Quantification of Residual Perfume by Py-GC-MS in Fragrance Encapsulate Polymeric Materials Intended for Biodegradation Tests

Abstract

Perfume encapsulates are widely used in commercial products to control the kinetic release of odorant molecules, increase storage stability and/or improve deposition on different substrates. In most of the cases, they consist of core-shell polymeric microcapsules that contain fragrance molecules. A current challenge is to design and produce polymeric materials for encapsulation that are both resistant and non-persistent. The selection of such eco-friendly formulations is linked to a deep understanding of the polymeric material used for encapsulation and its biodegradation profile. To collect this information, pure samples of capsule shells are needed. In this article we present an innovative quantification method for residual volatiles based on pyrolysis-GC-MS to enable validation of sample quality prior to further testing. The presented analytical method also led to the development of a robust and comprehensive purification protocol for polymers from commercial samples. Standard techniques are not suited for this kind of measurement due to the non-covalent embedding of volatiles in the 3D structure of the polymers. We demonstrated the confounding impact of residual volatiles on the estimated biodegradability of fragrance encapsulates.

Are Fragrance Encapsulates Taken Up by Aquatic and Terrestrial Invertebrate Species?

“…By investigating both markers using fluorescence microscopy, the structural integrity and stability of the test material were confirmed, and we were able to detect any potential leak of the oil after breakage of the shells. The fragrance encapsulates were prepared according to procedures in the literature (Gasparini et al, 2020; León et al, 2017; Paret et al, 2019).…”

“…By investigating both markers using fluorescence microscopy, the structural integrity and stability of the test material were confirmed, and we were able to detect any potential leak of the oil after breakage of the shells. The fragrance encapsulates were prepared according to procedures in the literature (Gasparini et al, 2020;León et al, 2017;Paret et al, 2019). Melamine-formaldehyde resin (1.12 g; Urecoll SMV; BASF), 0.12 g of methylated melamine-formaldehyde resin (CYMEL ® ; 9370 Resin), colloidal stabilizer (4.90 g, poly[acrylamide 20%, acrylic acid 80%] 20% w/w in water), and water (42.0 g) were introduced into a 200-ml reactor at room temperature.…”

Country‐Specific Environmental Risks of Fragrance Encapsulates Used in Laundry Care Products

“…Typical melamine‐formaldehyde fragrance‐delivery systems used in laundry care products were used to prepare the test material. A protocol for preparing such an FE suspension at the lab scale has been reported by Gasparini et al ( 2020 ).…”

“…The shells are designed so that the contained fragrance is released by the action of friction or pressure, which will rupture the shells. Because the test material of interest is one composing the polymeric shells, a protocol was developed to remove the fragrances and the additives from the capsules (Gasparini et al, 2020 ). The protocol consisted of several steps of drying, grinding, and extraction by organic solvents or water.…”

“…They are spheres with a typical diameter between 10 and 50 µm and a wall thickness <1 µm (Laroche & Gonzalez, 2018 ) containing the fragrance components. The shells are often made of cross‐linked thermoset melamine‐formaldehyde polymer and can also consist of other cross‐linked thermoset polymers such as polyurethane, polyurea, and polyamide, but to a lesser extent (Gasparini et al, 2020 ). Diverse chemistries are employed in the preparation of polymeric FEs involving phase separation polymerization, interfacial polymerization, or both (Jacquemond et al, 2009 ; León et al, 2017 ; Paret et al, 2019 ).…”