La technique SBSE dédiée à l analyse de composés odorants par GC-MS-Sniffing
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1 La technique SBSE dédiée à l analyse de composés odorants par GC-MS-Sniffing Annabelle Cingöz, A.Borcy, C. Henneuse January, 26-27, 2015
2 Introduction Packaging and «Off-Flavour» Packaging requirement: -ensure the integrity of the content -ensure the safety of the consumers European regulation N 1935/2004 N 10/2011 (plastic) Off-Flavour: - Are caused by the packaging, ageing, food/packaging material interactions - Occur by volatile transfer, diffusion into the food or chemical reactions Light, Oxygen, Moisture, Temperature Alteration of the physical and chemical properties: ageing, oxidation, interactions with content derivatives, etc Container Stability, Organoleptic properties etc Ingredients Polymers, Additives Contents Auxiliaries VOC Degradation products
3 Aim of the study Odorous compounds emitted by different polyolefin formulations for caps and closure applications after accelerated ageing (solar simulation) Analysis of a formulation without anti-uv additive (worst case) Influence of slip agents and anti-uv additives Comparison with a commercial reference
4 Experimental protocol Conditioning Polymer material in contact with water Accelerated ageing in Q-SUN Xenon Test chamber (solar radiation simulator chamber) Controlled temperature 40 C Extraction of volatiles: sequential EG-PDMS procedure 1)Twister EG silicone Magnetic stirring / 1h 2) Twister PDMS Magnetic stirring / 1h TD-GC-MS-sniffing (expert panel)
5 GC-MS-Sniffing analysis MS Sample Separation Sniffing GC-MS-Sniffing analysis : correlation chemistry/odour Organisation of the olfactive space according to 6 axes (amine, hesperidic, terpenic, sulphured, pyrogenous and sweet) 45 descriptors (references molecules) are used to characterise the odours (qualitative and quantitative analysis based on a relative intensity scale)
6 GC-MS-Sniffing analysis Formulation without anti-uv Octanal Chemistry Heptanal Nonanal 0 Time--> Hexanal Odour Heptenal Time--> Minor compounds can be responsible of odour!
7 Comparative study - VOCs Total VOC Alkanes Ketones Aldehydes Alcohols F11 F10 F4 F3 F2 F1 (without stabilizer) Commercial reference Formulation Slip agent Anti UV Reference A 1 F1 B No F2 B 2 F3 B 3 F4 B 1 F10 C 2 F11 D 3 Other compounds Number of hits
8 Comparative study - Odour Odorous notes NI: fresh, fatty, flowery, musty and burnt notes ND: fresh, fatty and earthy notes Terpene: fresh note Sulphurous: sulphurous note Ketones: fresh notes Aldehydes: rancid, fatty, green and fresh notes Alcohols: green and fresh notes F11 F10 F4 F3 F2 F1 (without stabilizer) Commercial reference Formulation Slip agent Anti UV Reference A 1 F1 B No F2 B 2 F3 B 3 F4 B 1 F10 C 2 F11 D Number of hits
9 Conclusion of the study SBSE coupled with GC-MS-Sniffing is a powerful technique for the identification of organoleptic contaminants in aqueous samples. Effect of sunlight exposure of PO on the organoleptic properties. Degradation of slip agents. Odorous compounds coming from the stir bars themselves have to be taken into account
10 GC-Sniffing analysis of EG-PDMS Twisters GC-MS-Sniffing analysis of Twister without extraction step RT (min) CAS Nr Compounds Detected by MS Field of Odours references Evocation Intensity 5,09 ND cyclopentanone + diacetyl solvent/ether +fatty notes 1 + 1,5 5,52 unknown cyclopentanone solvent/ether note 1 5,8 ND acetyl pyrazine roasted note 1 13,4 ND diacetyl fatty note 1 14, ,3-Dioxolane, 2-methyl- cyclopentanone solvent/ether note <1 17,24 unknown alcohol cis-3-hexenol green note/grass 2 19, Methoxyethyl vinyl ether cyclopentanone solvent/ether note 2,5 22,73 unknown ether cyclopentanone solvent/ether note 2 23,17 unknown ether acetic acid -->cyclopentanone pungent--> solvent/ether note 2-->2,5 25,02 unknown acid acetic acid pungent note 1 35,38 ND 1-octen3-ol fresh note/mushroom 2 36,63 ND phenol ink 2 39,24 ND isobutylquinoleine earthy note, asparagus 1 EG vs PDMS Twister : numerous solvent/ether notes!
11 Many thanks to Mrs Anne BORCY For more information: Zone industrielle C Rue Jules Bordet B-7180 Seneffe BELGIUM Tél Fax annabelle.cingoz@certech.be
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