UHPLC-MS/MS Method for the Analysis of 2,6 Toluene Diisocyanate and 2,4 Toluene Diisocyanate Released from Microa-gglome
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UHPLC-MS/MS Method for the Analysis of 2,6 Toluene Diisocyanate and 2,4 Toluene Diisocyanate Released from Microa-gglomerated Corks in Wine Francesco Corrias 1 & Eleonora Cossu 1 & Paolo Cardu 2 & Alberto Angioni 1 Received: 8 May 2020 / Accepted: 16 September 2020 # The Author(s) 2020
Abstract Micro-agglomerate corks, made by agglutination of cork granulate through the addition of different adhesives, represent an important slice of the market of cork stoppers. Binder glues which are polyurethane- or butadiene-based have been used since they have strong agglomerating effect. Unfortunately, polyurethane-based glues can have isocyanide end group compounds which can migrate into the wine. 2,4-toluene diisocyanate (2,4-TDI) and 2,6 toluene diisocyanate (2,6-TDI), can be found in adhesive and could migrate into wine. A simple ultrahigh-performance liquid chromatography-mass spectrometry (UHPLC-MS/ MS) method for the determination of these active ingredients (a.is.) in wine has been developed. The method has been validated under Eurachem CITAC guidelines (Cooperation on International Traceability in Analytical Chemistry). Instrument limit of detection (LOD) and to a limit of quantification (LOQ) for 2,6 TDI and 2,4 TDI were 0.42 and 0.39 μg/L, and 1.72 and 1.57 μg/L, respectively. Four different solvents applied for recoveries showed quite different rates ranging for 2,6 TDI and 2,4 TDI from 17.96 to 88.53 %, and 40.08 to 99.18 %, respectively. Real sample analysis showed low residue levels, especially of 2,6 TDI, with values always below the LOQ. The data reported on real samples allowed to establish that from a risk management purpose, no toxicology risk can be accomplished. Keywords 2,4 TDI . 2,6 TDI . LC-MS/MS . Micro-agglomerated corks . Wine
Introduction The use of cork as stoppers is traced back to the ancient Romans; in fact, in the Greek and Roman world, it was customary to use it for the closure of amphorae (Denecker and Vandorpe 2007). In a bottle of wine, the type of closure represents one of the most important and delicate parts (especially in the case of fine and aging wines). Nowadays, wine bottle can use a different * Alberto Angioni [email protected] Francesco Corrias [email protected] Eleonora Cossu [email protected] 1
Department of Life and Environmental Science, Chemical food Analysis Laboratory, University of Cagliari, University Campus of Monserrato, S.S. 554 - Bivio Monserrato - Sestu. S.P. Monserrato Sestu Km 0, 700 Cagliari, Italy
2
via Dettori 58, 09067, Elmas Cagliari, Italy
device for their closing; the most used are cork, screwcaps, and synthetic polymer material such as Low-Density Polyethylene (LDPE); the use of one or the other is related to commercial purpose and wine philosophy (Godden et al. 2008). Screwcaps have been initially used in the whisky industry with excellent results, and have been introduced in the wine market in the late 1950s in France, after replacing a thin cork layer underneath the cap with neutral polyvinylidene dichloride (PVDC) (Courtney 2001). Their
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