft fractionation/purification method with the objective of enhancing the qualities of the filter aid. The fractionation method:
- improves the ability of the natural vegetable fibre raw material to adsorb mycotoxins and other toxins ;
- eliminates any bad taste and aroma impact which might otherwise be imparted by the fibres themselves to filtered liquid;
(c) attainment of the decontamination level objective - extraction of 80% OTA from wine and beer with 2g/litre of filter adjuvant:
- indeed, the target was surpassed in filtration trials, yielding up to 95% decontamination
- furthermore, the prototype has proven capable of extracting Plant Protection Product residues, a feature of specific interest to wineries, where currently no solution with such selective properties is yet available;
(d) confirmation that the micronisation process is critical to further enhancing the adsorption capacity of the filter aid;
(e) full proof-of-concept of the ability of this filter aid prototype technology to be deployed in the filtration processes currently prevalent in the brewing and wine industry.

The group decided to call the innovative filter adjuvant Activated Vegetable Fiber (AVF) and to register ADFIMAX as the brand of the product. ADFIMAX is also the name of the EU project.
The objectives of the work program were:
1. Scale up the AVF production process: after DEMYBE we had a labscale production and were able to provide production lot of around 5kg of reliable quality. The aim was to test bigger purification machines (700l vessel) and to validate the design of a production facility of around 100T/year.

2. Reduce production costs: within DEMYBE we focused on efficacy of the final product and achieved a great improvement in the adsorption capacity of the product. For a commercial development of the innovation we needed to reach economical efficiency.

3. Confirm the reliability of the scaled up production process to produce a consistent product with the DEMYBE characteristics

4. Confirm and demonstrate that using the selective filtration technology within a normal commercial filtration process reduced Plant Protection Products and OTA level and also did not have any impact on other qualities of the filtrated product such as taste, color or chemical composition. These test were also used to validate that the scaled up production process was able to provide a reliable

5. Investigate other mode of use of the AVF such as using them as a component of a depth filter sheet and evaluating the potential of this application. Investigate also other food liquid than wine and beer.

6. Prolong the regulatory work to get the AVF approved for the intended use. Food law and specific sub-class law such as wine making rules are obstacle to the use of the technology. ADFIMAX aim was to identify the regulatory path and start fulfilling the requirement of each identified rules. These included FDA, OIV, Codex alimentarius, …

7. Communicate and disseminate the technology where we see commercial potential. These included participation at wine congress and symposium., beer symposium, etc…

Project Results:
As a demonstration project ADFIMAX did not particularly aim at foreground production. There was however three foregrounds created:
(a) Discovery of a new process of AVF production:

At the origin of the project the objective of the scale up was only to use bigger vessel and therefore increase the batch size. From a 30 l vessel the plan was to use a 700 l vessel to perform the purification process. Although the scaling up of the batch did achieve the production quantity objective (to produce more tons) it appeared very quickly to the consortium that using a batch technology would always be a drag on the cost.
The team started to think at other ways to achieve the production objective and the idea of a continuous technology emerged. This was a very innovative design and needed to be tested. The team decided to build an intermediate size machine to validate the different hypothesis. This was a success and AVF produced by the continuous flow was successfully tested in industrial filtration trials. The use of the continuous purification machine enabled to substantially reduce cost of production and to ease further scale up of the production. The actual machine is able to process the first batches needed for commercial use.
The shift from a batch technology to a continuous technology is one of the foregrounds created by ADFIMAX.
(b) Discovery of the ability of the AVF to perform the adsorption function when integrated into a depth filter sheet
After DEMYBE we had a mode of use of the AVF as a pre-coat filter adjuvant in a diatomaceous earth filtration (DE). This filtration technology is common in wineries and breweries but it is more and more replaced by other technology such a cross-flow. One of the reasons of the substitution is the health concern of using the Kieselguhr/DE. The substitution of this hazardous product by AVF was a secondary objective of the DEMYBE project.
It appeared therefore that limiting the application of AVF to DE filtration only would limit the potential use of the product. ADFIMAX objective was to investigate the ability of the AVF to be used as a component of a depth filter sheet. Depth filter sheet are the main business of EATON.
EATON made some lab-scale filter sheet. This enabled EATON to test different composition of filter sheet and to produce material that was tested successfully.
The results show even a slightly better adsorption activity of the AVF when put into a filter sheet than just used as a pre-coat layer.
The confirmation of the potential use of the AVF into a filter sheet is the second major foreground of the ADFIMAX project.
(c) Discovery of another undesirable substance selective adsorption
Phtalate are undesirable liquid contaminant. The consortium made an exploratory trial to investigate if the AVF could remove these contaminants.
In an adsorption protocol the AVF was able to remove significant fraction of some Phtalate such as Dibutylphtalate (DBP). This new functionality of the AVF could increase even further the scope of ADFIMAX market applications.
(d)Technical results
ADFIMAX produced numerous technical results in wine and beer filtration. In each filtration significant Plant Protection Product reduction was achieved.
There are mainly two mode of use of ADFIMAX. One is as a pre-coat filtration adjuvant the other is integrated into a filter sheet as a fiber constituent. Technical results from both mode of use are presented below.
* Pre-coat application filtration
Nine DE (diatomaceous earth) wine filtrations were performed using the pre-coat mode of use. These filtrations were done in commercial wineries with commercial wine. The consortium used a Pilot filter of 0,864 m² and treated volumes between 1.500 to 3.000 Liters per filtration. The consortium received the authorization from the food safety agency (DGCCRF) to perform these tests. This authorization allowed the commercial wineries to sell the filtered wine. Around 16.000 liters of commercial wine were filtered with ADFIMAX during the project.
No OTA was detected in these wines. Total Plant Protection Product level was measured between 11ppb to 112ppb. This difference was mostly linked to the trial site. In all filtration, ADIFMAX integrated as a pre-coat reduced significantly the level of Plant Protection Product in the filtered wine while the blank filtration did not show any significant reduction.
Color and other wine parameters were measured and did not show any significant differences from the blank filtration.
Taste was detected significantly different for the first fractions and at the day of the filtration.
No significant taste differences were detected 15 days after filtration, neither for the first fractions nor for the final tank. The early impact of the filtration on taste is known and common for other filtration technology.
* Filter-Sheet application in wine and beer filtration
In the first step the consortium did laboratory tests with a filter sheet of 130 cm². These tests confirmed the ability of ADFIMAX fiber to adsorb Plant Protection Products when integrated into a filter-sheet. These tests were the basis of the foreground described here above.
Later in the project bigger filtrations were performed using 40 cm by 40 cm filter. These larger filtrations were performed in beer and wine in different countries (France, Switzerland and Germany)
Filter sheet were produced using ADFIMAX as an ingredient. These sheets were then used in a simple filter sheet filter replacing normal filter sheet such as BECOPAD.
Variations between Plant Protection Product results are due to factors such as: speed of filtration, total filtered volume and the type of filter sheet. Indeed numerous filter sheets were produced and a substantial improvement was achieved during the project.
Most of these factors were analyzed and enabled the consortium to define the mode of use of the AVF in a filter sheet.
The filter sheet production was only done at lab scale so the next step is to investigate the scale up the production of filter sheet. The sheet size of an industrial batch in a filter sheet factory means that it is not so easy to make an industrial production trial. This issue will be addressed in the exploitation of results.

(d) Regulatory results
In the food market we need to have regulatory approval for the use and the claim of the product. For our project there are different regulatory approvals for different markets and different kind of liquids.
In a first step we obtained the approval that the product is safe for food use. We submitted two dossiers, one to the Direction générale de la concurrence, de la consummation et de la répression des frauds (DGCCRF) in France and one in the FRESENIUS institute in Germany.
We obtained from the DGCCRF the authorization to use the product for experimental filtration and this enabled the wineries to sell the wine on the market. This authorization was critical for the project and was given for one year. A authorization for a second year was submitted and obtained. This will enable continuing the trials in 2015.
We obtained from Fresenius the following assessment:
“The sample sent to us was analyzed in accordance with the code of Federal Regulation of the Food and Drug Administration (FDA). In accordance with this regulation, the product is safe to use as intended if the goods correspond to the tested quality”
The Fresenius assessment is more general than the DGCCRF approval and certifies that the product is food grade world-wide.
The two first regulatory approvals do not however allow us to claim the specific function of the ADFIMAX product.
The group decided that the most valuable market for the ADFIMAX functionalities is the wine market. The wine production is regulated by the International Organisation of Vine and Wine (OIV) that list the authorized production methods. It is therefore critical that ADFIMAX becomes an OIV authorized production method.
Numerous results were obtained in the OIV:
- presentation of two communications to the OIV annual meeting.
- presentation of one communication to the scientific committee.
- One other country has decided to do trial with our product
- Confirmed interest from at least two other countries to test ADFIMAX
We also have prepared the safety dossier and the OIV Codex dossier. All these dossiers will be submitted to the OIV organization in early 2015.

Potential Impact:
The ADFIMAX project fulfilled its objectives with minor deviations. It confirmed the ability to produce efficiently and confirmed the functionalities of the AVF to reduce Plant Protection Product and mycotoxin content of beverages. Therefore the impact of the ADFIMAX project is a prolongation of the potential impact of DEMYBE.
In DEMYBE we identified that: “An external factor which is also driving market interest, concerns the need for improved food safety. Ever more stringent EU regulations are continually narrowing the legal limits for contaminants present in food and drink. Furthermore, measures aimed at improving health at work have become even more of an issue in 2011”
At the end of ADFIMAX we think this “external factor driving market interest trend” is still valid and probably even higher than at the beginning of DEMYBE.
The scale of the impact of ADFIMAX is now even wider by the confirmation that the AVF can be used as a component of a filter sheet. This will give an opportunity in many other markets using filter sheet filtration rather than limiting the application to DE filtration.
All this is improving the potential impact of our innovation.
The socio economic impact of the ADFIMAX project is in line with the DEMYBE final report impact.
The reduction of Plant Protection Product in food beverages is a society objective. The use of our technology at large scale would lead to a significant reduction of the population exposition to these products.
The use of a renewable resource to replace some of the Kieselguhr which is not renewable is in line with a durable economic activity. By substituting some of the Kieselguhr by fiber we leave more of this non-renewable resource for further generations.
The production of ADFIMAX will lead to the economic development of at least two SME’s in Europe for the production. Kieselguhr mining being mainly out of Europe, this substitution will also reduce imports.
The main dissemination activities were aimed at OIV. This is because wine is identified as the biggest market potential for our technology. These dissemination activities include scientific communication at different OIV committee. It also includes VINITECH visit and contact at the wine show.

The exploitation of the demonstration results will follow the expected path as explained in the DOW. Each company of the consortium is complementary in terms of result exploitation.
PJH is an interested in the exploitation of the results in the extraction and purification of the raw material. REALDYME is interested in the micronisation of the intermediate material made by PJH. EATON is interested in the micronized material to integrate this material in filter sheet. EATON is also interested in the commercialization of the filter sheet.
IFV is interested in dissemination and development of new technology in wine. Bodegas Riojanas would like to play a role in the Spanish communication of the product.
PJH and REALDYME will join forces to set up a production company/organization to enable the production of the first commercial product lots. This set up is forecasted in the mid-2015. The size of this production facility will be in relation with the first demand for the product. It is forecasted to be a small volume that fits with the branch approach that EATON is developing.
The demonstration results will also be exploited by IFV for the OIV approval of the oenological practice. Until we receive full approval our sales will be constrained. IFV has a critical role in getting the full approval for the wine industry. Most of the work has been done during the demonstration project. At this stage we need to support the validation process from other countries such as Switzerland and perhaps Argentina. These countries will make tests and will need product and mode of use. The results from these countries will support the OIV regulatory procedure.

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