Automated Solid‐Phase Microextraction GC‐MS/MS Method for Quantification of Volatile Limonene Oxidation Products in Encapsulated Orange Oil

Abstract Limonene, widely present in consumer products, is prone to oxidation and leads to the formation of undesirable reaction products. A solid‐phase microextraction ( SPME ) GC ‐ MS / MS method was developed for the quantification of volatile limonene oxidation products, in encapsulated oil samples, by the optimization of MS parameters and SPME sampling conditions including fibre coating, temperature and time. The detection limit of the method reached 10 to 15 ppb for the limonene oxides, and less than 5 ppb for carvone and carveol isomers. Standard addition calibration was utilized to compensate for matrix effects of the encapsulation, flavouring, and to optimize the accuracy and versatility of this method. Sample throughput and precision of the method were improved through in‐line automated SPME sample preparation. The popularity of limonene as a flavouring compound in many consumer products, allows this method to be adapted to quantify different levels of volatile limonene oxidation products in encapsulated matrices.