Plasticisers in poly(vinyl chloride) gasket seals and in food matrixes: food safety implications and analytical solutions by mass spectrometry

Lids seal against the glass rim with gaskets consisting of plasticized PVC and represent an issue as migration of plasticizers from these gaskets into foods. The plastisols used typically contain 25¿45% plasticizer, frequently epoxidized soy bean oil and sometimes phthalates, sebacates, citrates, acetylated mono/diglycerides and very recently with the promising alternative of polyadipates. Migration into the food can occcur both during sterilisation and storage; furthermore PVC degradation could induce the elimination of HCl and the correspondent potential formation of other derivatives. Toxicological data and legislative restrictions are not available for all the plasticizers and derivatives involved in this contest; there is also a lack for adequate analytical strategies for some of them. Mass Spectrometry combined with Gas Chromatography and\or Liquid Chromatography demonstrates to be the correct solutions either for single-target or multiresidual analysis of plasticisers and additives in PVC gaskets and also in the correspondent foodstuffs. In particular, a challenge task is reserved to the elucidation of the composition and quantification of the migrated material < 1000 Da derived by different polyadipates available on the market. Finally, high resolution MS instruments, possibly coupled to Ultra High Performance Liquid Chromatography can be further helpful for characterizing traces related to plasticizer derivatives.JRC.I.1-Chemical Assessment and Testin

Revision of a European Union official method to enforce legal provisions: The case of diclazuril

Diclazuril is a coccidiostat currently authorized as feed additive in the European Union (EU), with a legal limit set at 1 mg/kg. For official control, an official EU method based on reversed-phase HPLC coupled with UV detection at 280 nm needs to be applied. Recently, the EU Reference Laboratory for feed additives was informed that the recovery rate for diclazuril was very low when implementing this method and performed experiments demonstrating that the indicated sorbent mass of the solid-phase extraction (SPE) was too low. Objective: Therefore, the paper presents a modified method protocol and the results of an interlaboratory study, performed on two compound feedingstuffs containing diclazuril around the legal limit. Methods: The official method was modified by using a higher SPE sorbent mass and was further subjected to validation. Results: The obtained values for the relative standard deviation for repeatability were 4.5 and 11.2%, and the corresponding values for the relative standard deviation for reproducibility were 14.3 and 18.1%; the calculated HorRat values were 0.95 and 1.14. Furthermore, acceptable mean recovery values of 98 and 111% were obtained for the two test materials, respectively. Conclusions: Based on the obtained performance profile, it was concluded that the modified official method was fit for purpose. In consequence, the official EU method will be corrected accordingly. Highlights: The highlights of this work are reflected by the following terms, namely Diclazuril, correction of EU official method, and interlaboratory study.JRC.F.5-Food and Feed Complianc

A review of the work of the EU Reference Laboratory supporting the authorisation process of feed additives in the EU

This paper describes the operation of the European Union Reference Laboratory for Feed Additives (EURL) and its role in the authorisation procedure of feed additives in the European Union. Feed additives are authorised according to Regulation (EC) No. 1831/2003, which introduced a completely revised authorisation procedure and also established the EURL. The regulations authorising feed additives contain conditions of use such as legal limits of the feed additives, which require the availability of a suitable method of analysis for official control purposes under real world conditions. It is the task of the EURL to evaluate the suitability of analytical methods as proposed by the industry for this purpose. Moreover, the paper shows that one of the major challenges is the huge variety of the methodology applied in feed additive analysis, thus requiring expertise in quite different analytical areas. In order to cope with this challenge, the EURL is supported by a network of national reference laboratories (NRLs) and only the merged knowledge of all NRLs allows for a scientifically sound assessment of the analytical methods.JRC.D.5-Standards for Food Bioscienc

Electrooxidation of Chlorophenols Catalyzed by Nickel Octadecylphthalocyanine Adsorbed on Single-Walled Carbon Nanotubes

We described the synthesis of nickel octadecylphthalocyanine (NiPc(C10H21)8), followed by its adsorption on single-walled carbon nanotubes (SWCNT) to form SWCNT-NiPc(C10H21)8 conjugates. SWCNT-NiPc(C10H21)8 was used to modify a glassy carbon electrode (GCE) and for the electrooxidation of 4-chlorophenol and 2,4-dichlorophenol. The SWCNT and NiPc(C10H21)8 have a synergistic effect on each other in terms of improving electrocatalysis for the detection of chlorophenols. The stability of the electrode improved in the presence of NiPc(C10H21)8 or NiPc compared to the bare GCE. The presence of SWCNT improves the electrocatalytic behaviour of NiPc(C10H21)8 but not of unsubstituted NiPc. All modified electrodes showed improved stability towards the detection of 2,4-dichlorophenol. The best stability for 4-CP detection was observed in the presence of SWCNT for NiPc(C10H21)8