The market demands products that are sustainable. However, it is essential to remember that sustainability must never compromise safety. Alongside eco-design and LCA studies, the paper industry has an ally in prevention through laboratory analysis, including innovative approaches
Product sustainability is one of the main objectives of companies. However, there are regulatory requirements to be met and practical aspects to be taken into account, including the safety of the end consumer, which must always be guaranteed; an aspect that must also be assessed. It is precisely the risk assessment of cellulose-based materials and investigations into their safety, composition and compliance with end use that Marinella Vitulli, owner&director of Food Contact Center, spoke about at the Aticelca 2022 Congress.
The concept of sustainability
In order to verify and prove the environmental sustainability of a product, there are various schemes, starting with those created by the European Commission up to the guidelines prepared by industry, the PCRs (product category rules) or that set of rules and requirements for the development of EPDs, the environmental product declarations. For those in charge of analysis, an ideal tool is the life cycle assessment or LCA (life cycle assessment), according to ISO 14040 and ISO 14044.
In the context of the circular economy, among the actions of the so-called «5R rule» to achieve a zero-waste economy model – reduce, reuse, recycle, collect and recover -, the one that proves to have the greatest environmental impact is recycling, but the issue becomes particularly sensitive when we enter the realm of using recycled materials for certain types of products, especially when they have to come into contact with food.
«Whether we consider an item made of virgin cellulose or one made of a recycled material, we still have to consider that safety is a must. In the case of contact with food, article 3 of the Framework Regulation – EC Reg. No. 1935/2004 – stipulates that the article must not constitute a danger to human health, result in changes to the food or even simply sensory changes». This is the general rule that applies to all paper products, but then we have to figure out how to demonstrate compliance according to specific rules. And this is where things get complicated.
From general rules to specific rules
The main problem is that paper has no harmonised European regulation. Therefore, having to refer to «national laws, documents produced by associations, rather than Council of Europe resolutions» becomes a must. In this regard, Food Contact Center – which is an accredited laboratory for carrying out Moca (food contact materials) analyses – has developed its own tool called Matrix, «a matrix of regulations that makes it possible to check, at European level, all the countries that have a specific law for a given material, in this case for paper and cardboard. The tool,» explains Vitulli, «shows that the situation is definitely complicated, even though, when we talk about the ‘foodness’ of a material, this is ultimately represented by compliance with Italian, French and German laws».
In some respects, the regulations on food contact in Italy are much stricter than in other countries, «as far as materials containing recyclate are concerned, contact can only be made with dry food,» Vitulli continues. This implies that for contact with non-dry food, for example pizza, only pure cellulose materials are required.
The situation is different in France, however, «where there is a large list of substances with very challenging limits, especially for phthalates and crosslinkers. There is also the possibility of performing analyses using solvents and simulants, but the comparison with the law must be made with regard to migration into the food».
Germany, finally, refers to the BfR, i.e. recommendations – which in fact have the force of law – in which, as far as recycled materials are concerned, a table with the parameters of the various substances is given. Here too, compliance can be demonstrated by migration tests within the food.
Laboratory Analyses
When carrying out controls, the first step consists of extractive tests on the samples to be analysed. Once the contaminant values have been identified, the consumer’s exposure must be assessed. Only after these calculations can one arrive at proving the compliance or non-compliance of the material. «We always try to prove the real exposure to the consumer,» explains Vitulli, «because the mere presence of contaminants in itself is not enough to prove that they are dangerous to human health, we need to verify whether there really is a risk and whether there is real exposure».
The Food Contact Centre team recently carried out a study in collaboration with the CNR group of Pisa and Siena precisely in this area. «The research was carried out on parameters analysed in parallel: our group performed the analysis on paper and cardboard, while the CNR group on biological samples».
First of all, the analytical approach that would then be adopted was shared.
«For organic contaminants, it was a matter of analysing volatile, semi-volatile and non-volatile substances with the GC/MS gas chromatography-mass spectrometry technique, while for typical paper and cardboard contaminants, both volatile and non-volatile, the liquid chromatography technique was used».
The difficulty in using this technique, especially in screening, is the absence of libraries on the market. «In 2018,» Vitulli points out, «with the collaboration of the company Sciex and under the supervision of the CNR in Pisa, we carried out the construction of a library – our project for a few years already – then published and distributed in 2020».
The library is based on the LC Q TOF technique and is constantly being implemented. It currently collects 12,000 contaminants of paper and cardboard materials – both food-contact and non-food-contact – as well as another 1,700 substances that are also characterised by leavening time and mass/mass.
The results obtained
The analyses carried out on samples of paper and cardboard – both virgin and recycled papers – focused on the presence of phthalates analysed in gasmass and bisphenols analysed in liquidmass. The results obtained, explains Vitulli, showed that «about 10 per cent of pure pulp samples had these contaminants as content, while for recycled paper samples the values were much higher: more than 90 per cent of them recorded the presence of these substances».
«With the screening technique, we were also able to investigate the presence of other contaminants, which were recognised thanks to our database».
«With the screening technique, we were also able to investigate the presence of other contaminants, which were recognised thanks to our database». Tests carried out on biological samples by the NRC, on the other hand, showed «mainly the presence of metabolites and bifurcates within the urine samples».
This study has shown that contaminants are indeed ingested by humans, with an undoubted biological impact; however, an important aspect must be considered, «we are talking about ubiquitous contaminants,» the director points out, «and this means that human exposure arises from a combination of several factors, and it is not certain that this intake derives from the paper product».
The next step in the study, therefore, was to try to understand whether the substances found in the extraction tests actually corresponded to real migration.
The tests were carried out on bisphenols with extraction solvents and the results were then published in a thesis carried out in collaboration with the University of Florence. But that’s not all, the bisphenol migration test inside the pizza – carried out by means of a migration analysis inside the food accredited by the Food Contact Centre with Accredia – showed that there was no migration. In practice, the same samples that were found to be non-compliant with the extractive solvent tests were found to be compliant with the in-food migration test. This was achieved even when the sample was subjected to severely deteriorating conditions – for example, the cardboard specimen was heated in an oven for 24 hours.
«With this approach, the results show that there is no migration, also because bisphenols are heavy substances and therefore it is very difficult for them to migrate.
The situation is different for phthalates, which, on the other hand, did register some migration, but always within the legal limits».
In practice, the same samples that were found to be non-compliant with the extractive solvent tests were found to be compliant with the in-food migration test. «In this case, too, we performed the migration into the food – last year we also accredited Accredia for aluminium and iron migration into the food. Again, for the same samples that gave non-compliance, we were able to demonstrate compliance».
Prevention is better than cure
However, proving compliance through the analysis approach inside the food is not always permitted by law. For this reason, Food Contact Center, again in collaboration with CNR, validated a Fast-screening method focused on the main contaminants and especially on the presence of bleaching agents, substances regulated by UNI EN 648:2019. «Considering, therefore, that this standard must necessarily be applied for bleaching agents, it can be useful in the preventive phase to know whether there is already, within the material that will later go as a recycling component, a certain amount of bleaching agents, moreover, taking into account that the paper mill will later add others. For this reason,» explains Vitulli, «we have developed a screening method and a specific library of whitening substances» hat will be very useful for paper manufacturers.
«So we can work on prevention, always remembering that, in the paper industry, the use of recycling is very advantageous, but sustainability cannot compromise safety, and to demonstrate the latter there can be both traditional and innovative approaches that assess the possibilities of the law».
Beyond the laboratory
Food Contact Center was established as a laboratory in 2016. Accredited to perform Moca analyses, it now employs more than 15 specialised technicians and operates in two locations, in Pistoia and Brescia, as well as having an office in Cuneo. «We specialise in migration analysis, so we are mainly concerned with safety,» explains founder and director Marinella Vitulli, «but in the Brescia laboratory we are also equipped to carry out compositional analyses for material characterisation». However, Food Contact Center is not just a laboratory, it provides several services and to bring them together, two years ago, Food Contact Services was created. This new branch of the company deals with regulatory assistance, LCA (life cycle assessment) studies, assistance in the area of certification schemes, Accredia 17020 accredited inspection visits and LCA in the area of eco-design.